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Anal. Chem.

1983, 55, 164R-196R

(F24) Varnell, D. F.; Runt, J. P.; Coleman, M. M. Macromolecules 1981, 14, (G20) Schabron, J. F.; Bradfleld, D. 2 . Anal. Chim. Acta 1981, 129, 243-6.
1350-1356. (G21) Schenk, C.; Kayen, A. H. M. Cong. FATIPEC 1980, 15, 345-360.
(F25) Aylward, N. N.; TI, S. S. J . Polym. Sci., folym. Phys. Ed. 1981, 19, (G22) Sidwell, J. A.; Wllllamson, A. G. Int. Rubber Conf. 1981, 1, C8.1-
1805-18 16. C6.8.
(F26) Antoon, M. K.; Koenig, J. L.; Seraflnl, T. J. folym. Scl., folym. fhys.
Ed. 1981, 19, 1567-1575. THERMAL ANALYSIS
(F27) Stevens, G. C. J. Appl. Polym. Scl. 1981, 26, 4259-4278.
(F28) Stevens, G. C. J. Appl. folym. Scl. 1981, 26, 4279-4297. (Hl) Belorgey, G.; Prud'Hommme, R. E. J. folym. Sci., Polym. Phys. Ed.
(F29) Endrey, A. L. J. folym. Scl., folym. Chem. Ed. 1982, 2 0 , 1982, 20, 191-203.
2 105-21 16. (H2) Cardillo, P.;Casalini, A.; Galtlerl, A.; Vecchi, C.; Audlslo, G. Conv. Itai.
(F30) Coleman, M. M.; Sivy, G. T. Carbon 1981, 19, 123-126. Sci Macromol., 5th 1981, 249-51.
(F31) Sivy, G. T.; Coleman, M. M. Carbon 127-131. (H3) Das, A. N.; Baijal, S. K. J. Appl. folym. Sci. 1982, 27, 211-23.
(F32) Coleman, M. M.; Slvy, G. T. Carbon 133-135. (H4) England, J. C.; Long, R. E.; Townsend, D. J. Anal. Proc. 1981, 18,
430-7.
(F33) Slvy, G. T.; Coleman, M. M. Carbon 137-139.
(F34) Gupta, M. K.; Bansil, R. J. folym. Scl., folym. fhys. Ed. 1981, 19, (H5) Gilbert, M.; Vyvoda, J. C. Polymer 1981, 22, 1134-6.
353-360. (H8) Glans, J. H.; Turner, D. T. Polymer 1981, 22, 1540-3.
(F35) Kim, C. S.;Dodge, A. L.; Lau. S.F.; Kawasaki, A. Anal. Chem. 1982, (H7) Klshore, K.; Santhanalakshmi, K. N. J. folym. Sci., Polym. Chem. Ed.
5 4 , 232-236.
1981, 19, 2387-75.
(H8) Nishizakl, H.; Yoshlda, K. J. Appl. Polym. Sci. 1981, 26, 3503-4.
LI OUID CHROMATOQRAPHY (H9) Ragosta, G.; Greco, R.; Martuscelll, E.; Sadocco, P.; Seves, A,; Vlclnl,
L. Polymer 1982, 23, 466-72.
(GI) Afredson, T. Am. Lab. (FalrtleM, Conn.) 1981, 13, 44, 46-7, 49-51. (H10) Lockwood, R. J.; Alberlno, L. M. ACS Symp. Ser. 1981, No. 172
(G2) Alfredson, T. Int. Lab. 1981, (Sept), 46, 48-50, 52-3. (Urethane Chem. Appl.) 363-72.
(G3) Andrews, G. D.; Vatvars, A. Macromolecules 1981, 14, 1603-5. (H11) Smith, W. A.; Barlow, J. W.; Paul, D. R. J. Appl. Polym. Scl. 1981,
(G4) Danlelewlcz, M.; Kubln, M. J. Appl. Polym. Sci. 1981, 26, 951-6. 26, 4233-45.
(G5) Edwards, D. J. H. HRC C C , J. High Resolut. Chromatogr. Chromatogr. (H12) Sebenlk, A.; Osredkar, U.; Zlgon, M.; Vizovlsek, I.Angew. Makromol.
Commun. 1982, 5 , 161-3. Chem. 1982, 102, 81-5.
(G8) Eppert, G.; Llebscher, G.; Stief, C. J. Chrom8togr. 1982,238, 385-98. (H13) Turi, E. A., Ed. "Thermal Characterlzatlon of Polymeric Materlals";
(G7) Fech, J.; De Wltt. A. f r o c . Int. Wire Cable Symp. 1980, 29th, Academic Press, New York, 1981.
327-30. (H14) Ulukhanov. A. G.; Lapitskll, V. A,; Akutin, M. S.;Skokova, L. D. Plast.
(G8) Furukawa, M.; Yokoyama, T. J. Chromatogr. 1980. 198, 212-16. Massy 1981. 9 , 59.
(G9) Hagnauer, G. L.; Dunn, D. A. Nafl. S A M E Tech. Conf. 1980, 12, (H15) Walsh, D. J.; Higgins, J. S.; Zhikuan, C. Polymer 1982, 23, 336-9.
648-55.
(G10) Hagnauer, G. L. Ind. Res. Dev. 1981, 23, 128-33. MISCELLANEOUS TECHNIOUES
(G11) Hagnauer, G. L.; Dunn, D. A. Ind. Eng. Chem. frod. Res. Dev. 1982, (11) Rose, W.; Meurer, C. frog. ColloidPolym. Sci. 1980, 6 7 , 167-9.
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(G12) Haney, M. A.; Dark, W. A. J. Chromatogr. Scl. 1980, 18, 655-9. (13) Leahy, H. J., Jr.; Campbell, D. S. Surf. Interrace Anal. 1979, 1, 75-9.
(G13) Hayashi, H. Nagano-ken Elsel Kogal Kenkyusho Kenkyu Kokoku 1981, (14) Martin, M.; Reynaud, R. Anal. Chem. 1980, 52, 2293-8.
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49-5 1. 1980, 13, 1625-8.
(G15) Knopp, H.; Tenner, R.; Truempler, G. SYSpurRep. 1981, 19, 163-7. (17) Van Houwellngen, G. D. B. Analyst (London) 1981, 106, 1057-70.
(G16) Kroschwltz, H.; Niklas, 6.; Noack, R.; Tenner, R.; Truempler, G. 146, (18) Igarashl, S. Mlzu Shod Gljutsu 1981, 22, 697-701. Chem. Abstr.
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Food
Arthur K. Foltr," James A. Yeransian, and Katherine G. Sloman
General Foods Corporation, Central Research Department, White Plains, New York 10625

This review is focused on the time interval from October standardization and comparison purposes. Allvin (1P)
1980, which was the end of our last report (24P),to October presents a review on uses of NIR in determining various food
1982. Once again, we have tried to preferentially cite domestic components and Kaffka (12P)describes the applications of
and the more widely circulated foreign journals over less ac- computer-assisted NIR to measure the ripeness, total solids,
cessible journals when work of a similar nature has been and acid content of cherries, apricots, and plums, the amounts
reported. Recent publications of possible interest to the food of protein and fat in pasta, the ethanol content of wine, and
analytical chemist for general reference are the eighth edition the quality of pork and beef. NIR techniques are also de-
of Pearson's Chemical Analysis of Foods (7P),Develo ments scribed for the determination of fat, protein, and carbohydrate
in Food Analysis Techniques-2 (17P),and the puhished content of cocoa powder (13P) as well as for the fat, protein,
proceedings of the first European Conference on Food and water content of pasta products (15P)and cheese (9P).
Chemistry which dealt with recent developments in food Osborne et al. (22P) report on the application of NIR for
analysis (4P). Available standard reference materials for use analyzing flour for protein, moisture, particle size, color, and
in the determination of nutrients and trace elements in plants starch damage. NIR has also been applied to the multicom-
and agricultural food products are given by Alvarez (2P)and ponent analysis of meat products (5P, 6P)sunflower seeds
standards for the analyst are also discussed by Watson (27P). (14P),and wheat, soybean, pork, and fresh potatoes (1IP).
The proceedings of a nutrient analysis symposium presented Shenk et al. (23P)have evaluated a NIR system for estimating
at the 93rd annual A.O.A.C. meeting have been published the protein, in vitro dry matter disappearance, acid-detergent
(25P)which described the state of the art for routine nutrient and neutral-detergent fiber, cellulose, and calcium, phos-
analysis of foods. phorus, and potassium in forage and grain.
A great deal of interest and activity have been noted in the
development of methods which make use of near-infrared ADDITIVES
reflectance spectroscopy. These methods are rapid, lend Ion-pair liquid chromatographicmethods for food additives
themselves well to automation, and are often reported to be of various types were discussed by Cornet et al. (11A) in a
as accurate as the more conventional methods used for chapter on chromatographic application. Faugere (14A) re-
I64R 0003-2700/83/ 0355-1 64R3$06.50/0 0 1983 Amerlcan Chemical Soclety
FOOOS

(57A). Archer (3A) extracted a l l a h from oils with methanol


before HPLC with 280-nm 8 V detection.
Holley et al. (24A) measured sorbic acid in salami by an
isooctane extract ct
alternate wavelen h correction to the UV absorbance of an
still had some spice interference. Na-
kayama et al. (48A) specified a DEGS/H,PO, GC column to
avoid interference to sorbate in miso analysis. Other studies
GOA) showed that ethyl oleate was the interferant in GC
measurement. Fukasawa et al. (29A) adapted a wine-sorbic
acid method to other foods that utilized UV absorbance after
bromination. GC and colorimetric methods for processed
compbr i;c and LC' peak ribs stored on cheeses were compared by It0 et al. (30A)who found that the
dlsk. Organlrslional acliv~les are ACS. AOAC thiobarbituric results came out high due to interfer-
ASTM. E-19,and AOAC. ences. Werner et al. (67A) favored a steam distillation, UV
scanning approach for analysis of low sorbate concentrations
in cheese. Parks et al. (55A) methanol-extracted citrus peel
to determine sorbate before cleanup and HPLC to achieve
a 0.5 ppm detection limit. A part-per-million of sorbic acid
in wine was detectable by using TLC on polyamide in work
by Chretian et al. @A). A way to alleviate interferences to
sorbic acid when applying the offical Japanese GC methqd
to wines was published by Matsukawa et al. (45A). Sorbic
and benzoic acids in drinks were simultaneously determined
by HPLC. using a perchloric acid/2-propanol/water mobile
phase by Collinge et al. (9A). HPLC conditions to optimize
the separation of benzoic and sorbic acids from sauerkraut
and liquid foods were given by Froehlich (Z6A). Horinopuchi
et al. ( E A ) made use of dialysis before ether extraction and
GC to analyze for sorbic acid and saccharin at the same time.
Fang et al. (Z3A) varied tetramethylammonium salt concen-
trations to adjust their ion-pair HPLC separations of benzoate,
sorbate. and saccharin.
The trifluoroacetates or heptafluorobutyrates of gallates
and hydroxybenzoates were prepared by Bajardi et al. (5A)
methodology for preservatives in foods. Collinge
found that gradient elution facilitated separations
of sorbates, benzoates, salicylates, and hydroxybenzoates in
mayonaise when using RP-18 columns. Hydroxybenzoate
esters extracted from processed meats were quantified by
direct HPLC of CH,CN extracts in work by Perfetti et al.
(56A). Flores et al. (Z5A) effected a preliminary separation
of preservatives from meat by the TAS technique before their
TLC separations. Rubach et al. (60A) reported isotacho-
phoretic preservative separations in less than 15 min on water
extracts of baked goods.
Galensa et al. (20A) formed benzoyl derivatives of p-
hydroxybenzoic esters for normal and reversed-phase HPLC
as well as GLC analysis of complex food matrices such as
mustard. Benzoic and vanillic acids down to the low parts-
per-million level in soy sauce were measured by Kihara (%A)
who cleaned up the sample solution with NaHCO,-MeCI2
viewed HPLC methods for food preservatives. A multitech- partition before HPLC. Kitada et al. (36A) pursued ethyl
nique procedure for elucidating types of antioxidants in oils ether extraction from soy sauce as preliminary separation
using TLC, column chromatography. and TMSGC was given before HPLC of saccharin, benzoic acid, and p-hydroxy-
by Nakazoto et al. (49A). Van Peterghem et al. (65A) used benzoate esters. Different initial separations such as ether
a n elaborate TLC method with three solvent systems and two extraction and steam distillation were examined by Ogawa
adsorbants to separate 11 fat antioxidants. Wyatt (68A) et al. (52A) in attempts to differentiate natural and added
studied the precision of his CH,CN extraction-GC method benzoates in ginseng tea and bamboo shoots. Results of
for oil antioxidants over a 2-week span. Min et al. (47A) collaboratively studying the Karasz methods for sulfites,
employed a setup to sweep off antioxidants that they had benzoates, sorbates, ascorbates, and blood added to beef were
assembled earlier for volatile flavor compounds in oil which reported by Maxstadt et al. (&A), with good agreement for
involved trapping on the demounted GC column. Fry (Z7A) all but the latter found. A headspace GC method using flame
showed that conversion of TBHC),to tprt-hutvlnuinone WRS
~ ~ ~~ ~~~~~~~ ~~~~~~~~~ ~~~~
~ ~ ~ ~~~
photometric detection for SO2 was employed by Hamano e t
the cause of low recoveries in GC analysis. Austin et al. (4Aj al. (23A) for various foods. Isshiki et al. (29A) reported their
analyzed TRHQ by GC after CH,CN extraction hy cnnverting version of a direct injection GC method for propionic acid in
it t o the TMS derivative. R H A and R H T were measured bakery products. The p-nitrobenzyl derivative of propionates
down to microgram levels by Maruyama et al. (43A) who was formed by Takasuki et al. (64A) after water extraction
converted the latter to a cresol before reacting both to hep- and before GC measurement in a method for bakery goods.
tanuorobutyric esters for EC GC. Masoud et al. ( M A )applied Bread was analyzed for bromate by Oikawa et al. 6 4 A ) using
fluorescence, UV, and electrochemical detection to antioxidant suppressed ion chromatography with a borate buffer. Ally-
species separated by isocratic HPLC. Brieskorn et al. (6A) lamine traces from allyl isothiocyanate decomposition were
found a twofold increase in sensitivity possible by determining visualized by fluorescence of its dansyl derivative after TLC
phenolic antioxidants and tocopherols with a rotating glassy separation in a paper by Kostyukovskii et al. (37A). Burk-
carbon voltammetric instrument. Sakurai et al. (6ZA) de- hardt (7A)gave a qualitative test for 3-(5-nitro-2-furyl)acrylic
termined BHA and BHT in fish by pentaneCH,CN partition, acid in wines using absorbance at 365 nm after removing
Florisil cleanup, and GC separation. Spark (62A) used alu- phenolics with PVP from red wine. An AOAC method was
mina columns with UV detection and colorimetric tests for modified by DeSiena et al. (ZZA) to function better a t low
methods fast enough to detect ethoxyquin in fish meal in a nitrite levels in fabricated foods. Suzuki et al. (31A)utilized
factory environment. Ethoxyquin at below 100 ppm was found ion exchange isolation before electrophoresis of EDTA as an
in spices by using reversed-phase HPLC by Perfette et al. iron complex.
ANALYTICAL CHEMISTRY. VOL. 55. NO. 5, APRIL 1983 i0SR
FOODS

Methods using GC for examination of emulsifier compo- anhydride was made detectable in olive oil by Amelotti et al.
sition were reviewed by Haken (22A). A staged procedure for (7B)using a colorimetric test. Sengupta et al. (19OB)could
systematically detecting emulsifier additives not allowed in detect oxalic acid in oil by reducing it to glycolic acid and
Switzerland was published by Martin et al. (42A) who em- developing a color with phenylhydrazinium chloride.
ployed column, thin-layer, and gas chromatographic separa- Adulterated peanut oil was shown to contain cyclopropenoic
tions. Thin-layer methods for 19 different emulsifiers were or cyclopropanoicfatty acids by Bianchini et al. (17B)using
studied collaboratively by Martin (41A). Ethoxylated capillary GC of methyl esters. The denaturant denatonium
monoglycerides in bread were measured gravimetrically by benzoate was detectable in rapeseed oil when Damon et al.
Lawrence et al. (40A) after precipitation with Ba2+ and (48B) separated it on a bonded-cyano HPLC column. Car-
phosphomolybdate. Inoue et al. (28A)separated the tartaric bon-13 to carbon-12 ratios were studied by Bricout et al. (25B)
trimethylsilyl compound by GC to determine diacetyl tartaric of vanillin isolated from natural vanilla and synthetic sources
esters added to coffee creamers. Normal phase HPLC sep- to assess adulteration. Juergens (113B)separated vanillin and
aration allowed Hurst et al. (26A) to quantify lecithin in 4-hydroxybenzoic acid by HPLC to evaluate their ratio as an
chocolate after CHC13 extraction and Sep-PAK cleanup. authenticity marker. y-Lactones along with vanillin were
Kundu (39A)reported being able to detect 2 pg of silicone found in enhanced coconut flavor vs. only 6 in an investigation
oil in vegetable oil by silica gel TLC. by Pflannhauser et al. (162B). Petrus et al. (160B) reviewed
The methylation of saccharin with diazomethane was methods to detect citrus oil and juice adulteration. Wild et
studied by Ishikawa et al. (70A)who gave conditions to control al. (231B)detected Tagetes extracts in orange oil by HPLC
the ratios of N-methyl and 0-methyl derivatives. Takatsuki separation of xanthophyll diesters. A TLC method for toxic
et al. (63A) methylated saccharin with CH31 and a phase muscarine and muscimol from poisonous mushrooms mixed
transfer catalyst to avoid diazomethane hazards. Noda et al. with edible ones was published by Stijve (199B).
(51A)analyzed milk products for saccharin by flame photo- Large amounts of work still appear on developing and re-
metric GC after dialysis, solvent extraction, and methylation. fining methodology for food mycotoxins. Honvitz et al. (101B)
An amino acid analyzer permitted Vesely et al. (66A) to discussed the considerations necessary for quality assurance
measure L-a-aspartyl-L-phenylalanine methyl ester (APM) in in trace analysis for food contaminants and toxins. The IU-
drinks down to 20 nmol. Prude1 et al. (59A)determined Usal PAC (107B) reviewed methods for mycotoxin analysis with
(APM HC1) in dairy products with a modified amino acid emphasis on feeds. Crosby (46B)reviewed cleanup procedures
analyzer instrument. Grosspietsch et al. (21A) found they applicable to dyes, mycotoxins, and polycyclic aromatic hy-
could directly inject fiitered water extracts of foods onto a (2-18 drocarbons. Literature from 1965 to 1980 was reviewed by
HPLC column to determine acesulfam-K with tetrabutyl- Lee et al. (128B)that dealt with TLC methods for 17 myco-
ammonium HS04 present in MeOH/HzO mobile phase. toxins. Levi (131B)discussed studies on the likelihood and
Kenndler et al. (34A)employed isotachophoresis to measure analysis of mycotoxins in coffee. Stoloff (200B) reviewed
glutamate, guanosine 5’-monophosphate, and inosine 5’- methods for many toxins in foods. Weber (226B) covered
monophosphate in food aqueous extracts. A fluorimetric mycotoxin methodology based on TLC and HPLC separations.
measurement of monosodium glutamate following fluoresca- Minicolumn techniques for screening for mycotoxins were
mine reaction was used by Ang et al. (2A)for noodle and snack listed by Holaday (93B). Issaq et al. (108B)listed aflatoxin
analysis. Kato (33A)separated glycyrrhizinate from tartrazine Bl! Bz, G1, and Gz separation conditions on six commercial
and p-hydroxybenzoate in foods by HPLC on a Zipax SAX silica gel plates. The advantages of homogeneity and solvent
column and 254-nm UV detection. Yamada et al. (69A) economy were stated by Whitaker et al. (230B)who favored
monitored their HPLC effluent at 250 nm for reversed-phase a water slurry method of extracting aflatoxin from peanuts.
HPLC of glycyrrhizinic acid. Ethyl vanillin in chocolate and Cohen et al. (43B)separated TFA reaction products of afla-
syrup was extracted with water ethanol/acetic acid before toxins extracted from corn and feeds with fluorescence HPLC.
HPLC separation by Hurst et a[ (27A). Postal et al. (58A) Davis et al. (49B)gave modifications to the fluorimetric-iodine
method for screening for B,. A comparison of HPLC and CD
methods for aflatoxins in corn and nuts led DeVries et al.
(52B) to consider the former (TFA-HPLC) equivalent. A
micro-ELISA (enzyme linked immunosorbent assay) was re-
ported by Biermann et al. (18B)to be rapid for B1 in food.
El-Nakib et al. (58B)had earlier studied ELISA and compared
quinine from drinks and drugs with results that agreed with it to a solid phase RIA, finding the former more reliable for
fluorometric methods. Coatings of coumarone-indene resin B,. Brumley et al. (28B)confirmed aflatoxins B1 and M1 by
on citrus fruits were determined down to trace amounts with negative-ion chemical ionization MS. Francis et al. (63B)gave
two-development TLC in a paper by Fujinuma et al. (18A). their HPLC procedure for B1, Bz, G1, and Gz that monitored
Iwaida et al. (32A)analyzed beverages for added taurine using fluorescence in a silica gel packed cell after a normal-phase
an ion exchange column and 1% H3P0 mobile phase. The silica column separation. Friesen et al. (67B)had data from
presence of caramel color was affirmediy measuring 5-(hy- a check sample program that showed no significant differences
droxymethyl)-2-furaldehydein a mixture of various flavoring between BF, CB, EEC, and HPLC methods for aflatoxins in
materials and ingredients by Alfonso et al. ( I A ) . peanut meal and corn meal. Shotwell et al. (192B)evaluated
the Holaday-Velasco and modified Holaday minicolumn
ADULTERATION, CONTAMINATION, methods and found the former superior for peanuts, producing
DECOMPOSITION no false positives. McKinney (139B)employed a silica Sep-
The use of GLC separations to elucidate adulteration of fats PAK as a first stage cleanup of a toluene-CH&N solution
and oils was reviewed by Prada Rodriguez et al. (164B). of cottonseed extract and then went to minicolumn, TLC, or
Gegiou et al. (73B)analyzed oils for the 2-position fatty acid HPLC measurement. Haghighi et al. (83B)analyzed pistachio
to detect reesterification. Fincke (62B) discussed the limi- nuts for Bl and G1 by HPLC separation of their TFA-pro-
tations of triglyceride analysis to detect cocoa butter adul- duced fluorescent derivatives. A method for spices by Awe
teration. Glyceryl ethers, separated as unsaponifiable matter, et al. (13B) used a 10-pm silica gel HPLC column and a sil-
were used by Wijsman et al. (232B) to find beef fat in pork ica-packed fluorescence flowcell. Wei et al. (227B)used HPLC
fat. Several workers applied different techniques to detect separation after Sep-PAK and TLC cleanups for aflatoxins
fatty acid anilides and aniline in edible oils mixed with de- in soy sauce but found them unstable in that food. A com-
natured oil. Wheals et al. (229B)separated unusual compo- parison of methods led Trucksess et al. (212B)to consider the
nents by SEC before TLC, IR,and MS identification. Luckas AOAC cottonseed and ginger ones suitable for sunflower seed
et al. (133B)monitored GC fatty acid separations for unusual meal, but not the peanut method. Stubblefield et al. (201B)
peaks and also separated aniline and anilides by HPLC. Stahl investigated aflatoxin measurement in animal tissues and
et al. (197B) employed a TAS procedure to transfer aniline found that two-dimensional TLC (AOAC 26.A14C) gave good
to a TLC plate and then reacted it with fluorescamine. Vioque recoveries. Hurst et al. (105B)deliberately contaminated cocoa
et al. (222B) visualized their TLC separations with p-di- beans to test methodology for B1, GI, Bz,and Gz that used
methylaminocinnamaldehyde. Jeuring et al. (111B) used reversed-phase HPLC, with UV and fluorescence detection.
electron capture GC for 2,4,6-tribromoaniline after saponi- A composite method for six mycotoxins based on HPLC
fication and bromination of anilides. The adulterant maleic was described by Chaytor (38B)that could detect 1ng of each

166R ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983


FOODS

per injection. Roberts et al. (17OB)scaled down the EEC The analysis of natural and synthetic hormone levels in
method for B1 using TLC and found that it was applicable foods and feeds using HPLC was reviewed by Jaglan et al.
to ochratoxin A analysis for simple samples. Kleinau (120B) (110B).Purdy et a1. (166B)added tritiated progesterone to
discussed BF, derivatization of ochratoxin A directly on TLC sample extracts before gradient HPLC on a Diol column with
plates. The electrochemicalbehavior of trichothecene toxins UV and radioactivity effluent measurement and separated
was related to the unsaturated a,p keto group by Palmisano progesterone and Len metabolites of it. An enzyme immu-
et al. (166B) who measured deoxynivalenol (Vomitoxin) by noassay for progesterone was described by Arnstadt et al.
DPP and also GC (after silanization). Sano et al. (17RB) (12B)who applied it to milk. Veal was analyzed for stilbene
reacted trichotheceneswith nicotinamide and %acetylpyridine derivatives by radioimmunoassay (RIA) as well as GC-M8 by
to measure them fluorimetrically on TLC plates. Scott et al. Brunn et al. (30B) who discussed the relative merits of the
(184B) detected the heptafluorobutyrlsilyl ether of deoxy- methods. Gauch et al. (71B) examined foods for synthetic
nivalenol by IEC or single-ion MS after GC separation. stilboestrols by separating dansyl derivatives by silica gel 60
Schweigbardt et al. (182B)gave separate HPLC schemes for TLC followed by an alumina TLC step or else HPLC for
separating the aforementioned toxin and zearalenone from confirmation. A RIA procedure for 17-P-oestradiol in rnilk
food. A systematic approach to detect ten Fusarium toxins or plasma was detailed by Glencross et al. (79B). Detection
using Florisil and XAD-4 column purification before TLC and of oestrogenic hormone traces in meat with an electrochemical
GC was given by Kamimura et al. (116B). Ilus et al. (106B) detector scanning HPLC effluent was demonstrated by
followed kieselgel TLC with high-performance TLC in a Frischkorn et al. (69B)who proportioned lithium electrolyte
method for Fusarium toxins in grains. Suzuki et al. (203B) into the mobile phlase.
capitalized on the EC response of butenolide to create a GC Penicillin traces in milk were detected down to 10 ppb by
method for this toxin. Radioimmunoassays for T-2 toxin were Miura et al. (142B) with an enzyme immunoassay using
reported by Lee et al. (130B)in milk and (129B)in corn and fluorescencedetection. Mochalov et al. (143B)discussed GC
wheat. Pestka et al. (158B)developed an ELISA test for 'I?-2 EC and TLC methods for penicillin in milk. A scheme to
toxin that could detect 2.5 pg in 2 h. Chaytor et al. (40B) identify penicillin, ampicillin cephapirin, and cloxacillin was
analyzed for T-2 toxin in corn by conducting GC-MS sepa- presented by Herbst (92B) based on an agar-well diffusion
ration-monitoring at m/e 350 and 436 after trifluorosilylation. bioassay. Nose et al. (148B) reported a method for multi-
A minicolumn screening test for aflatoxin M1 in milk was synthetic antimicrobial detection in meat products based on
described by Holaday (94B) that took 10 min. Friesen et al. selective ion exchange and Florisil adsorption, desorption, and
(68B)had check sample results for M1 in milk that showed GC or fluorescence measurement. Hoshino et al. (100B)
better reproducibility for labs using HPLC methods. Lafont methylated clopidol with diazomethane after extraction firom
et al. (127B) gave their TLC (UV) method for MI in milk chicken and eggs and measured residues with EC GC. Ornori
powder that included a column cleanup stage first. An in- et al. (152B)also performed diazomethane methylation and
terference to HPLC analysis of M1 in milk originating from EC GC, but confirmed clopidol with GC-MS. Turkey was
citrus waste fed to cows was noted by Price et al. (165B). examined for iproriidazole and its metabolite by Garland et
Fremy et al. (66B) presented details of their reversed-phase al. (70B) with GC-MS on a Silar 1OC column.
HPLC-fluorescence method for M1 in milk products and Methods for sulfonamidesin foods and feeds were reviewed
confirmed identity by 'TFA reaction and rechromatography. by Horwitz (9823)who called for more collaborative study on
Pestka et al. (159B)ran both radioimmunoassay and ELISA the chromatograplhic ones. Horwitz (99B) also discurised
tests for M1 in milk and found the latter more specific and performance limitations of sulfonamide residue methods,
sensitive. Tripet et al. (211B)separated several aflatoxins in noting that the Bratton-Marshall is too insensitive for the
milk products by TLC, using simple one-dimensionalsystems regulatory limit. HPLC separation with electrochemical de-
for milk and triple-direction development for complex foods. tection gave Alawi et al. (5B)detection limits of 10 ppb in milk
Van Egmond et al. (2Y6B) confirmed B1 and MI aflatoxins for sulfonamides. Nukiyama et al. (150B)used UV absorption
on TLC plates, reacting the spots with TFA and developing at 260 nm for HPLC detection after first cleaning up sulf-
in another direction. Biondi et al. (20B) employed a re- anilamide traces on a silica gel column. Vilim et al. (221B)
versed-phase TLC separation in two directions with visual screened pork for sulfamethazine traces by Bratton-Marshall
estimation of MIfrom milk. and HPLC methods, confirming positives with TLC. Thomas
et al. (207B)analyzed pork for this drug, doing a fast screen
Penicillic acid was converted to a fluorescent derivative &r on a TLC plate that was then visualized with fluorescamine.
two-dimensional TLC developmentby Ehnert et al. (56B)who Suhre et al. (202B)added carbon-13 labeled sulfamethazine
could estimate 5 ng in a spot. Hanna et al. (84B)examined to pork extracts and ratioed 12Cdrug peaks to those with 13C
chicken meat and organs for this toxin using HPLC and by GC-MS. Parks (157B)screened for the drug by ion-]pair
254-nm absorption. Cocoa beans were analyzed for patulin extracting with tetrabutylammonium hydroxide before TLC.
and penicillic acid by Chaytor et al. (39B) who employed Matusik et al. (138B)found the Manual and Steller method
GC-MS for the TMS volatile derivatives. Seafood toxin satisfactory for sulfamethazine metabolites after some mod-
methods were reviewed by Ragelis (167B). Shoptaugh et al. ification. That method-Manual et al. (135B)-involved
(191B)modified the Bates fluorimetric procedure for paralytic extraction, diazomethane methylation, and EC GC mea-
shellfish toxintg to assay clams and mussels. Cereals were surement. Malonski et al. (134B)compared GC, GC-MS, and
examined for citrinin by Nakazoto et al. (146B)whose scheme colorimetricmethods for pork samples, finding GC-MS more
used solvent partition and fluorescence spectrophotometry. definitive. Honey was analyzed for sulfathiazole residuecg by
Moldy rice was extracted with acetonitrile-water by Schmidt Argauer et al. (10B)with HPLC at 294 nm following a silica
et al. (180B)and measured for sterigmatucystinby HPLC with gel column cleanup. Juergens (115B)also reported an HF'LC
246-nm detection. Satratoxins G and H in cereals were sep- separation by using ion pairing for sulfathiazole and a H3P-
arated on Partisil PXS 5/25 with 254 nm absorbance detection 04-CH3CN mobile phase for chloramphenicol. Hollstein et
in a paper by Stack et al. (196B). Engstrom et al. (59B) al. (96B) determined chloramphenicol in milk by EC GC of
discussed losses of Rubratoxin B due to sample handling and its TMS derivative.
gave an HPLC ieilica column method. Heisler et al. (87B)used Antibiotic residue testing in milk was reviewed by Billon
Cla reversed-phase chromatography to separate Alternaria (19B). A method for levels of 50 ppb oxfendazole in milk was
toxins, monitoring at 324 and 278 nm. Lafont et al. (126B) published b Tsina et al. (213B)who conducted a reversed-
could separate PR toxin by direct TLC or else convert it to phase H P L 8 separation. Tetracycline drug resides in honey
an imine derivative before TLC, measuring both species after were detected in H[PLC effluents at 272 or 357 nm in work
further conversion to H fluorescent derivative on the plate. by Juergens (114B). Ivermectin levels in cattle and sheep were
Tenuazonic acid was extracted from tomato paste by Scott followed over time using HPLC-fluorescence methodology by
et al. (183B) who did paired-ion HPLC or ion exchange sep- Tway et al. (215B). Alykov (6B)determined aminoglycoriide
aration after solvent partition cleanup. Pyrrolizidine alkaloids antibiotics in milk and biological fluids by extraction and
in goats milk were converted to retronecine first and then fluorimetry. Vancomycin residuals in cooked lobster meat
derivatized to the heptafluorobutyrates before EC GC by were traced by Herbst (91B)using bioautography. Traces of
Dienzer et al. (50B). These compounds were also separated xylazine in foods were determined down to 90 ppb by Rogaitad
by reversed-phase HPLC and confirmed by MS and GC-MS et al. (171B) using packed and capillary GC with N-P (and
of TMS derivatives in a study by Dimenna et al. (53B). flame ionization detectors. Furazolidone in fowl and cattle
ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983 167 R
FOODS

was measured by Heotis et al. (9OB)by multiple development veloped by Joe et al. (112B),cleaning up an isooctane extract
TLC after solvent partition cleanup. Winterlin et al. (233B) on alumina before HPLC with UV absorption and fluorescence
reported sensitivity to 0.5 ppb for this drug in turkey with detectors in series. Gertz (74B) used a nonionic detergent in
their HPLC procedure. Egg yolk and albumin were analyzed petroleum ether to extract 3-4-benzopyrene from food, and
by Taylor et al. (206B) for xylonidine by means of capillary then complexed it and other PNA’s with caffeine-formic acid
GC-MS and levels were followed during the time after before a column cleanup, HPLC, and TLC. Kolarovic et al.
treatment. Wood et al. (235B) reported modifications to a (121B)used caffeine complex formation to extract PNA’s from
DPP electrochemical method for nicarbazin in chicken that vegetable oils and ultimately separated them by capillary GC
functioned to detect the 0.1 ppm regulatory level. Sakano et after TLC group segregation. The Gertz procedure for PNA
al. ( I 76B) used HPLC to monitor residues of diaveridine in compounds in smoked meat and fish was extended to fatty
chicken eggs and meat and could also measure sulfa- foods by Van Heddeghem et al. (217B) using caffeine com-
quinoxaline with the method. Meat was assayed for traces plexation and cleanup before HPLC with fluorescence de-
of oleandomycin by Rutczynska-Skonieczna (174B) who sep- tection. Sagredos et al. ( I 75B) gave details for a TLC sepa-
arated the drug by two-dimensional TLC. This author (173B) ration that included a preliminary caffeine complexation of
also used 2-D TLC for ethopabate residues in eggs. Bluethgen PNA’s. Tonogai et al. (210B)published a rapid procedure
et al. (21B) derivatized and determined several fasciolicides for benzo[a]pyrene that used a fluorimetric base line con-
in milk by GC. Amprolium traces in chicken and eggs were struction after alumina cleanup. Vassilaros et al. (219B)ex-
measured by Petz et al. (161B)with N-specific GC after a tracted PNA’s from fish and fractionated them on alumina
preliminary distillation as picoline. to separate aliphatics and S- and N-containing moieties and
Nitrosamines are among the organic species whose elec- then performed further GPC or capillary GC-MS separations
trochemistry was reviewed by Bratin et al. (24B). Hotchkiss for identity. The history and analysis of polychlorinated
(102B) reviewed the advances in separation and specificity biphenyls (PCB’s)were reviewed by Cairns et al. (33B). These
for nitrosamine analysis in foods over the past decade. Klein authors (34B) compared GC-MS and EC-GC methods for PCB
et al. (119B)discussed nitrosamine literature methods for food measurement and discussed the superior freedom from in-
and beverages. Sen (187B) reviewed TLC methods for ni- terfering compounds with chemical ionization MS detection.
trosamines. Walters (224B) also presented a short review on A splitless GC capillary separation with electron capture
N-nitroso compounds in food. A method for N-nitrosodi- detection was the basis of a method for PCB’s in milk fat by
methylamine (NDMA) in malt beverages was described by Tuinstra et al. (214B). Kuehl et al. (124B)examined tissues
Hotchkiss et al. (103B)which introduced a methylene chloride for chlorophenols and PCB’s using chemical ionization neg-
extract into a GC-TEA system without cleanup. A beer ative-ion MS after GPC or steam distillation cleanup. Morton
method by Andrzejewski et al. (8B)distilled first from caustic et al. (145B) analyzed for pentachlorophenol (PCP), penta-
and partitioned NDMA into solvent from the distillate before chloroanisole, and the 2,3,4,5 and 2,3,5,6 isomers of tetra-
GC-TEA. Aitzenmueller et al. (4B)discussed possible artifacts chlorophenol ethylating the phenols before EC GC in a me-
in beer analysis that might be formed. Mark1 et al. (136B) thod for fat samples. PCP and 2,3,4,6-tetrachlorophenol were
compared nine techniques for NDMA analysis in beer and extracted from gelatin by Stijve (198B)who chromatographed
brewing materials, finding that direct CHzClz extraction them on a DEGS-H3P04 column with EC detection. Brugel
bettered distillation. Sen et al. (188B) treated beer with (27B)converted PCP to the acetate before EC GC in a method
sulfamic acid and HC1 before distillation, CHzClzextraction, for gelatin. Borsetti (22B)analyzed milk and cattle blood for
and GC TEA analysis. Owens et al. (154B) constructed a PCP residues by extraction and EC GC on an SP 1000-H,P04
liquid nitrogen controller to regulate cold trap temperatures packed column. Mason jar lids and preserved food were
in a TEA analyzer. Verhagen et al. (220B)reacted NDMA analyzed for PCP by Heikes et al. (86B)who methylated to
to a secondary amine which when derivatized with 443-7- pentachloroanisole before EC GC. PCP residues in mush-
nitrobenzofuran was measured by fluorescence HPLC. Cross rooms were determined by Schoenhaber et al. (181B) using
(47B) reviewed methods for volatile nitrosamines in bacon. steam distillation, extraction into CHzClz,and either GC after
Owens e t al. (153B) gave improvements to the mineral oil acetylation or direct HPLC. Residues of 2,3,7,8-tetrachloro-
distillation method for volatile nitrosamines in bacon fat. Sen dibenzodioxin in goats milk were detected down to the low
et al. (189B) gave a fast liquid-liquid extraction for volatile part-per-trillion level using GC-MS and monitoring the 321.9
nitrosamines in bacon fat, which were then injected into a m / e ion in work by Raisanen et al. (169B). Brumley et al.
GC-TEA. Massey et al. (137B) demonstrated that the low (29B) monitored 12 ions and calculated ratios in a low-reso-
flows of microbore HPLC could make an LC technique lution GC-MS method for the 2,3,7,8 compound in fish.
amenable to a TEA analyzer. Nonvolatile nitrosamines were Aitzenmueller et al. (3B)analyzed milk for 2-hydroxybiphenyl
detected by Samuelsson et al. (177B)using DC, normal pulse, using an Extrelut column extraction and normal-phase silica
and differential pulse voltammetry. Hotchkiss et al. (104B) HPLC after elution and concentration. The presence of 4-
used a combined GC-TEA and GC-MS system to confirm the nitroso- and 4-nitrophenols in smoked fish was shown by Borys
identity of volatile nitrosamines separated on packed and (23B)who separated them from alkylphenols and phenol by
capillary columns. Havery et al. (85B)gave a fast method for HPLC after XAD-4 concentration. Ivie et al. (109B) inves-
volatile nitrosamines in milk consisting of CHzClzeluates from tigated carrots for psoralen presence using HPLC techniques
a celite column directly injected into GC-TEA. but found none. Wells et al. (228B) analyzed fish for con-
Gilbert et al. (75B)presented a review on advances in trace tamination with “Eulan WA New” by methylating extracts
diet constituent analysis, covering nitrosamines, dioxins, and with CH31and tetrabutylammonium hydroxide before EC GC.
mycotoxins, emphasizing MS methods. Dougherty (55B) A literature review on the migration of packaging material
reviewed trace analyses for contaminants that are facilitated components into foods led Niebergd et al. (147B)to speculate
with negative-ion chemical ionization MS. Hydrocarbons due that model systems should predict potential migration from
to pollution could be differentiated by Berthou et al. (16B) partition properties. Gilbert et al. (76B)reviewed headspace
from those of biological origin by diastereomer distribution GC methods used to measure residual monomers in plastic
as determined by glass capillary GC with MS detection. packaging. Ettre (61B)reviewed the purge and trap method
Adachi (1B) employed GC-EI-MS to fingerprint crude oil as a way of extending detection limits for residual printing
contamination of oysters by poly(methylnaphtha1ene) and solvents in packaging film, among other applications. Hol-
poly(methy1phenanthrene)detection. Kwan et al. (125B)were lifield et al. (95B) gave a multiresidue scheme wherein
able to establish trends relating to mussel proximity to pol- headspace vapors from packaging were compared to com-
lution sources by applying pattern recognition routines to puter-stored retention times. Colli (44B) discussed common
hydrocarbon composition. Organic sulfur species in clams and solvents and GC methods for packaging ink volatiles. A
eels were identified by GC-sulfur photometric detection and method for volatiles originating from food packages using
GC-MS by Ogata et al. (151B)who developed information on empirical headspace calibration was presented by Eiceman
marker compounds for crude oil pollution. Adachi (2B)de- et al. (57B). Habegger et al. (80B) gave a heated headspace
tected poly(methylbipheny1s) using GC-MS to examine ex- method for residue solvents in packaging films that used
tracts from rice contaminated with petroleum. Min et al. cyclohexane as an internal standard. Kolb et al. (123B)
(141B)found they could measure biphenyl and phenyl ether discussed a GC “multiple headspace extraction” for printed
in oil by a purge and trap technique a t 160’. A method for films in which successive vial gas flushes are summed to ap-
polynuclear aromatic hydrocarbons (PNA’s) in beer was de- proximate total partition. Vinyl chloride oligomers were

l 6 8 R * ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983


FOODS

ether-extracted from resins and separated by SEC on Bio- in honey was quantified by Sporns (195B)by HPLC with UV
Beads or Sephadex before GC analysis with packed and ca- absorbance monitorin on a steam distillate. Kid0 (117B)
pillary columns5 monitored by FID, Hall, and MS detectors, measured formaldehyfie in fish paste by reacting steam dis-
in a study by Gilbert et al. (77B)who also used a silica LC tillates with 2,4-dinitrophenylhydrazinebefore FID-GC. Cline
separation to segregate non-C1- from C1-containing extracta- et al. (42B)formed a pentafluorobenzyl ester of the benomyl
bles. Vreden et al. (223B) attempted to quantify migrated- metabolite carbendazim to inject it into an EC GC for esti-
styrene monomer by direct GC of headspace over strawberries mation in walnuts. Grapes and wines were analyzed for im-
but found volatile aroma interferences. Styrene monomer was idazolidine-Qthione traces by Caccialanza et al. (32B) who
extracted from polystyrene-contacted foods with hexane and separated it on a reversed-phase HPLC column monitored at
reacted with bromine water to form the bromo compound by 240 nm. The toxaphene metabolite camphechlor was deter-
Novitskii et al. (149B)who then performed EC GC. Gilbert mined in milk fat b,y Cairns et al. (35B),using methane CIMS
et al. (78B)monitored m / e 104 for styrene liberated from food of packed-column GC effluent. Swallow et al. (204E) com-
heads ace and separated by packed-column GC-MS. Palla pared their GC detection procedure for tutin and hyenanchin
(155Bf also employed GC-MS for styrene traces, adding in honey to a mouse assay. A method for 4(5)-methylimidasole
deuteriostyrene to wine samples, brominating extracted mo- in food formulated with caramel color was presented by
nomer, and ratioing the 2H to ‘H fragments shown. Sponholz Yoshikawa et al. (23%) which diazotized the compound before
et al. (194B)developed a HPLC method for styrene in wines, TLC separation as a colored species. Thomsen et al. (208B)
measuring it at 254 nm in a reversed-phase effluent. Gawell determined the aforementioned caramel impurity by HPLC
et al. (72B)added a-methylstyrene before distilling foods from ion-pair separation and detection at 215 nm.
MeOH/H20 arid then performed reverse-phase HPLC. An- Roy et al. (172B) automated a uric acid method that
other version of a HPLC method by Varner et al. (218B) measured a color developed with phosphotungstic acid before
analyzed directly for the monomer by dissolving polystyrene and after immobilized uricase contact. Spice contamination
in THF, precipitating polymer with MeOH, and then injectin with uric acid was correlated to insect infestation by Brown
supernatent. Additional experiments by Watabe et al. (225Bj et al. (26B) who monitored oxygen released from a uricase
demonstrated the ability to selectively retard polar compo- reaction with a specific electrode. Wolfschoon-Pombo et al.
nents vs. styrene with CC on a liquid crystal stationary phase (234B)used a test kit that coupled uricase action on uric acid
in an electric field. Baumann et al. (14B)investigated aromatic in milk to a catalase reaction and then dehydrogenase,finally
amine migration into food-simulating solutions with electro- measuring a NADH absorbance change to estimate the uric
chemically detected HPLC separations. Traces of 2,4- and acid content. Hoover et al. (97B)discussed using jack bean
2,6-toluenedimine from food boilable pouches were measured meal as an economical source of urease. Thrasher et al. (209B)
by Snyder et al. (193B) by concentration before HPLC with tested for alkaline phosphatase in suspect particles to confirm
254-nm detection. Ardrey et al. (9B)listed extensive data on mammalian faeces. Scott et al. (185B)solvent extracted ergot
retention indices of GC-separable compounds among which alkaloids from flour with a partition cleanup before re-
were plasticizers, antioxidants, contaminants, etc. A cleanup versed-phase HPLC with fluorescence detection. Dent (51B)
for bis(2-ethylhexyl) phthalate traces in fish oil that used reported collaborative results of the operations necessary to
Bio-Bead and alumina columns before EC GC was given by separate thrips and similar insects from frozen blackberries
Burns et al. (31B). Haesen et al. (81B)studied the migration and raspberries. L h (132B) had data on a collaborative study
of phenolic antioxidants from plastic to oil with a TLC on light filth in tea. Freeman (65B) modified the procedure
technique and color development. Haesen et al. (82B) ana- for extracting light, filth from sage. This author (64B)also
lyzed dairy produds for antioxidant migration with TLC also. described a method for light filth in corn.
The sizing compound distearylcarbamoyl chloride was mea- A method for indole in shrimp was developed by Chambers
sured in olyethylene-coated papers by HPLC at 254 nm in et al. (36B)in which1 the compound is extracted with methanol
a methoif by Helmer et al. (88B). and separated on a C18 HPLC column with fluorescence de-
Zimmerlie et al. (237B) reviewed tetrachloroethylene in tection. These authors (37E) also gave a procedure that ex-
foods and proposed a distillation-GC method. A heated tracted into ethyl acetate and cleaned up on a polyamide
headspace method for halocarbons in foods was described by column before HPLC with 217-nm absorbance detectiion.
Entz et a1. (6013) who analyzed the vapors with EC GC and Cheuk et al. (41B)determined indole colorimetrically without
found variations in the vapor phase partition depending on steam distillation. Takahashi et al. (205B)measured dimethyl
the food matrix. Saxby et al. (179B) also published a vial- sulfide in incubated headspace over rice to correlate its pre-
heads ace GC technique for solvent residues due to be reg- cursor with age andl storage. Meltzer et al. (140B)develolped
ulateifby the EEC, and found that calibration slopes de- a method to detect cyclic compounds formed from polyun-
pended on matrix and CHzClzcould not be separated from saturated 1Scarboln fatty acids when soya bean oils were
coffee aroma. DiPasquale et al. (54B) experimented with extensively heated. Henion et al. (89B)analyzed for histamine
oxygen doping of nitrogen carrier gas to enhance the electron in tuna fish by capillary separation of ita TMS derivative with
capture sensitivity of CHzClzresidues in oils and liquid foods. positive ion CI MS detection.
Kolb et a1. (122B) determined residual perchloroethylene in
eggs using an OV-101 capillary column and EC detection on CARBOHYDRATES
a headspace sample. Ethylene oxide residues in food were Increased use of IHPLC for the determination of individlual
swept out by nitrogen and measured by EC GC after con- sugars is the outstanding feature of the literature reviewed
version to 2-bromoethanol on a Florid-HBr column gas in this period. It ha3 unfortunatelybeen necessary to eliminate
scrubber in spice analyses conducted by Mori et al. (144B). some articles which report similar techniques because of lack
King et al. (118B)analyzed headspace above blended grape- of space. Automatic methods for reducing carbohydrateshave
fruit by EC GC for methyl bromide residues. An electron been described by Boehringer et al. (18C) using the reaction
capture GC method by Rains (168B)separated ethylene di- with 4-hydroxybenzohydrazide and by Robin et al. (109C)
bromide extracted from flour and biscuits with hexane. Re- using tetrazolium lblue after gel chromatography and with
action products of ethylene oxide and theobromine were parallel detection with orcinol. Polyamide powder has blsen
identified by mass and UV spectroscopy studies after TLC suggested by Lehmann et al. (70C) as a means of removing
separations of cocoa extracts in a report by Pfeilsticker et al. pigments in the analysis of chocolate for sugar. The use of
(163B). Scudamore (186B)could determine 0.2 ppb residual glycerine in sodium hydroxide as a replacement for Fehling’s
2-aminobutane in potatoes with HPLC separation and B solution has been proposed by Ma (72C).A reagent con-
fluorimetric detection of the dansyl derivative. Arikawa et taining phenolphthaleinhas been used by Shahine et al. (11112)
al. ( I I B ) examined vegetables for traces of acrylamide, ex- for the indirect spectrophotometricdetermination of reducing
tracting, brominating, and finally conducting an EC GC sugars. A glucose sensing electrode using glucose oxidase, in
separation on a cleaned-up fraction. Cox et al. (45B)reported conjunction with a glassy carbon electrode, has been descrilbed
a method valid in the 10-60 ppb range for chlorobutanoltraces by Matsumoto et al. (77C)to measure glucose in orange juice.
in milk by using a combined distillation-extraction and EC Brobst et al. (21C) have reviewed three chromatographic
GC. Beck et al. (15B) derivatized 1,2,3,4-tetrahydro-1- methods for the analysis of sugar mixtures, HPLC, GC, and
methyl-&.carbolinewith pentafluoropropionicanhydride after TLC and suggest that the method chosen depends on the
extraction and measured it by monitoring single ions from nature of the sample. A minicolumn of aluminum oxide has
capillary EI-GC-MS. Phenol at low parts-per-million levels been used by Gorin et al. (46C) to clean up onion extract
ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983 ims~
FOODS

before HPLC chromatography. Iverson et al. (58C) have al. (121C) for the determination of nonreducing oligo-
compared the separation and ease of preparation for the saccharides. HPTLC using multiple developments has been
analysis of five sugars by HPLC and GLC and found the GLC applied by Nurok et al. (88C) to the separation of malto
method not applicable to all foods. After extraction with 80% oligosaccharides. Cryoscopy has been proposed by Fitton
ethanol Quemener et al. (97C) have separated four oligomers (36C) as a rapid means of determining dextrose equivalent.
from leguminous seeds by HPLC. Two detectors of mono- Methods for the determination of pentosans have been de-
saccharides separated by HPLC have been compared by scribed by Douglas (32C) using spectrophotometry after
Binder (15C) who reports finding much greater sensitivity at controlled acid treatment and by Folkes (37C) by gas chro-
188 nm than is obtained by refractive index detection. matography of the furfural produced after acid treatment.
Fluorimetricdetection of sugar borate complexes after reaction Dextran in cane juice has been determined by Li Sui Fong
with 2-cyanoacetamide has been used by Honda et al. ( 5 5 0 et al. (71C) by haze measurement before and after dextranase
in the automated HPLC analysis of reducing sugars. The mass treatment. Radley (1OOC) has edited a book on starch and
detector has been found by Macrae et al. (73C) to provide analysis of starch products. A method for starch analysis in
greater sensitivity and stability than the refractive index cereal products has been reported by Batey (12C) which uses
detector in the HPLC of carbohydrates. An amperometric thermostable a-amylases. A method for amylose in milled rice
detection technique has been used by Hughes et al. (56C) for has been submitted to international cooperative testing by
carbohydrate detection after HPLC separation. Semiquan- Juliano et al. (63C) and the effects of defatting were deter-
titative and qualitative determinations of sugars have been mined. Amperometric titration with iodate-iodide solution
described by Qureshi et al. (99C) on capillary tubes partly of starch in a dimethyl sulfoxide-water system has been de-
filled with diphenylamine hydrochloride. Near-infrared re- scribed by Voss et al. (120C)for the determination of amylose
flectance spectroscopy has been examined for its usefulness content. A calibration has been devised by Osborne et al.
in determining individual sugars in dry mixtures by Gian- (93C) which measures the degree of starch damage in flour
giacomo et al. (44C), and preliminaryresults appear promising. by near-infrared reflectance analysis, A sensitive method using
An enzyme scheme which determines D-glucose, D-fructose, @-amylase-pullulanasehas been suggested by Kainuma et al.
and D-mannose has been described by Sturgeon (113C). (64C) for the determination of the degree of gelatinization and
Various separations of sugars on chemically modified silica retrogradation of starch or starch products, and Kugimaya
gel, with bonded amino groups, have been described by Orth (68C) has proposed measuring the susceptibility of the starch
et al. (92C). Fluorodensitometric measurement has been to @-amylaseas a means of characterizingits gelatinized state.
applied by Iwakawa et al. (59C) to sugars separated on TLC GLC has been used by Mitchell et al. (81C) as a means of
plates and sprayed with ethylenediamine sulfate. Silica determinin the adipate content of acetylated distarch adipate.
columns impregnatedwith HPLC Aminc Modifier 1have been Hydroxyallyl groups in etherified starch have been deter-
used by Aitzetmueller (4C) for the analysis of carbohydrate mined by GLC analysis of the reaction products with hydriodic
mixtures such as fruit juices, jams, and syrups. Akhavan et acid, by Kawabata et al. (65C), and hydroxypropyl groups have
al. (5C) have compared the effectiveness of ion-exchan e been determined by Tsai et al. (117C) by a colorimetric
cleanup with that of lead precipitation for acids before 8 C procedure. Galactomanman in guar seeds has been analyzed
determination of sugars and find ion-exchange preferable. by McCleary (78C)using the enzyme galactose dehydrogenase.
Sugars in sugar refinery products have been determined by @-Glucanin barley has been determined by Martin et al. (76C)
Charles (25C) by HPLC using refractometric and conducto- after treatment of extracts with cellulase and enzymic de-
metric determination. Cellobiose dehydrogenase has been termination of the released glucose. An automated method
used by Canevascini et al. (24C) for the direct determination for glycogen has been developed by Haagsma et al. (47C) using
of lactose in milk and milk products. An enzyme procedure amyloglucosidase and enzymic glucose determination.
using p-D-galactosidase to hydrolyze lactulose, a series of A review of methods for polysaccharide thickening agents
enzymes to remove glucose, and then to determine the fructose in foods has been published by Scherz et al. (105C). General
as a measure of lactulose has been proposed by Geier et al. methods for these polysaccharideagents have been described
(42C). Parrish (94C) has studied spectrophotometric proce- by Pechanek et al. (95C) using electrophoresis separation, by
dures and HPLC for the analysis of lactulose and other sugars Friese (40C) using TLC, by Mergenthaler et al. (79C) using
in sugar mixtures and found the HPLC method faster and separation on DEAE cellulose columns and TLC or GLC
as accurate. Sugars and polyhydric alcohols have been sep- analysis after hydrolysis, and by Hunziker et al. (57C) using
e
arated by Angyal et al. (8C) usin HPLC on cation exchange
resins in the calcium form. TL after extraction and puri-
fication has been applied by Maier et al. (74C) to the deter-
gel permeation chromatography. This technique has also been
used by Barth et al. (1IC)for the separation of water-soluble
cellulosics. Another procedure for analysis of natural thick-
mination of esters of sugars and fruit acids in foods. A col- eners and gums has been described by Preuss (96C) using
laborative study has been conducted by Zygmunt (125C) on methanolysis and capillary gas chromatography. Gas chro-
the HPLC determination of mono- and disaccharides in cereals matography has been proposed for the analysis of thickeners
and the method has been adopted as official first action. An in milk products by Glueck et al. (45C) after separation from
HPLC technique has been developed by Brandao et al. (19C) the product and hydrolysis. Alginate in beer has been de-
to separate and quantitate mono- and disaccharides and termined by Schur et al. (107C) using a colorimetric deter-
sorbitol, using HPLC columns in tandem. Mono- and di- mination for mannuronic acid separated by TLC after hy-
z
saccharides have been anal zed by Adam ( I C ) using as
chromatography of sodium orohydride derivatives, eit er f-l
trimethylsilated or acetylated. Fluorescaminehas been found
drolysis of the gum and by Fey et al. (35C) by a similar
procedure after separation of the alginate by the use of
Sephadex G-50. Carrageenan in dairy products has been
by Chen et al. (27C) to be useful for the quantitative analysis determined by Murray et al. (86C) by fluorimetric assay with
of amino sugars and of chitin. acridine orange. Galacturonic acid has been determined by
Reviews of analytical procedures for polysaccharides have Birnbaum et al. (16C) using an enzyme method, and by GLC
been published by Aspinall (9C) and Heyraud et al. (52C). after enzyme hydrolysis and potassium borohydride treatment
High-resolution separation of oligosaccharides has been re- by Ford (39C). Oli ogalacturonic acids have been separated
ported by Scobell et al. (109C) using silver-form cation ex- by Thibault (116C)%ychromatographyon polyacrylamide gel.
change resins. Two HPLC columns in series have been used The use of m-hydroxydiphenylas chromogen forming reagent
by Fonknechten et al. (38C) to separate oligosaccharides. for anhydrogalacturonic acid has been recommended by
Three cation exchange columns, Ca form, connected in series Robertson (102C) for the determination of pectic substances
have been used by Schmidt et al. (106C) for the separation in fruits. Dissolved pectin in fruit juice has been determined
of malto, xylo, and cello oligosaccharides. Carbohydrate ol- by Meurens (80C) by iodometry of the cupric copper precip-
igomers have been separated by Cheetham et al. (26C) using itated with pectate. A method for the molecular weight
a radial compression module. Waniska et al. (122C) have distribution of pectins has been developed by Barth (1OC)
compared ultrafiltration, gel permeation, and adsorption using gel permeation chromatography. A near-infra red re-
chromatography methods for separating oligosaccharides, the flectance technique has been found by Wingfield (124C) to
latter was found to be the most efficient and effective. A be useful for the detection of cellulose in flour.
“reaction column” which converts nonreducing sugars to re- James et al. (61C) have edited a treatise on the analysis of
ducing sugars, placed after a separation column and followed dietary fiber in food covering various procedures and problems.
by a reducing sugar reagent, has been proposed by Vratny et Four dietary fiber procedures have been compared by Heck-

170R ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983


FOODS

man et al, (50C) who found the Furda method to be practical, al. (98C) and Lattanzio et al. (69C), by colorimetry by Kim
to be informative and to have acceptable precision. The details et al. (66C),and by color development after TLC by Hoehn
of this method which determines soluble and insoluble fiber et al. (54C). Zeatin and zeatin riboside have been determined
have been published by Furda (41C). Methods for analysis by HPLC by Stahly et al. (112C) after extraction from pears,
and chemical characterization of dietary fiber have been peaches, and apples.
published by Theander et al. (115C), Selvendran et al. (IIOC),
and Schweizer et al. (108C). All use hydrolysis after separation COLOR
to determine constituents of the fiber components. A SUC- Artificial and natural colors, plant pigments, and related
cessful collaborative study of the Goering and Van Soests compounds are included in this section of the Review. A
neutral detergent fiber method has been reported (6C) on six review of chromatographic and spectrophotometric methods
products. Studies of neutral-detergent fiber methods have for the determination of natural and synthetic coloring ma-
been carried out by ColWinge et al. (28C) comparing different terials has been published by King (460). The use of HPLC
enzymes, temperatures, and digestion sequences, by Roth et to separate food dyes has been described by Maslowska et al.
al. (104C)who suggest the use of p-glucanase to help filtration (510)using P1C reagent A, by Boley et al. (110)with meth-
of barley kernels, by Dovell et al. (330 who propose a method anol-H20 plus cetrimide as mobile phase, by Lawrence et al.
for fiber in oranges and other foods, and by Anderson et al. (490) using ion-plair chromatography with tetrabutyl-
(7C) who have exhaustively analyzed the dietary fiber of corn ammonium phosphate, and by Puttemans et al. (610) using
bran. Characterization studies of dietary fiber have been the same counterion. Ion-pair extraction and ion-pair (ad-
reported by Bither et al. ( I 7C) who reported the neutral and sorption TLC have been used by Van Peteghem et al. (710)
acidic composition of the alcohol insoluble residue from foods, to analyze 17 food dyes. The use of photoacoustic spectros-
by Brillouet et al. (20C) who reported on the fractionation of copy after thin-layer chromatography has been proposed by
wheat bran noneitarch polysaccharides, and by Belo et al. (13C) Ashworth et al. (40) for the determination of several food dyes.
on the analysis of pectic substances in detergent-extracted A scheme for extraction and separation of water-soluble ar-
dietary fibers. A method for characterizing lignin has been tificial acidic dyes hias been prepared by Corradi et al. (180)
described by Hedges et al. (51C) using gas capillary chro- using TLC. Ion-pair thin-layer chromatography has been
matography of cupric oxide oxidation products. Cell-wall applied by Gonnet et al. (360)to the analysis of water-soluble
polysaccharide and lignin levels have been determined by food dyes. Food colors have been determined by Fogg et al.
Riquet et al. (101C) by different methods who found that a (300) by dc voltaminetry with good precision. Polarographic
sharp separation of these polysaccharides was not obtained behavior of some azo dyes has been studied by Hart et al.
by the Van Soest methods. Modifications of the Van Soest (370) and optimum conditions for determination by differ-
methods have been suggested by Marlett et al. (75C) for the ential pulse polarography have been established. An ex-
improved determination of lignocellulose and hemicellulose. traction procedure for water-soluble colors from foods using
A method for the determination of starch in dietary fiber polyamide columnti has been proposed by Crosby (240).
sources hm been proposed by Dintzis et al. (31C) using enzyme Ion-pair extraction has been suggested by Puttemans et al.
treatments Nonstarch polysaccharides have been determined (630) to transfer dyes from water extracts to chloroform1 as
in plant foods by Englyst et al. (34C) by GLC of constituent a cleanup technique. The same authors (620) have evaluated
sugars as alditol acetates. Craddick et al. (30C) have suggested TLC, paper chromatography, and HPLC for identification of
that glass filter paper be substituted for the fritted glass dyes extracted as ion pairs and found the extraction to be
crucible in asbestos-free fiber determinations. essentially quantitative (600). Dyes after water extraction
Glycerol in wine has been determined by Ubigli (119C) after have been adsorbed on polyamide and then eluted with
oxidation to formaldehyde which is then determined as the methanol and identified by photometry on TLC by Ogiwara
3,5-diacetyl-1,4-dihydrolutidine. Components of maltitol-D- et al. (570). A system for extracting and determining dyes
sorbitol Eiyrups have been separated by Molnar-Per1 et al. in chewing gum has been described by Andrzejewska (1D) with
(82C) by GLC after trimethylsilylation. Pinitol and other identification by TLC. Ion pairing HPLC has been suggested
cyclitols have been analyzed by Ghias-Ud-Din et al. (43C) by by Hurst et al. (410) for the analysis of amaranth in licorice
HPLC with refractive-index detection. D-Sorbitol has been products. Indigo carmine has been determined by Boley et
Separated from foods by dialysis and determined by GLC by al. (120) in boiled sweets by HPLC after extraction amd
Tsuda et al. (118C). Sugar alcohols in gum have been de- cleanup on a Sep-I’AK CI8 cartridge. Tartrazine has been
termined by Oesterhelt et al. (9OC) by GLC of the TMS or determined in foods by Hurst et al. (420) by HPLC, aind
acetyl derivatives after water extraction. A modified acety- Kobori et al. (470) have studied the polarographic behavior
lation procedure has been applied by Mount et al. (84C) to of this dye for quantitative estimation in foods. Differential
the estimation of sugar alcohols by GLC. pulse polarography has been found by Fogg et al. (310)to be
Monoterpene glycosides and norisoprenoidprecursors from of use in studying the degradation of Red 10 B during pro-
grape juices and wines have been separated by Williams et cessing. HPLC haai been applied by Bdiley (50) to the (de-
al. (123C) by reversed-phase column chromatography on CIS termination of intermediates in FD&C Blue No. 2, by Cox et
bonded phase columns. Phytoestrogens from soya beans have al. (230) and by Calvey et al. (160) to similar analyses of
been determined by HPLC by Murphy (85C) using gradient FD&C Yellow No. 5, and the procedure for intermediates and
elution. Recent advances in the analysis of glucosinolates have byproducts in FD&C Red No. 40 has been submitted to
been reviewed by Olsen et al. (91C). Glucosinolates have been collaborative study by Cox et al. (220).
analyzed by Heaney et al. (48C) using gas chromatography Natural pigments have been separated by TLC on poly-
and the same authors (49C) report on the importance of the amide by Kanada et al. (450). An identification method for
derivatization conditions for the determination of indole color E 160b (oriana, annatto) has been described by Corradi
glucosinolates. Sinalbin and sinigrin have been determined et al. (200) using TLC to se arate its components. Beet
by isotachophoresis and conductometric detection by Klein pigments have been analyzed y! Bilyk (100) by preparative
(67C). Neohesperidin dihydrochalcone has been separated TLC followed by a multiple development TLC technique.
from intermediates and from alcoholic beverages by Tateo et Beetroot red, E 162, has been analyzed by TLC on silica gel
al. (114C) using liquid chromatography with gradient elution. by Corradi et al. (19.D). A fractionation technique for analysis
Stevia components in natural sweetener products have been of betalaines has been described by Bilyk (90) after extractiion
analyzed by TlLC and GC by Nakajima et al. (87C), by with ethanol, followed by spectrophotometry and TIL!.
Iwamura et al. (CiOC) by thin-layer densitometry, by Hirokado Quantitative determination of individual betacyanin pigments
et al. (53C) by silica gel TLC, and by Ahmed et al. (2C, 3C) has been achieved by Schwartz et al. (660) using HPLC, and
by HPLC! from leaf samples. Isolation and detection of sa- Schwartz et al. (670) have compared spectrophotometric amd
ponins in food have been included in a review by Oakenfull HPLC methods for quantitation and prefer HPLC. Ex-
(89C). Potato glycoalkaloids have been determined by HPLC tractable colorant in ground pepper has been determined by
by Bushway et al. (22C), by radial compression HPLC by Drdak et al. (280)by methyl ether extraction and colorimetry.
Morris et al. (83C), by a modified titration method by Caramel types have been fractionated by gel chromatography
Bushway et al. (23C), by a rapid colorimetric method by by Hellwig et al. (380) into color components, typical elution
Bergers (14C), by TLC by Coxon et al. (29C), and by fluo- diagrams facilitate classification. Cochineal has been detected
rodensitometric TLC by Jellema et al. (62C). Vicine and in meat products by Andrzejewska (20) by TLC after puri-
convicine have lbeen determined by HPLC by Quemener et fication on polyamide. Curcumin in turmeric has been de-
ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983 * 171 R
FOODS

termined by Asakawa et al. ( 3 0 )by HPLC after solvent ex- nation of alkaline phosphatase in casein has been reported
traction. Mustard has been analyzed for turmeric by Un- by Murthy et al. (26E)using a rapid colorimetric test, and
terhalt (700) by the formation of rubrocurcumin after ex- the method has been adopted as official first action. The same
traction. Saffron coloring principles have been identified by authors (27E) have studied the use of alkaline phosphatase
Corradi et al. (210) by TLC. activity in skim milk impregnated paper disks as a positive
A review of the advantages of HPLC for separating plant control standard. Improved sensitivity for alkaline phos-
pigments has been published by Schwartz et al. (650). An- phatase in milk and cream has been obtained by Linden et
thocyanins in grapes have been examined by Piergiovanni et al. (18E)by the use of additives to induce transparency (and
al. (580)using HPLC. The effect of mineral acids used during stop the reaction) and thus facilitate the colorimetricreading
extraction on the chromatographicprofiie of anthocyanins has of the end point. A colorimetric method for the determination
been described by Moore et al. (530). Postcolumn reactors of a-amylase activity in cereal products has been published
after HPLC separation have been found by Galensa (350)to by the British Standard Institution (5E). Collaborative studies
provide quantitative data for flavonoids when applied to to- have been made by Mathewson et al. (22E) on a-amylase
mato skins. Flavonoids in barley and hops have been de- analysis by three methods and (23E) on a simplified rapid
termined by McMurrough (520) using HPLC, in beer by colorimetric method for a-amylase; all procedures were applied
Delcour et al. (250)using gradient elution HPLC after column to sprouted wheat. Isoelectric focusing has been used by
cleanup, and in carrots by Yates et al. (730) using column MacGregor et al. (20E) to separate and then determine, by
cleanup and GLC. Procyanidins in wines and ciders have been using the amylopectin @-limitdextrin plate technique, a-
determined by Lea (500) using HPLC. Schemes for the amylase enzymes in germinated barley. An explanation of
separation of the flavonol glycosides of fruits have been the high falling numbers obtained when a-amylase is deter-
presented by Henning et al. (390) by HPLC with identifi- mined at bath temperatures lower than 100 OC has been of-
cation by TLC and spectroscopy. The flavanols L-epicatechin fered by Varriano-Marston et al. (33E), and the effect of
and Dcatechin have been isolated from grapes by Baranowski altitude on the falling-number value has been discussed by
et al. ( 6 0 ) using column chromatography. Hesperidin in Lorentz et al. (19E). The qualitative official test for egg
orange juice has been determined by Galensa et al. (340)by pasteurization has been compared unfavorably with the Roche
HPLC after extraction and polyamide cleanup. The flavo- Amylochrome test for a-amylase activity by Cattaneo et al.
noids rutin, hesperidin, and naringin have been determined (7E);the latter gives quantitative results. A nephelometric
in citrus fruits by Drawert et al. (270)by GLC and by column technique for predicting diastatic power in barley has been
and thin-layer separation (260). Hesperidin in orange drinks suggested by Swanston (31E) which measures @-amylase
has been determined by Sontag et al. (690) by HPLC and concentration.
amperometric detection. Bianchini et al. ( 8 0 )have separated Luciferase has been used by Ching (BE) in a rapid and
17 polymethoxylated flavones on an HPLC column with the sensitive assay procedure for ADP glucose pyrophosphorylase
use of four mobile phases. The hydroxyflavoneglycosides of in wheat seeds. Ascorbate oxidase in wheat flour has been
some spices have been isolated by Hoffmann et al. (400) by isolated and characterized by Pfeilsticker et al. (29E)using
paper chromatographyand TLC and identified by UV spectra thin-layer isoelectric focusing. A polarographic method has
and by color reactions. Separation and identification of ca- been used by Takahashi et al. (32E)to determine ascorbic acid
techins and proanthocyanidins in spices have been described oxidase inhibitor in fruits and vegetables. Rennet enzymes
by Schulz et al. (640) by column cleanup followed by TLC. have been fractionated and identified by Reimerdes et al.
Tea catechins have been separated by gas chromatography (30E) using conventional techniques (ion-exchan e chroma-
by Zaprometov (740). An automatic system for the chro- tography and electrophoresis). Martin et al. &E) have
matography of tea catechins has been developed by Nakagawa evaluated bovine rennets by using a synthetic hexapeptide;
(550). Gas chromatography of trimethylsilylated derivatives the effect of pH was studied. Chromatography on DEAE
has been used by Nagata (540)to determine flavanols in tea cellulose has been used by Collin et al. (12E) to determine
leaves. Theaflavins in tea have been assayed by HPLC by chymosin and bovine pepsin A in bovine rennets and pepsins,
Wellum et al. (720) and by colorimetry with Flavognost by and McMahon et al. (24E) have evaluated the formagraph,
Cloughley (170). A procedure for the analysis of unconjugated an instrument for measuring milk clotting, for comparing
pterins in foods has been described by Kohashi et al. (480) rennet solutions and found it satisfactory. A sulfur dioxide
using HPLC with fluorescence detection. Methods for tannins probe has been used by Alexander et al. ( I E )as a sensor in
in sorghums have been evaluated by Earp et al. (290),and an automated continuous-flowsystem for the determination
the vanillin-HC1 method is recommended. of glucose oxidase by reacting the hydrogen peroxide from the
Synthetic &carotene added to food has been determined enzyme reaction with hydrogen sulfite. Lysozyme has been
by Kamikura (440)using column chromatography on alumina. determined in egg white by Galyean et al. (14E)by ion ex-
Carotenes in tomatoes have been determined by Cabibel et change chromatography and UV detection. Measurement of
al. (150)using HPLC on a magnesium oxide column. HPLC nitrite production has been used by Junker et al. (16E) to
has been used by Bushway et al. (140)to determine a- and determine nitrate reductase in starter cultures. Pectic enzymes
@-carotenesin fruits and vegetables. Similarly Baranyai et in commercial enzyme preparation have been separated by
al. ( 7 0 )have used HPLC to determine carotenoids in paprika HPLC on a Spheron 1000 column and its ion-exchange de-
products. rivatives by Mikes et al. (25E). Peroxidase in sweet corn has
Reversed-phase HPLC has been described by Braumann been determined by Naveh et al. (28E)using a chemilumi-
et al. (130)as a means of analyzing chloroplast pigments from nescent procedure.
plants. Chlorophylls and their derivatives in spinach have Endopeptidases in malt have been extracted in aqueuous
been determined by Schwartz et al. (680) by HPLC with NaCl and cysteine and assayed on Azure-A hide powder or
gradient elution. gelatin by Anderegg et al. (2E). A radioisotopic method using
Methods for evaluating the color of meat samples have been denatured lz5I-labeledhuman serum has been suggested by
discussed by Pipek et al. (590). Transmission spectrometry Kas et al. (I7E) for the determination of low levels of pro-
has been used by Fransham (320)to evaluate haem pigments teolytic activity in foodstuffs. Proteinaseactivities at low levels
in muscle slices. Gel permeation chromatography has been in milk have been detected by Cliffe et al. (11E)using Hide
applied by Fraser et al. (330)to the separation and subsequent Powder Azure. Proteinases in sterile milk have been assayed
characterization of the colored components of processed palm by Chism et al. (9E) after incubation for 3 days and mea-
oil. Johnston et al. (430)have found good correlation between surement of fluorescence after addition of fluorescamine.
Hunter color values on semolina and lutein and p-carotene Peptidase activity in starter cultures and Cheddar cheese has
values. As an initial step in the study of oxidative browning been detected by Cliffe et al. (IOE)using a modified starch
in white wine, Nickenig et al. (560) have separated and gel electrophoretic technique.
identified phenolic compounds in the wine. Plant henolic enzymes have been determined by Blume
et al. (3E7 by HPLC analysis of the phenolic acids formed by
ENZYMES enzyme action. A metachromic agar-diffusion method for the
The presence of enzymes in foods may be used as both a determination of milk ribonuclease activity has been described
quality index and an index of proper preservation techniques. by Cantafora et al. (6E). The standard method for trypsin
Interest in analytical methods for these compounds therefore inhibitors in soy products has been modified by Hamerstrand
continues to be high. A collaborative study of the determi- et al. (15E)to remove the possibility of obtaining erroneous

172 R ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983


FOODS

high values, and Fernandez et al. (13E) have studied the reversed-phaseliquid chromatography (successively)followed
relationships of trypsin inhibitors and the content of tannins by final purification using AgN03impregnated TLC (58F)and
and polyphenols. A method for the analysis of urease activity Kolhe et al. (55F) report on the analysis for 3-oxotriterpenes
in soyabean products has been published by the British in the unsaponifiablle matter of some vegetable fats, finding
Standards Institution (4E). it to be present in 5 of the 14 fats examined. A rapid, simple
colorimetrictest using thymolphthalein is described (56F)for
FATS, OILS, A N D FATTY ACIDS the determination of acid value in oils which is reported to
A detailed comparison was made of methylene chloride and require only about 1 min to perform and which gave results
chloroform for the extraction of fats from food products in- similar to those obtained by the standard IUPAC test, Kuridu
volving samples of ten different retail foods (22F). Extracted and Deb (57F) report on a column chromatographic method
material was midyed by GLC and it was reported that CHC13 for determining unnaponifiable matter in fats and oils which
(a suspected carcinogen) can be replaced by CHzClz(each in they claim has advantages over standard methods, and the
a 2:l mixture with methanol) without loss of efficiency. A automatic determination of oxidation stability of oil and fatty
pulsed NMR method is given ( 5 9 9 for determining lipids in products is also given wherein volatile reaction products are
food products in which up to 4% of water does not interfere captured in a water trap and detected conductometricdly
and Robertson and Windham have compared results of the (36F). A procedure is presented for the analysis of oleate,
AOCS extraction-gravimetric method (Ai 3-75) with those linoleate, and linolenate hydroperoxides in oxidized ester
obtained by NIR and NMR spectroscopy for measuring the mixtures by reducing the hydroperoxides, separating the re-
oil content of wnflower seed (91F), finding no significant sulting hydroxy esters by argentation TLC, and then analyzing
different in total oil contents. Morrison (73F)describes a rapid the esters by GC ail their TMS derivatives (35F) and Bond
turbidimetric method for determining wax in sunflower seed et al. (18F)provide a differential pulse polarographicmethod
oil wherein the oil is heated, filtered, mixed with an equal for determining the malonaldehyde extracted from vegetable
volume of acetone, chilled in an ice bath and the turbidity oils using 2 M HCl as supporting electrolyte. The derivative
measured and compared against a calibration curve and a technique is used with UV spectrophotometry to measure the
comparative study was made of the Anton Paar density meter oxidative alteration of lipids (30F) and a TLC method is
against conventional dilatometry for determining the solid-fat described for determining the acetone insolubles in crude and
index of fats and oils (;'IF). A GLC method is provided for degummed rapeseed oils using chromarods followed by
the characterization of commercial waxes (61F)with the waxes quantitation using flame ionization detection (298')with the
being analyzed both before and after treatment with diazo- results obtained for phosphatides comparing favorably against
methane (for fatty acids) or acetic anhydride (for alcohols) gravimetric results. Tulloch reports (105F) on the use of 13C
and Miller et al. (70F)provide a rapid procedure for extracting NMR to nondestructively investigate the conjugated unciat-
milk fat which correlates well with Babcock results. Dry- urated acids in seed oil triacylglycerols, making structural
column extraction methods are given for the quantitative identifications of component acids from shifts of double bond
isolation of lipids of both partially defatted and dry roasted carbons and of carbons close to the double bond systems and
peanuts (3F) and for the quantitative extraction and class obtaining quantitation from signal intensities. The IGC
separation (i.e., neutral and polar lipids) of lipids from animal analysis of triglycerides on silanized glass capillary colunins
muscle tissue (ti5F). A new spectrophotometric method was is presented (43F,103F),mono- and diglycerides were analyzed
developed (81F)for determining the solid fat content (SFC) from rape oil and lard by GC of their silylated derivatives on
of crude palm oil, based on the different solubilities of the a glass capillary column coated with SE52 (89F),and Lainza
endogenous carotenes in the solid and liquid components of and Slover ( 6 0 9 make use of SP-2340 glass capillary colunnns
the oil, which has a 0.99 correlation for SFC as compared to for GC analysis of the trans fatty acid content of foods, with
that of the wide-line NMR technique and Bernard and Sims results reported for a variety of products. A multistep
( 1 O F ) describe an IR method for determination of total un- TLC-GC procedure is presented for determining the tri-
saturation (or iodine number) in pure, hydrogenated and glyceride composition of olive oil ( 2 6 0 ,the mass spectrometric
partially hydrogenated oils requiring no sample weighing and determination of triglycerides of selected fats by the direct
requiring only about 2 min per analysis. The phenolic acids chemical-ionization technique is described (95F), and Dlas-
of virgin, refined, and solvent extracted olive oils were de- gupta et al. ( 2 8 0 report on a new method for determining
termined by reversed-phase column HPLC (24F) with values glyceride composition of fats by oxidation, fractionation of
being obtained for protocatechuic,p-hydroxybenzoic,vanillic, the derived azeleoglycerides by TLC and quantitation of the
caffeic, syringic,p-coumaric,sinapic, 0-coumaric, and cinnamic fractions obtained by colorimetry. A colorimetric microdlet-
acids, and Bhuchar et al. (13F) describe a bromine titration erminationfor peroxide values is given (6F)which incorporates
method for on-line control of solvent extraction of whole aluminum chloride as catalyst, Yamaguchi reports on a sen-
ground-nut kernels which takes advantage of the facts that sitive and simple colorimetric method for determining fatty
some 80% of the ground-nut oil fatty acids are unsaturated acid hydroperoxides with horseradish peroxidase (11IF), and
and that bromine in the presence of a mercury salt will sat- Guhr et al. (44F) provide a standardized method for deter-
urate any double bonds including conjugated bonds. Based mining the polar fat fraction in frying fats using a silicic acid
on a successful IUPAC-AOAC collaborative study, a chro- column to retain the polar fat. A simple and rapid GC method
matographicmethod has been proposed to assess deterioration is given for the assessment of used frying oils (82F)wherein
of frying fats by measuring polar and nonpolar components analysis is achieved on a short column packed with 3% JXR
separated on a silica gel 60 column (107F),with the method and parameters are adjusted to provide a pattern in which
being adopted as official first action by the AOAC. Tyman the dimeric est,ers emerge as a doublet peak with a retention
et al. (106F)report an HPLC procedure for determining the time of about 3 min, a procedure is described for determining
long chain phenols and polymeric material in the phenolic hydroxytyrosol and tyrosol in the polar fraction of olive oil
lipids of cashew nut-shell liquid and a rapid column method by reversed-phase HPLC (42F),Meltzer et al. (69F) have
is described for measuring the unsaponifiable matter in fatty measured the cyclic monomers formed in thermally abused
acids ( 6 6 n with comparison made against the official AOCS soybean oils by gas chromatography after first hydrogenating
and ASTM methods. A colorimetric spot test is presented the oils and then separating a major portion of the saturated
by Robern and Gray (9OF)for monitoring the accumulation components from the cyclic monomers by low temperature
of oxidative products in heated oils wherein oils containing crystallization, Schulte (94F) presents a simple apparatus for
4, 10, and 20% altered triglycerides (as determined for com- the rapid analysis of polymerized triglycerides by gel chro-
parative purposes by silica gel chromatography) gave blue, matography (using a 1 m X 6 mm column of Biobeads El-X
green, and yellow spots, respectively, with bromcresol-green 2 and methylene chloride as the solvent/eluant), and Park
incorporated with silica gel on a slide, and analysis has been et al. ( 8 3 0 provide an HPLC method for determining the
made of the unsaponifiable fraction of many vegetable oils hydroperoxides formed by autoxidation of vegetable oils. The
by Lercker et al. (62F) by use of capillary GC on OV-17 of GC-MS analysis of the flophemesyl (dimethyl(pentafluor0-
the trimethylsilyl derivatives of unsaponifiable fractions first pheny1)silyl) derivatives of a series of fatty acid methyl ester
separated by TLC. Chromatographic procedures are given derivatives is reported (40F) and Min presents a correlation
for the isolation and identification of kahweol palmitate and of sensory evaluation against instrumental gas chromato-
cafestol palmitate from green coffee wherein a petroleum ether graphic analysis of edible oils (72F) reporting that flavor
extract was fractionated by preparative normal-phase and qualities could be correlated at 0.99, 0.98, and 0.95, respec-

ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983 173R


FOODS

tively, for soybean oil, hydrogenated soybean oil, and corn oil. glycerides by a combination of TLC followed by GLC (67F).
The rapid determination of mono-, di-, and triglycerides has Hsieh et al. (47F)have determined the saturated steryl esters
been performed by an enzymic technique after fractionation and acylglycerols in wheat endosperm by direct gas chroma-
by TLC (21F)and diacylglycerols have been measured as their tography on a column of 3% OV-17 on Gas Chrom Q and an
labile dimethylborate esters using reversed-phaseTLC (85F). automated colorimetric method is described for determining
Goiffon et al. (41F) provide retention indices for the HPLC free fatty acids in vegetable oils using the flow injection
analysis of fat triglycerides, El-Hamdy and Perkins report on analysis technique (31F). Three analyses (ATR-IR spec-
the HPLC determination of natural triglyceride mixtures trometry to follow trans-isomer formation, refractive index
covering the effects of column packing as well as "critical pair" to follow I value, and GC for fatty acid composition) were
separation (33F,34F),and HPLC has also been applied to the automated (17F) to follow the progress of vegetable oil hy-
analysis of the fatty acid composition of soybean oil after first drogenation, Mouillet et al. ( 7 4 9 report on a rapid titrimetric
forming the p-bromophenacyl esters of the fatty acids which method to monitor the fatty acids produced by the lipolysis
are then separated by gradient elution (50F).HPLC methods of milk and Battaglia et al. (8F)describe the enzymic de-
are reported for the analysis of triglycerides with methanol- termination of polyunsaturated fatty acids in foods by mon-
acetone as mobile phase and refractometric detection (88F), itoring the change in absorbance at 234 nm after addition of
with acetonitrile-isopropyl alcohol and hexane with UV de- lipoxygenase to a solution of food.
tection (46F)and with propionitrile or acetonitri1e:ethyl ether Chromarods-S modified with silver nitrate was used to effect
(2:l) as the mobile phase on a LiChrosorb RP-18 column (93F). a TLC analysis of the isomeric unsaturated fatty acids of
Petersson et al. (87F)describe the HPLC separation of natural partially hydrogenated menhaden oil using flame ionization
oil triglycerides into fractions with the same carbon number detection (96F),Scholfield reports (9ZF)on argentation HPLC
and numbers of double bonds and give results for palm oil, of methyl esters of vegetable oils and shortenings on an Am-
low erucic acid rape oil, and cocoa butter. Nimura et al. (8OF) berlite XE-284 column treated with AgN03, and partial ar-
make use of the fluorescent labeling of fatty acids with 9- gentation resin chromatography(Amberlyst XN-1010 sulfonic
anthryldiazomethane in neutral methanol to obtain improved acid resin with a portion of the sulfonic acid protons replaced
sensitivity by fluorimetric detection using HPLC for the by silver ion) has been studied to determine the effect of silver
separation and determination of geometric and positional levels on elution and separation of methyl octadecadienoate
isomers of long-chain fatty acids, the analysis of fatty alcohols isomers ( 2 9 and used to determine saturated and mono-, di-,
and acids by HPLC as their p-(methy1thio)-benzoateesters tri-, and tetraenoic fatty esters (IF). A new GLC method is
is reported (109F) and Svensson et al. (101F)describe the described for the determination of cyclopropenoic and cy-
analysis of geometric and ositional isomers of long-chain clopropanoic fatty acids in cottonseed and kapok seed oils by
monounsaturated fatty aci& by reversed-phase HPLC using use of glass capillary columns coated with BDS or Carbowax
an "interference refractive index" detector followed by glass 20M (15F) and Kint et al. (53F) report on the analysis of
capillary GC. Chemical ionization mass spectrometryhas been cyclopropenoid fatty acids by employing Raman spectroscopy.
used to identify positions of double bonds in polyunsaturated The HPLC analysis of cis and trans isomers of monounsa-
fatty acids (1OOF)and for the detection of hydroxy fatty acids turated fatty acids was performed with columns treated with
in biolo ical samples using both positive and negative CI-MS AgN03 (7F) and a method is given for the separation and
in comknation with capillary GC (98F). Neissner (78F) determination of fatty acids by isotopic dilution and radio-
provides a two-dimensional TLC method for the analysis of gas-liquid chromatography (9F).
complex mixtures of partial glycerides of castor oil fatty acids A method is provided for the rapid extraction of phos-
on activated silica gel plates and also a technique for the pholipids from plant oils and then estimating them by col-
preparation and TLC analysis of fatty acids after esterification orimetric determination of total phosphorus (102F),Stefanov
with mesoerythritol (77F). A two-stage TLC method et al. report a procedure for the quantitative determination
(CHC13:MeOH:HAcin a ratio of 98:2:1 followed by hexane- of phospholipids in sunflower seeds by two-dimensionalTLC
ETOET-HAC in the ratio of 470:30:1) is presented for sepa- and photometric determination of phosphorus (99F), a
ration of lipid classes (169. Glass capillary GC with a FFAP chromatographic method is presented for the isolation of
coated column was used to determine isomeric unsaturated phospholipids in peanut oils with the phosphorus being es-
fatty acids in edible fats ( 1 1 2 9 , Dasgupta et al. (27F) report timated by colorimetry and conversion factors provided for
on the use of ferric chloride-methanol reagent to convert fatty calculating the individual phospholipids from the elemental
acids into their methyl esters after 10 min of reflux prior to phosphorus (97F),and the determination of phospholipid in
GC analysis and Wilson described a rapid GC method (11OF) foods was also accomplished by a combined liquid chroma-
for determining erucic acid in rapeseed oil in order to comply tograph-automated phosphorus analyzer (51F). Biacs ( 1 4 9
with legislation requirements. The determination of erucic describes a gel chromatographic method for fractionating
acid in food oils is also effected by first separating the methyl sunflower and rapeseed lecithin with the fatty acids being
esters on a silica gel TLC plate and locating the erucic acid analyzed by GC, phospholipids are determined by TLC after
fraction by spraying with dichlorofluoresceinand comparing their column chromatographic separation from total lipid
against standards and then analyzing the fraction by gas extracts (39F),and TLC is also used to determine the phos-
chromatography, using tetradecanoic acid methyl ester as pholipids of milk without previous isolation from total lipid
internal standard (108F). Meijboom and Jongenotter (68F) extracts (38F) with the method described being reported to
give a combined TLC and GC procedure for the determination neither lyse the phospholipids nor cause any appreciable losses
of low erucic acid levels in oil after methylation with BF3- based on studies with phospholipid standards. A rapid and
MeOH with the cis-docosenoic methyl ester fraction being practical method is reported for the GLC measurement of the
analyzed by GC before and after ozonolysis. Trans isomers sn-1,2-diacylglycerolmoieties of natural glycerophospholipids
in shortenings and edible oils were determined by IR spec- using polar wall-coated open tubular columns (75F),a general
trophotometry at 967 cm-l, with base line calibration achieved method is given for analysis of phosphatidylcholines by HPLC
by use of standard methyl linoleate-methyl elaidate mixtures after formation of the phosphatidic dimethyl esters with re-
(63F), Marchand et al. (64F)describe complementary tech- sults given for egg (48F), Hanson et al. describe the HPLC
niques incorporating AgN03-TLC, methoxy, acetoxy- analysis of egg-yolk phospholipidsextracted from freeze-dried
mercury-adduct formation, ozonolysis, and gas chromatog- material in methanol with complete separation of neutral
raphy for the identification of trans,trans-18:2 isomers in lipids, phosphatidylcholine, sphingomyelin, lyso-
margarines, and HPLC is used with an infrared detector phosphatidylcholine, and phosphatidylethanolamine being
(monitoring at 5.72 ,urn) to determine free acids and mono-, attained in 30 min (45F)and a rapid HPLC method is also
di-, and triglycerides (84F). A rapid technique was developed reported for the determination of phosphatidylcholine in
for the determination of triglycerides according to their degree soybean lecithin (76F). Hurst and Martin (498")determine
of unsaturation using mercuric acetate adducts and TLC with the lecithin in chocolate b HPLC after extraction with a
flame ionization detection (86F),the fractionation of tri- modified Folch reagent anBthen eliminate interfering com-
acylglycerols was accomplished for peanut and cottonseed oils pounds with a Sep-PAK prior to chromatography, an HPLC
by use of reversed-phase HPLC (12F) and a method is pro- procedure described as suitable for the analysis of phospho-
vided for the determination of esterified safflower oils using lipids in tissue extracts is given (23F)wherein the separation
pancreatic lipase to selectively hydrolyze the acid at the 1- is accomplished on a microparticulate silica gel column using
position and then analyzing the free acids and the 2-mono- isocratic elution and UV detection at 203 nm and a solvent

174R ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983


FOO13S

mixture of acetonitrile-methanol-85% phosphoric acid pulse polarography after separation by steam distillation is
(1305:1.5 by volume), and Beutler and Henninger have de- reported (46G),Flanders et al. describe the application of two
termined lecithins in food by use of an enzymic method (1IF). different trapping/ isolation, methods coupled with flame
A novel system for separation of phospholipids by HPLC is photometric GC for the analysis of the volatile sulfur coim-
given wherein radioactively labeled phospholipids are sepa- pounds from cooked (hen) eggs (19G),and a procedure is given
rated on a column of LiChrosorb Si 60 (10 pm) with use of for the analysis of roquefortine in blue cheese and blue-cheese
a two-stage elution system, with half of the eluate being passed dressing using HPLC with both ultraviolet and eledrochemical
through a flow-through radioactivity detector and the other detectors and a LiClhrosorb RP-2 column after extraction of
half collected for scintillation counting (5F). samples with ethyl acetate (94G). A method is described (50G)
A HPLC method for cholesterol in foods is given which in which the alkaline aroma components of Swiss Gruyere
makes use of the benzoate ester of cholesterol and a Bondapak cheese are isolated by vacuum gas stripping of grated cheese
C18column with UV detection (79F), Tsai and Hudson have samples at room temperature followed by ether extraction of
analyzed 24 oxygenated cholesterols and structurally related the alkalinized distillates, and they are then analyzed by GC
compounds by HPLC using a silicic acid column with various using nitrogen specific detection combined with mass spec-
mobile phases and show the effect of various functional groups trometry.
on the retention volumes (104F),El-Hamdy (32F)reports on Grandolini et al. (27G) describe a GC method for deter-
the application of HPLC reversed-phase chromatography for mining quassin from beverages using a column of SE 30 on
separating triglycerides, cholesterol, and cholesteryl esters and Gas Chrom Q, quassinoids are determined in bitter Simiar-
its application in the analysis of natural and oxidized oils, and oubacea extracts by HPLC on Radialpak C using aqueous
Csiky (25.F)describes a technique for the trace enrichment methanol as eluant (82G),GC methods are described for the
and separation of cholesterol oxidation products by adsorption determination of volatile aromas in syrups and brown sugars,
HPLC wherein the oxygenated sterols are concentrated on with 29 flavor compounds identified in brown sugars (24G)
a short precolumn of Nucleosil NO2with hexane as the mobile and also for the determination of the volatiles responsible for
phase and separation is accomplished on a longer column with characteristic molasses aroma (25G),and the HPLC analysis
the same stationary phase but with a hexane-propanol or of 5-hydroxymethyl-%furaldehyde(HMF) in caramel solution
hexane-butanol gradient. In an effort to provide more ac- is given which is applicable to brandies or liqueurs (IG). The
curate cholesterol data for foods, Fukui et al. (37F) report on analysis of both furfural and HMF in brandy and honey is
the determination of cholesterol by TLC, GC, GC-MS, and reported using reversed-phase HPLC on a LiChrosorb RP-18
by an enzymic and a colorimetric method. A GLC procedure column and UV detection at 285 nm (38G),the glycosides of
is described for the direct analysis of cholesterol after ex- liquorice (including glycyrrhizin) have been measured by Chen
traction of foods with chloroform-methanol (2:l) (52F), a and Li (7G)by means of extraction in ammonia, separation
biochemical method is applied to the analysis of cholesterol using ion-exchange chromatography, and detection by tur-
in fats and oils making use of the H 2 0formed when cholesterol bidimetry at 530 nm after heating the eluate with HC104,and
is oxidized by cholesterol oxidase to develop a colorimetric a HPLC method is also given for the determination of gly-
method for its determination (20F),and Knights (54F) reports cyrrhizin in foods such as soy sauce and miso (42G)wherein
on a combined TLC-GLC method for the quantitative analysis the glycyrrhizin was isolated with a polyamide column priior
of plant sterols. A GC method is given for the determination to HPLC analysis on a reversed-phase C8 column using TJV
of 0-sitosterol in meats, soya, and other protein products ( 4 9 . detection. Woodbury (97G) has developed a method which
Byrne et a1. (19F)report, on the determination of 0-sitosterol determines the pun ency of capsicum by use of HPLC wiith
and 0-sitosterol-D-glucoside in whiskey by HPLC after first spectrofluormetric cfetection, Shankaranarayana et al. (76G)
collecting them on a short Amberlite XAD-2 column from give a titrimetric method for determining the flavor strength
which they are eluted with chloroform-2-propanol (3:l) and in alliums based on oxidation of the steam distillate with
HPLC is employed by Kashimoto et al. (113F)to determine chloramine-?’, TLC followed by spectrometric measurement
sesamolin, sesamin, and sesamol in sesame oil. is used to analyze for the sinapine contents of mustards (39G),
Bajaj determines the capsaicin in capsicum fruits spectiro-
FLAVORS AND VOLATILE COMPOUNDS photometrically after first effecting a chromatographic sep-
aration from interfering pigments (2G),and a procedure is
A number of new bo0k.s have been recently published which provided for the determination of isothiocyanic esters (applied
are directed toward the analysis, control, and understanding to allyl isothiocyanate in mustard) in which the ester is fiirst
of flavors and aromas and which serve as useful reference converted into a thiourea and then titrated with mercuric
works for the flavor analyst. Among these are the 3rd acetate solution using a mercur or silver amalgam electrode
Weurman Symposium Proceedings of the International Flavor (IOG). A combined ‘TLC-HPL: procedure is given (81G)for
Conference (74G),The Quality of Foods and Beverages (6G), the determination of the main pungent principles of ginger
which provides the proceedings of the Second International wherein the dried and powdered root is first extracted with
Flavor Conference held in Athens, Greece, and The Analysis ethanol under reduced pressure (results are given for 12
and Control of Less Desirable Flavors in Foods and Beverages samples including data for 6-, 8- and 10-gingerols and 6-, 8-,
by Charalamboiis (5G). Food Flavors, Pt. A: Introduction, and 10- shogaols), Oberdieck described methods (59G) used
by Morton and IMacLeod (56G),Theimer’s Fragrance Chem- for the isolation by steam distillation of the essential oils of
istry the Science of the Sense of Smell (83G), and The 10 varieties of marjoram and subsequent separation of the
Chemistry of Heterocyclic Compounds in Flavors and Aromas volatiles obtained by column chromatography prior to GLC,
by Vernin (92G) are also useful references. Jennings and GC-MS, and IR analysis, and Haut and Core (29G) provide
Shibamoto have provided a book on the Qualitative Analysis a HPLC method for the analysis of menthol isomers which
of Flavor and Fragrance Volatiles by Glass Capillary Gas has been applied to the analysis of corn-mint (Mentha arvenis)
Chromatography (37G),which contains mass spectral data as oil. Davis and Cooks (12G) have made use of various hdS
well as GC retention indices for many volatiles (for OV-101 techniques to directly analyze nutmeg, taking data with both
and Carbowax 20M columns), and Kolor has reviewed the a sector type and a triple quadrapole MS-MS instrument,
mass spectrometric analysis of various classes of flavor com- using the scans of all precursor ions that yield mass-selected
pounds in a variety of foodstuffs (44G). fragment ions, to characterize groups of compounds with
The use of closed-system vacuum distillation as a means particular structural units, and also to pinpoint where MS-R4S
of quantitativelg and rapidly isolating moderately volatile spectra contained contributionsfrom more than one structural
compounds from food for GC analysis is described by Daniels isomer. Kihara (40G)reports a spectrophotometric method
et al. ( I l G ) , advantage i s taken of the charge-transfer com- for general application to the measurement of maltol in plants
plexes formed with nitro-aromatic compounds by pyrazines by extracting with methylene chloride and then forming the
(formed by the heat treatment of foods) to effect their TLC maltol-Fe complex by addition of FeC13,a GC method is given
separation on Silica Gel G (89G),and Parliment and Spencer for the determination of the volatile phenols in soy sauce
(62G) describe the use of simultaneous detectors (FID plus (58G),and a scheme has been developed for the characteri-
FPD detectors for nitrogen and also sulfur) combined with zation of the nonvolatile minor constituents responsible for
capillary gas chromatography for measuring specific flavor the objectionable taste of defatted soybean flour (34G) by
compounds in complex natural mixtures. sequential HPLC analysis. The volatile flavor of defatted
The determination of diacetyl and acetoin by differential soybean flour has been analyzed by GC and the fractions with

ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983 17!i R


FOODS

objectionable flavor of characteristic beany, grassy, and green in meat by autoxidation of fatty acids as their 2,4-DNP de-
odors were further examined by MS and IR with 25 com- rivatives (69G, 70G),Lee et al. (47G) report on the analysis
pounds identified and 2-pentylfuran and ethyl vinyl ketone of methyl-3,4-dimethyl-5,6-dihydro-a-pyran 6-carboxylate in
believed to be key compounds for the beany and grassy odor roast beef volatiles by IR, NMR, and MS, and Golovnya and
(33G),Eldridge (17G)and Ohta et al. (61G)have determined co-workersdescribe methodology for the isolation and analysis
individual and total isoflavone content in soybean products of 27 volatile sulfur-containing compounds of salted and
by HPLC, and the volatile flavor compounds of roasted salted-boiled pork by GC with flame photometric detector
peanuts have been analyzed by GC fractionation followed by (26G). A purge and trap technique combined with GC-MS
IR and MS identification with a total of 131 compounds being is used to determine the volatile organic compounds in fish
identified (32G). The volatile flavor components of Idaho (16G),and Whitfield et al. (95G) report on the analysis of
Russet Burbank baked potatoes were also analyzed by GC oct-1-en-3-01and (5Z)-octa-1,5-dien-3-01by GC, microreaction
fractionation and IR and MS identification with 227 com- GC, NMR, and MS in the flavor of prawns and sand lobsters.
pounds being identified (9G),the volatile carbonyls of fresh The determination of 2-acetyl-5-bromopyrole has been
tomatoes and tomato preparations were isolated as their made in the volatiles of cocoa butter by GC with identification
2,4-DNP derivatives and separated for analysis by TLC (63G) made by retention time, NMR, and MS (31G), Ziegleder
and by subsequent HPLC using reversed phase technique makes use of the measurement of methylated pyrazines
(88G),and Pyysalo et al. (67G) report a GC method for the formed during the roasting of cocoa (by capillary GC on a
analysis of sesquiterpene lactones from mushrooms as their Carbowax 20M column) as a means of monitoring degree of
trimethylsilyl derivatives on a capillary column coated with roast (99G),and Wang reports on the analysis of trace volatile
OV-101. Methods are given for the analysis of the volatiles organic compounds in coffee by means of a headspace con-
of roasted pistachio nuts which employ GC-MS after first centration technique followed by GC-MS measurement (93G).
fractionating the volatiles into basic and neutral-acidic Tress1 et al. (86G)describe GC-MS methods used to analyze
fractions (78G),a TLC method is provided for the analysis N-alkyl- and N-furfurylpyrroles in roasted coffee, the sul-
of pyrazines formed by peanut oil interactions with a-amino fur-containing compounds in roasted coffee have been de-
acids a t elevated temperatures (90G), and a procedure is termined by distillation-extraction, adsorption chromatog-
reported for the determination of the heterocyclic flavor raphy, and capillary gas chromatography (87G),a technique
volatiles formed in the basic fraction of roasted mung dal by is given (68G) for the quality evaluation of roasted coffee
TLC and GLC (91G). Cant and Walker describe a colorimetric through storage by quantitative trace analysis of aroma com-
method suitable for the routine analysis of indole in butter ponents using GC-MS, and Toth (84G, 85G) describes GC
and milk fat (3G)and techniques are described for the analysis methods for the separation and analysis of phenol fractions
of saturated hydrocarbons in foods by use of sequential col- from smokehouse smoke.
umn, thin layer, and gas chromatography after extraction with A rapid, automated enzymic method is reported (98G)for
pentane of HC1 treated samples (14G). the determination of alcohol by using flow injection analysis
A capillary GC method using a Carbowax 20M column is which is suitable for beverages, Sponholz and Wuensch (80G)
given for the analysis of the volatiles in cold-pressed grapefruit provide an enzymic method for the determination of di-
oil with a comparison made of internal-standard and nor- hydroxyacetone in the presence of glycerol in alcoholic bev-
malization methods for quantitation (96G),a GC method is erages, and GC analysis for aldehydes in (German) wines is
provided for the determination of trans,trans-a-farnesenein described (79G). A procedure for the gas chromatographic
samples of distilled Mexican lime oil and cold-pressed Valencia analysis of volatile esters in wines is presented (77G) alon
orange oil using direct injection (57G),and Mansell and Weiler with data for various commercial wines, Schreier reports (75G7
(51G) report a radioimmunoassay for the determination of on the determination of additional volatile constituents of red
limonin in citrus plants. Nomilin, a new bitter component wine by GC and GC-MS techniques, and a headspace GC
in grapefruit juice has been determined chromatographically method is iven for the determination of safrole in flavored
and measured in commercial juices with concentrations found beverages ?73G) such as vermouth. Postel and Meier (66G)
to be highest in early season juices and decreasing with fruit present a method for the GC determination of 2-acetolactate,
maturity (ranging from 1.6 to less than 0.1 ppm) (71G). Pino 2-acetohydroxybutyrate, diacetyl, pentane-2,3-dione, and
(65G)has developed correlations between sensory evaluations acetoin in grape must and wine, a HPLC method is given for
and gas chromatographic measurements of orange volatiles, the determination of acetaldehyde in wine as its lutidine
finding high correlation coefficients for specific compounds derivative (60G)and a reversed-phase HPLC method is re-
such as myrcene, 2-hexanol, linalool, and a-terpineol, and ported for the determination of @-asarone(a constituent of
Rouseff and Fisher (72G) report on the determination of calamus oil) which is used as a flavoring (e.g., vermouth) and
limonin and related limonoids in citrus juices by HPLC on which is regulated in much of Europe (55G). An enzymic assay
a Zorbax CN column using IPA-hexane-CH30H (12:ll:Z) as for acetaldehyde is provided (54G)for grape juice and wine,
mobile phase with UV detection. The flavor volatiles of Martin et al. (53G)report on the determination of congeners
cultivated strawberries have been analyzed by GC-MS and in alcoholic products by GLC using GC-MS as a confirmation
the data obtained correlated with sensory data (the methyl- technique, and Leppanen and co-workers (49G)describe the
thiol acetate and butyrate compounds are reported for the headspace adsorption (on Chromosorb 101) followed by GC
first time) (15G),a GC method is given for measurement of analysis for the determination of thioacetates and other
furaneol in cultivated and wild strawberries, pineapples, and volatile sulfur compounds in alcoholic beverages. Lehtonen
mangoes using a Carbowax 20M capillary column with FID has developed a GC method for analyzing phenols in alcoholic
detection (64G),and 4-(p-hydroxyphenyl)-2-butanonehas beverages as their 2,4-dinitrophenyl ethers using glass capillary
been determined in 39 samples of raspberries and foods in- GC and EC detection (48G),a microwave spectroscopic me-
corporating raspberry flavorings by GC-MS (52G). Methods thod is provided for determining methanol in wine (43G),and
are given for the analysis of 1-(4-hydroxypheny1)-3-butanone a combined LC and HPLC method is given for the analysis
(or raspberry ketone) in foods by a rapid TLC method on silica of carbonyls from beer at the parts-per-billion level after
gel plates (23G)and by HPLC on a LiChrosorb Si 100 column collecting them as their 2,4-DNP derivatives (28G). A rapid
(20G) and a rapid colorimetric method is reported for HPLC method is reported for the determination of 2-fur-
measuring the aroma index of steam distillates of raspberries aldehyde and hydroxymethyl-2-furaldehyde in alcoholic
by the intensity of the blue color formed when these distillates beverages using a reversed-phase technique (22G),Frattini
are treated with vanillin in concentrated sulfuric acid (45G). et al. (21G)describe the LC fractionation and GC-MS analysis
High-resolution glass capillary GC analysis was made of the of the volatile components of mountain wormwood essential
aliphatic lactone in the aroma fraction of dates (41G) and oil, and Etievant (18G)describes the analysis of the volatile
Ismail et al. have analyzed the flavor components of canned phenols in wine by GLC and GC-MS after solvent extraction
plums (36G) and plum juice (35G) by GC and GC-MS. and column chromatographic fractionation on a DEAE-cel-
Chairote and co-workers (4G)have determined the volatile lulose column, Dickenson (13G) provides a headspace ca-
flavor components of apricot by GC-MS after isolation by pillary GC method for the determination of dimethyl sulfoxide
vacuum distillation and fractionation on silica gel columns, in malt, wort, and beer and Cheney et al. (8G)report on the
and the GC-MS analysis of cranberries is reported with the analysis of ethanol in solution by alternating current ten-
identification of 70 compounds (30G). Reindl and Stan sammetry, reporting satisfactory results for vodka but indi-
provide HPLC methods for determining the aldehydes formed cating that substances having surfactant properties (such as

176 R ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983


FOODS

fusel oils in distilled spirits) gave interferences. (28H). The volatile components of raw tuna have been clor-
related by Human et al. (26H) with the quality of the fkh.
JDENTITY Total volatile basic nitrogen, determined after steam distil-
This section is concerned with analysis of pure foods, de- lation, has been fouind to increase with deteriorating quality
tection of foods in foods, and indicators of quality. Pattern by Billon et al. (5H).
recognition techniques have been proposed by Leegwater et Detection of high-fructose corn syrup in apple juice by mius
al. (44H) as a means of differentiating French and German
brandies by the use of four flavor components as characteristic
variables. Chinese alcoholic beverages have been analyzed
b
spectrometric I3C 12C analysis has been submitted to col-
laborative study y Doner et al. (15H) and the method
adopted first action. Analytical techniques have been de-
by Ng et al. (55H) using gas chromatography and ratios of scribed by Brause et al. (6H) for the verification of the au-
higher alcohols to methanol were found to be useful criteria thenticity of apple juice. Components of apricot pulp halve
for identification. The use of liquid scintillation counting of been determined and tabulated by Fuchs et al. (20H). Ana-
14C has been suggested by Martin et al. (50H) for the dif- lytical data on blueberries, blackberries, and elderberries,
ferentiation of synthetic ethanol from ethanol of fermentation. includingamino acids, has been reported by Kuhlmann (42H)
Total alkaloid value has been suggested by Hadorn (21H) as for the expressed juices of these berries. The papers included
means of estimating cocoa mass in cocoa containing products. in a symposium on citrus nutrition and quality have been
Theobromine and caffeine contents of chocolate and milk published by Nagy et al. (54H). Flavonoids and citrus quality
chocolate have been reported by Herrmann et al. (22H) and have been discussed by Rouseff (6623. Analytical data on
of various natural and red Dutched cocoas by De Vries et al. Israeli orange amd grapefruit juices have been reported by
(12H). The use of gas chromatographic triglyceride analysis Cohen (823, and Wallrausch (78H) has determined and tab-
has been reported by Fincke for the examination of cocoa- ulated data on grapefruit juices. The use of spectrometric and
butter-substitute fats (18H) and for cacao butter (19H). fluorometric examinationof orange ‘uice and orange pulpwalsh
Sterols and met hylsterols in cocoa butter and cocoa butter to detect mixtures of the two has been described by Petrus
substitutes havt? been studied by Homberg et al. (25H) and et al. (59H). Data on trace metals in orange juice have been
qualitative distinctions have been made. Foreign fats in cocoa summarized by McHard et al. (46H). Pattern recognition
butter have been detected by Dick et al. (13H) by GC exam- techniques have been used by Bayer et al. (4H) to select five
ination of the urisaponifiables for steroids. Interpretation of elements (Ba, B, Ga, Mn, and Rb) in orange juice concentrate
triglyceride patiterns by GLC has been proposed by Padley which can be used as indicators of geographical origin. A
et al. (57 M) as a means of determining the amount and type collaborative study has been carried out by Doner et al. (16H)
of “cocoa butter equivalents” added to chocolate. The degree of the mass spectrometric procedure for the detection of high
of roasting of cacao has been estimated by Ziegleder (85H) fructose corn syrup in orange juice; the method was adopted
by GC determiriation of methylated pyrazines. first action. Tagetes extract in orange oil has been identified
An HPLC method for the determination of 5-hydroxy- by Wild et al. (80m by the examination of the carotenoid
methyl-2-furaldehyde and caffeine in coffee and chicory ex- pigments. Literature data have been compiled by Wrolstad
tracts has been described by Smith (73H),and the detection et al. (82H) on free sugars and sorbitol in fruits and on sugars,
of the furaldehyde can be used to distinguish coffee from sorbitol, nonvolatile acids, and free amino acids in fruit juices
coffee-chicory extracts. Changes in the volatiles of roasted (83H). Elementary contents of 15 standard fruit and vegetalble
coffee during storage have been studied by Radtke-Granzer materials have been listed by Daniel (IOH). Free and total
et al. (61M. Triglyceride GLC has been used by Timms (76H) amino acids in citrus juices and strawberry and blackberry
to detect as little as 5% of nonmilk fats in milk fat. A rapid mashes have been determined by Tateo et al. (75H). Twen-
detection procedure for cows milk in goats milk has been ty-four fresh fruits have been analyzed by Richmond et al.
described by Mitchell (52H) using electrophoresis on cellulose (63H) for sugars and sorbitol by HPLC.
acetate. Cows milk in sheep and goats milk has been detected Electrophoresis techniques including gel electrophoresis and
by Krause et al, (40H) by the use of isoelectric focusing on methods for the identification of cereal varieties by exami-
polyacrylamide gels containing urea. A polarographicmethod nation of the grain proteins have been discussed by Wriglley
for mercapto groups has been used by Lechner et al. (43H) et al. (81H).Data on minerals and protein contents in hard
to detect whey powder in skimmed milk powder. The am- red winter wheat cultivars have been obtained by Dikeman
monia content of milk has been determined by Soederhjelm (14H). Electrophoresishas been used by Joudrier et al. (31H)
et al. (7113)using an ammonia electrode, and the ammonia to detect the presence of barley in hard wheat flour paste by
content may be used as an indicator of biological deterioration the characteristic amylase polymorphism in the two species.
or aging. Casein and whey-protein containing casein have been Rice or buckwheat flour in wheat flour has been determined
differentiated by Kabus et al. (33H) by amperometrictitration by Ohara et al. (5CiH) by electrophoresis of the proteins.
of the SH and 5% groups. Total protein, casein, and whey Electrophoresis of the prolamins of wheat, rye, barley, and
protein in dairy products have been determined by Douglas oats has been used by Hohlfeld et al. (24H) to detect those
et ei. (17H) by the use of the phosphorus to nitrogen ratio. grains in flours and foods. Mineral contents of a selection of
Phosphatidylcholinecontent determined by TLC and GC has cereals and baked products have been determined by Mahoney
been suggested by Liem et al. (45H) as a specific basis for WH).
egg-yolk determination in food products. Egg content in Three percent of added sugar has been detected in maple
pastry has been determined by Kaffka et al. (34H) by the use products by Carro et al. (7H) by stable carbon isotope ratio.
of NIR spectrometry. Sweet almond oil has been differen- Sugar-adulteratedand natural honeys have been differentiated
tiated from blends with apricot and peach-kernel oil by Salvo by Zagaevskii et al. (84H) by the color produced with camphor
et al. (6710 using TLC and GC of the sterols. Argemone oil solution and by the amylase activity. Further testing to
has been determined by Shenolikar et al. (68H) in edible oil confirm high-fructosecorn syrup adulteration of honey when
by TLC, and argemone oil and rapeseed oil have been detected certain hotope ratios are obtained by the AOAC test has been
in mustard seed oil, also by TLC, by Datta (11H). A TLC recommended by White (79H). Polarographic suppression
procedure has been used by Sengupta et al. (70H) to detect of the 0 peaks during the determination of fructose has been
palm oil in vanaspati. Combined column and gas chroma- found by Marek et al. (49H) to be a means of detecting the
tography have bleen applied by Kapoulas et al. (37H) to the addition of invert sugar to honey.
determination of seed oik in olive oil. Tallow in lard has been Electrophoreses has been used by Armstrong et al. (223 to
detected by Juarez et al. (32H) by gas chromatography of the determine isolated soybean protein in raw and pasteurized
fatty acids. The use of gas chromatographyfor the assessment meat products and by Valas-Gelleiet al. (77H) to determine
of used frying oils has been described by Paradis et al. (581fl milk and soy proteins in meat products. Gel permeation
by measurement of the dime, triglyceride content. chromatography has been applied by Iijima ‘29H) to the
Protein patterns obtained om cooked and frozen crab analysis of soyabean pvotein products in foods. A rapid
meat have been shown by Krzynowek et al. (41H) to differ- chromatographic m e t h d using modified circular pager
entiate between genera by the use of polyacrylamide gel chromatography ha13been developed by Jebsen et al. (30.H)
isoelectric focusing. An index using biogenic amines has been for the detection of foreign proteins in minced meat. Soybean
found by Karmas (38H)to provide a quality indicator for protein in meat products has been determined by Crimes et
seafood. Ethanol has been described by Iida et al. (27H) to al. (9H)by analyzing the soluble peptide for serine and by
be useful as a quality index for albacore and for other raw fish an immunosorbent assay procedure. The enzymatic analysis
ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983 177 R
FOODS

of galactose in soya has been applied by Morrissey et al. (53H) Uthus et al. (1344 to report lower interferences in arsine
to the quantitation of soya proteins in soya-meat blends. detection. A one-piece design apparatus was shown by Ev-
Linear gradient polyacrylamide gel electrophoresis has been erson (455) for arsine generation in AOAC method 42.005.
applied by Babiker et al. (323 to the detection of horse meat Liddle et al. (815) listed o timal conditions for generating
in beef. Enzyme staining of isolectric focusing gels has been arsine with sodium borohy&ide for AAS. Brooke et al. (164
used by King et al. (39“) to detect buffalo, horse, pig, or distilled inorganic arsenic first from HC1 or chelated it to
kangaroo meat in beef. Feather meal in protein concentrates separate it from organic arsenic before hydride AAS in their
has been determined by Maestro et al. (47H) by TLC of the studies on fish. Maher (834 used ion exchange to separate
amino acids. The amino acid content of collagen from various inorganic from methylated arsenic species in clams and then
fabrics has been determined by Polzhofer (60H)by amino acid determined the fractions separately by reduction to arsine and
analysis and the information applied to the analysis of the graphite tube AAS. Kurosawa et al. (775) examined shark
collagen coating on synthetic sausage skins. Tryptophan and tissue for arsenobetaine, separating it by an HPLC connected
hydroxyproline contents of sausages have been suggested by directly to an ICP plasma spectrometer set to 193.7 nm.
Sokele et al. (72“) as indicators of quality. Biogenic amines Burkhardt ( 2 0 4 described his temperature-controlled ap-
have been described by Slemr (69H) as potential chemical paratus for wet ashing foods and the diethylammonium-di-
indicators of meat quality. Patterns obtained by HPLC and ethyldithiocarbamate chelation steps before flameless AAS
electrophoresis for protein supplements such as @-casein, of As, Pb, Cd, Hg, and Se. Mueller at al. ( 9 6 4 used wet
@-lactoglobulin,and soyabean protein have been described by digestion and the same extractant for these elements in a
Reimerdes (62H) as distinctive and useful for detecting these graphite furnace AAS method. Arafat et al. ( 7 4 used wet
additiveg. Proteins of vegetable and animal origin have been acid-peroxide digestion before hydride generation and flame
differentiated by Ring et al. (64H) using disk polyacrylamide aspiration AAS for As, Al, Fe, Zn, Cr, and Cu in plant samples.
gel electrophoresis. These same protein types have been An AutoAnalyzer was used for the reduction of As and Se to
examined by Kaiser et al. (36H) by isoelectric focusing in hydrides with flameless AAS by Agemian et al. ( 2 4 . Holak
agarose gel. Proteins in binary raw meat mixtures have been (645) reported a collaborative study on closed-system digestion
examined by Kaiser et al. (35H) using the same technique, followed by ASV and both normal and hydride AAS for metals
and mixtures could be analyzed. Soya, egg albumin, and wheat including As, Se, Pb, Cd, Cu, and Zn. A review on selenium
gluten have been separated by Rizvi et al. (65H) by sodium trace methodology for food was written by Hofsommer et al.
dodecyl sulfate gel electrophoresis. Soya proteins in food have (624. Hahn et al. (584 illustrated how condensation of the
been determined by Hitchcock et al. (23H) using an en- hydride improved selenium AAS methodology for vegetable
zyme-linked immunosorbent assay. Analytical data showing analysis. An interference in the direct determination of Se
differences in mineral and proximate analyses content between by flameless AAS, namely, HC1, was discussed by Hofsommer
mechanically deboned and hand-deboned broiler parts have et al. (634 who recommended C U ( N O ~addition.
)~ Vijan et
been obtained by Ang et al. (1H). A staining technique using al. (1364 described the inhibitory effect of other metals in
iodine has been used by Sreedharan (74H) to distinguish Se hydride generation and they advised using 7.5 M HCl to
papaya seed from black pepper. The stable-isotope ratio complex those metals first. Inui et al. (674cleaned up acid
technique has been used by Martin et al. (51H)to determine digests of tea and liver by ion exchange before Se hydride
natural vanillin in adulterated vanillin extract, and the vanillin generation into a graphite tube furnace. Reamer et al. (1144
to potassium ratio permitted differentiation between vanilla compared several wet and dry ashing methods for Se losses,
extracts from Java and Madagascar. following retention with 7bSe. Several food materials were
analyzed by Rigin (1164 who used extraction of Se’” with
INORGANIC 4-nitro-0-phenylenediamine in toluene, generation of the
An extensive review of trace element determination via hydride from this solution, and detection of Se by atomic
spectrophotometric techniques was published by Marczenko fluorescence in a helium stream. 82Sewas added by Reamer
(844, within which food applications were considered. Mirza et al. (1154to samples before wet digestion and complexation
( 9 0 4 discussed the properties of 4-benzoyl-3-methyl-1- with this reagent and then ratioed to 8oSe after GC-MS.
phenylpyrazolin-5-one as a broad spectrum extraction reagent Raptis et al. (1124 followed wet and dry digestions with the
for metals. A novel test strip for Cu, Zn, Cd, Ni, and Co ions eneration and filtration of elemental Se, which was measured
was prepared by Tanaka et al. (1294 with 2-(2-thiazolyl- E y X-ray fluorescence.
azo)-p-cresol reagent in a PVC film. Blake (114 presented The procedings of the AOAC “Symposium on Analytical
a large review on sample preparation before atomic absorption Methodolo for Lead in Foods” were compiled for publication
spectrometry (AAS). Atomic spectroscopy literature from July
to December 1981 was cited by Lawrence (794. The hydride
by Boyer 0, Sampling and homogenization to improve
data uniformity for lead in canned food were discussed by
generation technique as applied to AAS methods was reviewed Suddendorf et al. (12w). Rains et al. (1114 and Koirtyohann
by Godden et al. (524. Verlinden et al. (1354 prepared a et al. ( 7 4 4 all presented the advantages of using a L’vov
review concerning hydride-AAS approaches. Several different platform in electric furnace AAS for lead analysis, and also
spectrometric methods such as AAS, ICP emission, X-ray recommended NH4H2P04to level remaining matrix effects.
fluorescence, and NAA were covered when Pickford (10 8 4 Dobeka (334 reported results of analyses conducted by op-
reviewed trace diet components. An apparatus that automated erators of different experience levels and concluded that
the time and temperature control aspects of wet ashing was routine trace lead analysis was reliable if attention was given
used by Nakajima et al. ( 9 9 4 to expedite the removal of to contamination control. Miles (894 compared studies in-
organic material from polished rice samples. Schramel et al. volving ASV and furnace AAS lead measurement to assess
(1194 described a Teflon tube holder for accelerated de- reliability for infant formula analysis. Mergey et al. (884
composition at 160 OC and 10-12 bar pressure. A stepwise increased sample throughput by conducting wet digestion and
procedure for dry ashing sugar was given by Saito et al. (1184. ASV in a single tube without Metexchange reagent. Lead and
Techniques for the direct introduction of solid samples into cadmium were precipitated to preconcentrate them before
a carbon tube for AAS were shown by Grobenski et al. (564. AAS measurement of a sulfated ash solution in a method by
Brooks et al. ( I 7 4 reviewed the instrumental determination Gorshkov et al. (534 applied to grain and potatoes. Kruse
of arsenic, covering 1971-1981. Cottenie et al. (314 discussed (765) wet-ashed fish in Teflon beakers with loose covers
plant analysis for many metals including arsenic by ICP preceding furnace AAS. Poldoski (11OJ)found that treatment
plasma emission and listed the effect of using different spectral of his graphite furnace tube with Mo and La solutions gave
lines and operating conditions. Jones et al. ( 7 1 4 evaluated more even atomization of lead and cadmium from fish digests.
a procedure for separating elements by ion exchan e before Caristi et al. (235) mixed 50% NH4N03solution with citrus
direct or hydride generation ICP determination. 1 sample
inlet for an ICP spectrometer that permitted hydride intro-
juices before introduction into the electric AAS furnace for
Pb, Cu, Fe, and Zn analysis. Nembrini et al. (1014 gave the
duction along with usual ionic solutions was presented by advantages of using a “Lumatom” digesting solvent before AC
Wolnik et al. (1385). Hahn et al. ( 5 9 4 employed a cqld polarographic measurement of tin, lead, and copper. This
condensation trap to concentrate hydrides before ICP emis- technique was further discussed by Dogan et al. (404. A
sion, achieving an order of magnitude better sensitivity than collaborative study of a method for Pb and Cd using ASV after
direct introduction. Some changes in graphite furnace gas dry ashing was reported by Capar et al. (225)and adopted
purging and addition of EDTA to the sample solution allowed official first action (AOAC). Mrowetz (945) determinted Pb,

178R ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983


FOODS

Cd, and Cu by A8V after dissolution of an oxide ash in H2SO4 digests as quinolin-8-01complex in CHC13before dissolution
solution and then added HC1 to do Sn. Debacker et al. (364 in acid and ICP emission. A method that could detect a
found they could measure Sn and Pb in the same stripping nanogram per milliliter of Mo by differential pulse polarag-
voltammogram in a methanol-2-propanol-HC1 electrolyte. raphy (DPP) was given by Chatelet-Cuzin et al. ( 2 5 4 who
Good agreement with other tin methods was found by Dabeka optimized electrolytes. Vanadium in foods was determined
et al. ( 3 4 4 when they aspirated food acid digests into a colorimetrically by Bermejo-Barrera et al. ( 9 4 using 8-
N20-C2H2AAS flame with added K+ ion. A comparison of hydroxyquinoline in isoamyl alcohol. Agrawal (34 showed
ICP plasma emission and AAS was made by Ishii et al. (684 that absorption at 555 nm after complexation with 2-meth-
in studying Mn, Fe, Co, Ni, Cu, Zn, Cd, and Sr in shellfish, oxy-N-m-tolylbenzolhydroxamicacid could determine V in
who founcl matrix effects on calibration slopes for ICP. A fruits, vegetables, etc. Chelnokova et al. (274 demonstrated
method for multielement measurement in oils by direct as- that coprecipitation with antipyrine dye salts could recover
piration of a hydrocarbon solution into a plasma spectrometer traces of Co, Ma, Cu, and Zn from excesses of other elements
was given by Dijkstra et al. (374. before spark source emission spectrometry. Boron in plants
A modification of the AOAC procedure for mercury in fish and soil when measured by ICP emission was shown to cor-
which used a hot water bath open-tube digestionwas reported relate well with the Azomethine H method by Gestring et al.
by Duve et al. (4.24. Callum et al. ( 2 1 4 employed subtilisin (514. A study of dry ashing conditions to prepare vegetables
enzyme treatment to liquify tissue before extraction, clean- for Na and K analysk was made by Rowan et al. (1174. Patti
up-derivatization, and EC GC of methylmercury residues. et al. (1074 fused shellfish samples with Na202,precipitated
Margler et al. (854 separated methylmercury by TLC before hydroxides and, after ion exchange, measured technetium-99
pyrolysis and cold vapor absorption measurement. Milk by p counting. Abukawa et al. ( 1 4 succeeded in separating
products were combusted with oxygen in a sealed bomb before cesium-137 from rubidium on a Duolite C-3 column in a
liberation of Hg vapor and AAS in the work of Narasaki method for soil and food samples.
(1005). Dumarey et al. ( 4 1 4 pyrolyzed samples on quartz Fluoride in plants could be determined on alkaline fused
filter paper, collecting Hg on gold-coated sand which, after ash solutions with a commercial electrode after Eyde (46J)
a second adsorption-desorption from gold, was measured as masked aluminum with citrate. Fluoride traces in salt samples
cold vapor in a sitream of Nz. Hirano (614 discussed high could be measured by Kokubu et al. ( 7 5 4 with an electrode
values given by combustion-gold desorption methods vs. acid after concentration on a ZrIv-loaded cation exchange resin.
digestion. Levels of mercury in tuna fish were established by Allegrini et al. (54 looked at total diet composites for iodine
Ahmed et al. (45') who use pressure acid-digestion and then content by neutron activation analysis after removing C1 iin-
used H202with W radiation to destroy soluble or anics before terference by combustion and adsorption. Black et al. (10J
ASV from a gold (electrode. A colorimetric methoffor mercury discussed the effect of light on the stability of response of an
in fish was presented by Gras et al. (554 that titrated a iodide electrode. Milk was analyzed for total iodine by DPP
complex with di-p-naphthylthiocarbazoneat 510 nm to the after ashing and oxidation of iodate in a method by Curtis
same intensity as a known standard. A generation flask design et al. (324. In their use of an iodide electrode for milk
was given by Suddenorf et al. (1214 to introduce cold Hg measurements, Lacroix et al. (785) found that not enough SH
vapor into either an ICP plasma, AAS, or UV monitor. Ebdon groups were formed to interfere from conventional pasteu-
et al. (434 increased the atomic fluorescence detectability of rization. Yamanobe et al. (1394 combusted samples in oxygen
Hg vapor 10-fold by sheathing the stream in argon. Detection and converted iodine to 3-iodo-2-butanone which was sub-
limits of low picogram per milliliter were reported for Hg by jected to ECGC. McCurdy et al. (874 coprecipitated iod-
Tanabe et al. (1234 when the emission from a helium mi- ine-131 with CUIin assaying milk for that element. A modified
crowave plasma was monitored. method for bromide entailing conversion to 2-bromoethanol
Results for CLI,Mn, and Zn in beef were found to be in was presented by Stijve (1204 who shortened the analysis
agreement with rished solutions when Mohamed et al. (914 time. Momokawa et al. (925) analyzed fish-jelly for bromine
directly aspirated homogenized tissue into air-acetylene AAS. by titrating bromate formed after oxidizing the ash. Leuen-
Harnly et al. (604 described a technique of wavelength berger et al. (804 separated nitrate and bromide ions on
modulation wherein less sensitive lines were utilized to extend NH2-HPLCpackings using 210-nm UV detection. Nagayania
calibration ranges by orders of magnitude for Cu, Fe, K, Mg, et al. ( 9 7 4 extracted bromate from bread, adsorbed it on
Mn, Na, Zn, and Ca. Kobayashi et al. ( 7 3 4 managed to DEAE-Sephadex A25, and determined it by TLC after elution.
extend sensitivity for zinc analysis to below 1 ng/mL by Watanabe et al. (1374 determined bromate in bread by ion
correlating carbonate dehydrase activity with concentration. chromatography, utilizing column separation and concentra-
Zn in milk was determined by Chauhan et al. (265) who tion trapping to remove C1-, PO:-, and SO?- interference.
formed a complex with 4-(2,3-dihydroxy-4-pyridylazo)- Twenty anions, including NO3-, NO2-, and SCN- were sepa-
benzenesulfonic acid or its 5'-chloro derivative. Andoh et al. rated by Tanabe et i d . (1244 using paper chromatography
(64 digested food samples in acid in a microwave oven before who measured NO3- in vegetables. Methods for nitrate anid
AAS for Zn and Cu. Clement ( 2 9 4 reported overcoming nitrite in meat were reviewed by Pallotti et al. (1064. Frouiin
interferences in Mg analysis by using N20-C H2 flame AAS. et al. (494 also presented a review of NO; and NO, methods
Karapetian et al. (724 found that copper couli be determined in meat. Brugel(184 reviewed methodology for nitrates and
after ashing milk without interferences using 6-phenyl-2,3- nitrites in edible plants. Terada et al. (1314 measured NO3-
dihydro-l,2,4-triazine-3-thione. Iron in beer and beverages in vegetables by separating water extracts on Zipax SAX iin
was analyzed by Hoyle et al. (655) with the colorimetric 0.05 M KH2P04buffer and monitoring absorbance at 210 nm.
reagent 2,4,6-trisi-4-(4-sulfophenyl)-2-pyridyl-l,3,5-triazine, Thayer et al. (1324 compared a similar separation to chemical
whose complex absorbed at 607 nm. Mortatti et al. (934 methods for NO, anti NO, and found HPLC more sensitive.
adapted the 1,lO-phenanthroline reagent to a flow injection Tateo et al. (1304 looked at meat extracts by an ion chro-
method and could determine iron at rates up to 180 samples matographic method and found that high C1- amounts re-
per hour. O'Laughlin et al. (1055) separated Fe2+,Ni2+,Ni2" quired removal as an interference. A GC method using EC
and Ru2+complexes of this reagent by HPLC of the paired: detection was given by Tanaka et al. (1284 wherein nitrite
ions with alkanesidfonic acids. Garza-Ulloa et al. (504 studied in milk was reacted with 1-hydrazinophthalazine. Tanaka et
other metals for possible interferences in the measurement al. (1274 also reported on this reaction being applied to other
of iron in beer with ferrozine reagent. Gouda et al. (545') foods with GC flame ionization detection. Nitrate in vege-
studied N-substituted phenothiazines as indicators for redox tables was reacted with 2-sec-butylphenol and measured at
titrations with ceric sulfate of Fe2+,MeV, VIv, and organic 418 nm in a procedure by Tanaka et al. (1264. Both nitrite
species. A procedure for Ni in food, among other samples, and nitrate in foods were determined by Tanaka et al. (125J)
was given by Pihlar et al. (1094 who, after wet-ashing, per- who combined both aforementioned reaction methods, de-
formed voltamme try on the nickel-dimethylglyoxime complex rivatized the 4-nitro-2-sec-butylphenol with pentafluorobenzoic
deposited ton a mercury drop. acid, and performed GC analysis after cleaning up other or-
Eivazi et al. (444 utilized the catalytic action of Mo on the ganic volatiles that interfered. Noda et al. (1045) employed
KI-Hz02 reaction to determine this metal in an AutoAnalyzer HPLC separation of the hydralazine-nitrite reaction product
apparatus. Before graphite furnance AAS, Ni et al. (1025) and monitored reversed-phase column effluents with UV
extracted Mo from acid digests with N-phenylbenzohydrox- absorbance or fluorescence. Rauter et al. (1134 used reaction
amic acid. Lyons et al. (824 extracted Mo from plant acid with p-cresol, steam distillation, and colorimetry to determine

ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983 179R


FOODS

nitrate in vegetables. Chikamoto et al. (285) favored reacting and Tsai and Ockerman provide comparisons of three tech-
nitrite in food extracts with p-bromoaniline and CuCl with niques for measuring the water binding properties of meat
subsequent EC GC analysis for the 1-bromo-4-chlorobenzene (18K). A method has been proposed for measuring the water
formed. Nitrite in milk powders by chemiluminescence de- hydration capacity of plant protein material by the AACC
tection was compared to colorimetric measurement by Doerr (13K),and use is made of the proximity equilibrium cell for
et al. ( 3 9 4 who found no significant difference in results. rapid determination of sorption isotherms (6K),this technique
Doerr et al. ( 3 8 4 analyzed meats for nitrite content by has been applied to determining the Aw of intermediate
chemiluminescence, Griess reagent, and DPP, finding com- moisture foods, and results show that it is applicable over the
parable precision but superior sensitivity for the former me- Aw range of 0.40-0.98 (7K). Multon et al. (1OK)describe a
thod. A collaborative study on cheese was reported by Cas- fast method and equipment with which the activity of water
tegnaro et al. (245) for GC-chemiluminescence methodology in foods can be estimated in 5-10 min and Northolt and
for N-nitroso compounds. Fox et al. (474 discussed chemical Heuvelman provide a simple, inexpensive control method
effects of meat ingredients and sample treatments, e.g., HgClZ, (11K)for testing the water activity of foods which depends
charcoal, and Carrez reagents as they affected Griess, chem- on the visible liquefaction of salt crystals with appropriate,
iluminescent, and DPP NO2measurement. Fox et al. ( 4 8 4 specific Aw values. Inverse gas chromatography is used to
had covered the effect of ascorbate and C1- on nitrite deter- provide water sorption isotherms for sucrose and glucose a t
mination by Griess reaction. Bousset ( 1 4 4 noted the effect very low levels (17K)and a spectrophotometric method using
of HgClz added before Griess reaction and recommended a blue dextran 2000 solution was devised ( I K ) to measure the
determining free NOz- without it. Berger et al. ( 8 4 also amount of water sorbed by the starch granules in suspension
discussed interferences in NO3- and NO2-analysis due to the (the dextran being too large to penetrate the starch granules
complex composition of meat curing mixtures. as the granules sorb water). A method to measure the water
A new method for natural carbon-14 content of foods was holding properties of dietary fiber under physiological con-
published by Mueller e t al. ( 9 5 4 who absorbed COz from ditions using suction pressure across a dialysis membrane is
combustion in NaOH, formed BaC03, liberated C02 into given (14K)wherein solutions of compounds of known osmotic
1-aminopropan-2-01, and then counted the resulting 1,3- potential were used to create a suction pressure across the
bis-(2-hydroxypropyl)ureaby liquid scintillation. Nissenbaum membrane containing the fiber sample, thus permitting the
et al. (1034 applied a water analysis procedure to orange juice determination of the water holding capacity of the fiber at
to measure oxygen-18 and deuterium. Blouin et al. ( 1 2 4 each suction pressure.
succeeded in using a commercial blood gas analyzer to quantify Oshima et al. (12K)report an electrical conductivity method
C02 liberated from still wines. Yuen et al. (1404 ashed oil for estimating the total solids in milk, and near-infrared
samples in an oxygen bomb before determining total P with photoacoustic spectroscopy is applied to the determination
a molybdovanadate reagent. Daun et al. ( 3 5 4 compared O2 of moisture in some solid materials (3K). Mladek and Beran
bomb, perchloric acid, and saponification digestions as well (8K) discuss sample geometry, temperature, and density
as colorimetry, AAS, and emission methods to determine P factors in the microwave measurement of moisture and provide
in Canola oils. Nakai et al. (98J determined pyrophosphate examples of calculations and experimental data for the
in blanching solutions by stabilizing turbidity with manganous moisture measurement for selected foodstuffs and agricultural
reagent and reading a t 625 nm. Phytate from pea meal was products. The application of microwave on-line moisture
extracted with TCA solution by Cosgrove (308 and selectively monitoring of driers is described for low hydrated materials
eluted from an anion exchange column to separate it from (Le., 6-14% H20) with the microwave meter having the ca-
other phosphate esters. Hydrogen peroxide traces in milk were pability for providing effective control of a drier in an in-
detected by Matsubara et al. ( 8 6 4 who overcame a protein dustrial plant (5K).
turbidity problem when complexing with Ti(IV)-4-(2-
pyridy1azo)resorcinol reagent. Iwaida et al. ( 7 0 4 compared ORGANIC ACIDS
three methods for residual H202 in foods and judged the Refinements made to an enzymic method for acetate in wine
4-aminoantipyrine color reaction the most reliable. Im- and juice by McCloskey (40L) obtained official first action
provements in this color test were described by Ito et al. (694 AOAC status. Trombella et al. (62L)used formic acid satu-
who extended detection of peroxide down to 50 ppb. Toyoda rated carrier gas to improve the gas chromatography of acetic
et al. (1334 used an oxygen electrode apparatus to measure acid during direct wine injection. Isshiki et al. (22L)deter-
peroxide through liberation of oxygen by catalase. Total mined propionic acid in bread by direct GC of a dimethyl-
cyanide in cassava was determined by Ikediobi et al. ( 6 6 4 formamide-formic acid extract. Overall organic acids were
by incubating with linamarase, adding alkaline picrate, and measured by conductivity after adding excess imidazole or
heating to produce a color absorbing a t 490 nm. Hahn et al. 2-amnopyridine in the work of Okayama et al. (43L).
( 5 7 4 discussed two instrumental dissolved oxygen-in-beer Markwalder (36L)reviewed enzymic methods for lactic acid
analyzers, comparing their results to the indigocarmine me- in cheese. Ayroulet-Martin et al. (3L) applied Ling’s milk
thod. Buckee (194 presented a scheme for concluding if hops method for lactic acid to meat, calibrating to compensate for
had been sulfured that detected S and SO2 after adsorption imcomplete extraction. Littman et al. (34L) analyzed egg
on copper gauze and liberation for titration measurement. products for tricarboxylic and related acids including P-hy-
Boland et al. ( 1 3 4 gave ways of preparing food samples for droxybutyric using capillary GC after cleanup and methyla-
pH measurement, reporting collaborative data. tion. Dorsett et al. (15L) investigated the usefulness of a
Selectrode for citrate activity in plant samples. A fourfold
MOISTURE sensitivity increase was reported for an NADH enzymic
A useful reference for a better understanding of the be- technique for citrate in vegetables by Girotti et al. (18L).
havior, state, and interactions of water in food systems is Ester-bonded citrate in starches was determined by spectro-
provided by Rockland and Stewart (15K). Zuercher and photometry and titration by Klaushofer et al. (26L). Down
Hadorn report on the determination of water by the Karl to 4 kg of citramalic acid in vinegars could be found in TLC
Fischer method for approximately 90 different foodstuffs, method of Valdehita et al. (66L). Sponholz et al. (58L)gave
providing comparative data and recommending the most fa- their method to determine 2-hydroxyglutamates in wines and
vorable Karl Fischer variant for each food ( 2 0 ,and Jones musts. Kozukue (29L)separated a-keto acids as DNPH de-
et al. (4K)have optimized the automatic Karl Fischer titration rivatives on an Lichrosorb Si-60 HPLC column in 10 min.
for the determination of moisture in grain. Commercial vapor Small amounts of oxalate in plants were determined by Turner
pressure thermocouple psychrometers were adapted for rapid (63L) by measuring COz via GC after decarboxylation. D-
water activity (Aw) measurements for foods in the 0.99 to 0.60 (+)-Malate in fruit juices was determined a t the parts-per-
range using a two-step procedure (19K) with analysis time million level using D-(+)-malate NAD oxidoreductase in the
estimated to be 4 to 8 min. Methodology is described for work of Knichel et al. (28L). Klein (27L)separated the organic
determining unfreezable water in protein suspensions by acids of sauerkraut brine using isotachophoresis. Fukuba et
low-temperature NMR (2K) and NMR spectroscopy has also al. (17L)described their leading and terminating electrolytes
been applied to studying the internal movement and binding useful to separate acids in shellfish by isotachophoresis. Droz
of water in raw and roasted coffee and also of grounds (16K). et al. (16L)used cation exchange for cleanup before separation
Muffett et al. (9K)make use of differential scanning calori- of juice and wine acids on reversed-phase HPLC with 225 and
metry to measure the unfrozen and free water in soy proteins, 210 nrn monitoring. Brugman et al. (9L)separated aromatic
180R ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983
FOODS

and substituted cinnamic acids, among others, with silica spectrophotometric relationships. Beer polyphenols were
adsorption HPLC. Fruit juices were analyzed for tartaric isolated and separated by HPLC by Kirby et al. (25L) in
malic and citric acids by reversed-phase HPLC by Bigliardi studies on haze formation.
et al. (6L)who used refractive index detection. Several re- A scheme to separate complex phenolic mixtures was de-
versed-phase and ion exchange columns were investigated for scribed by Kaluza et al. (23L) using Sephadex CL-6B and
carboxylic acid separations by Buslig et al. (11L)for appli- Sephacryl 5-200 with continuous monitoring of effluents.
cation to different fruit, and food samples. A separation Their method for p1,ant phenolics was used by Horvat et ill.
scheme utilizing column, thin layer, and gas chromatographic (21L) to analyze instant tea and pecans wherein both me-
stages of analysis was described by Tonogai et al. (61L) for thylation and TMS reactions were carried out before GC or
fruit-derived foods. Marsili et al. (3715) quantified dairy GC-MS. Wood smoke used for meat curing was examined by
product acids by monitoring and eluent from an HPX-87 Borys (8L)for nitroslo and nitrophenols using HPLC after an
column at 220 and 275 nni. Rajakyla (46L)monitored gluconic XAD-4 cleanup. Wittkowski et al. (70L) fractionated the
acid formation in fermentation liquors, introducingthe sample mono- and dihydroxyphenolsbefore GC-MS of trimethylsilyl
onto cation exchange HPLC columns after filtration. Ushijima derivatives in an investigation of beechwood smoke concen-
et al. (65L) utilized a commercial carboxylic acid chromato- trate.
graph to measure soy sauce acids as postcolumn colored de- Phytic acid in rapeseed meal was examined by Uppstrom
rivatives. Malic acid in wines was measured in an automated et al. (64L) with color development after phytase treatment.
enzymic method reportled by Lonvaud-Funel et al. (35L). Tangkongchitr et al. l(60L)differentiated phytate phosphorus,
Many derivatives of hydroxycinnamic acid in cranberries inorganic P and P not precipated by Fe(+3) by different
were elucidated by Marwan et al. (39L) who employed UV treatments before colorimetry. Saio et al. (53L)isolated phytic
and visible spectrophotometry as well as paper and liquid acid from vegetable proteins by iron precipitation before
chromatography but no hydroxycinnamic-quinic esters were hydrolysis and phosphorus determination. Latta et al. (32L)
found. Okamura et al. (42L)related the phenolic cinnamates determined phytate in whole rapeseed by color decrease wiith
in white wine to the quality, using reversed-phase HPLC and an FeC1,-sulfosalicylic acid reagent. Cosgrove (12L) aliao
280-nm detection. Hydroxycinnamic-quinic esters in fruits discussed his work in the determination of phytate in flour
were separated and measured as TMS ethers on glass capillary and ground field pea seeds. Graf et al. (19L) used HPLtC
columns and also by direct HPLC in a study by Moeller et separation for phytate in wheat bran after initial resin column
al. (41L). Schulz et al. (55L) investigated spices for hydrox- isolation. O’Neill et al. (44L) measured phytate in cereals by
ybenzoic and hydroxycinnamic acids with both packed and Fourier NMR spectroscopy of phosphorus-31.
capillary column CC of ‘I‘MS derivatives. Tanabe et al. (59L) Glycyrrizic acid from licorice extracts was detected at 254
monitored their HPLC eluent at 315 nm to achieve more nm after separation on a C18 HPLC column by Bell (41,).
sensitive detection of total ferulate in rice bran oils. Several Martin et al. (38L) compared a TLC to an HPLC separation
phenolic glucosides of fruit including 1-0-hydroxycinnamyl- for glycyrrizic acid and found the latter superior. Vora (6815)
P-D-glucosides were reported on by Reschke et al. (47L) who analyzed licorice for glycyrrizic acid salts in a collaborative
did two-dimensional TLC and also HPLC of acetylated de- study of an HPLC method requiring less than 15 min time.
rivatives on silica gel. Natural benzoic acid levels in dairy The use of p-bromophenacyl bromide to derivatize sterioside
products down to 0.4 ppm were analyzed by Richardson et and rebaudioside for ti secondary HPLC separation after initial
al. (4%) with GC of the methyl ester. Dewaele (13L)reviewed TLC was detailed by Ahmed et al. (1L). Abscisic acid from
the analysis of hops and beer for bitter acids employing HPLC potatoes was methylated by diazomethane before GLC in woirk
techniques. Axcell et al. (2L) reported good correlation of by Karavaeva et al. I(%%). Cows milk was analyzed for the
conductometricmeasurements to direct near-IR measurement presence of hippuric acid using color development with 13-
of hop a-acids. Hautke (2OL)avoided emulsions in extracting dimethylaminobenzaldehydein a study by Wolfschoon-Pombo
a-acids with polyethylene strips contacting the solvent layers. et al. (71L).
Verzele et al. (671,) monitored 270 nm in their HPLC method
for beer bitter acids to minimize response differences of NITROGEN
separate a-acids. IJndesirable humulinic acids were separated Methods for total nitrogen, protein nitrogen, and its conn-
by gradient reversed-phase HPLC in model system experi- ponents as well as other nitrogen-containing compounds are
ments by Schulze et al. (56L). Lance et ai. (31L) analyzed continuously being studied and improved as indicated in this
hop extracts on Spherisorb 5 ODs, adding citric acid to the period’s literature. A reference method for total nitrogen in
mobile phase to reduce column adsorption. Several HPLC meat and meat products using the Kjeldahl procedure has
systems were investigated by Dewaele et al. (14L)for sepw- been issued by the British Standards Institution (IOM).
ration of six iso-a-acids before choosing an ion-pair mode. Studies on the use of titanium dioxide catalyst in Kjeldalhl
Belleau et al. (51,)showed the dimer of gallic acid to be UM- determinations for meat and meat products have been carried
natural to beer in a method utilizing normal-phase HPLC. out by Stamm et al. (109M) and as catalyst for the automatic
Off-flavors in beer due to trihydroxyoctadecenoic acids were KjelFoss instrument, by Williams et al. (128M); and botch
measured by GC after diazomethane reaction and silylation authors found this catalyst suitable. A similar test on oilseed
in work by Yabuuchi et al. (72L). samples by Davidsoii (19M) has indicated good agreement
The analysis of brandies for phenol compounds was re- between Kjeldahl and KjelFoss using titanium oxide catalyst.
viewed by Puech (45L). Somers et al. (5715)discussed the Various catalysts for Kjeldahl have been compared by Ug-
interference of SO2in staridard methods for phenolics in wine. rinovits (116M) who obtained good results on various foods
Roston et al. (51L) reviewed HPLC methods for monocyclic with the copper sulfate-potassium sulfate catalyst. A pro-
phenolic acids. These authors (50L) also showed the utility cedure for the quantitative determination of pure protein in
of electrochemical detection at +950 MV to monitor HPLC meat products has been described by Kaltwasser et al. (6611.0
effluents for phenolic acids in beer and whiskey. The same which used Kjeldahl determination of residual nitrogen after
authors (52L)then expanded the scope of oxidative detection removal of nonprotein nitrogen. The automated KjelF’oss has
with a dual electrode detector. Kr gier et al. (30L) investi- been found applicable to meat products by McGill (85M).
gated oilseed for free, esterified, anJbound phenolic acids by Improved sensitivity for colorimetry of micro-Kjeldahldigesits
TMS-GC. Wilson (69L) first extracted phenolics from apple has been achieved by Nkonge et al. (9OM) by modifying thie
juice on Sephadex LH-20 before subsequent, normal- and reagents and reaction conditions for the Berthelot reaction.
reversed-phase HPLC separations. Lea (33L) also studied Nessler’s reagent has been used by Van Ginkel et al. (12OM)
these compounds employing a shift in pH to enhance his for the determination of ammonia in plant digests by con-
separations on the column. Roberts et al. (49L) noted for- tinuous flow analysis. Sodium hypobromite has been used
mation of compounds similar to thearubigens in stored tea, in a potentiometric titration for nitrogen in meat products
using HPLC techniques. Total phenols in plant material by by Schillak (104M) arid by Von Lengerken et al. (125M). Thie
the Prussian Blue method were evaluated by Budini et al. coulometric titration of proteins in milk products has been
(IOL)who commented on interferences and applied the described by Brauner et al. (9M) using electro-generated
measurement to strawberries. Tannins from plants were bromite. Protein in meat has been determined by Cipriani
bound to hemoglobin to precipitate them in a photometric (15M) by distillation firom sodium sulfate solution and titration
method by Schultz et al. (54L). Billot (7L) oxidized phenolics of the distillate with hydrochloric acid; results are correlated
from vegetables with copper(I1) to determine them with with the Kjeldahl method. Dye binding with Amido Black
ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983 181 R
FOODS

10B has been used by Liuzzo et al. (79M) to determine protein the carbon dioxide produced. High-temperature short-time
in floc-producingsugars and by Bruhn et al. (12M)using C.I. hydrolysis has been compared with long-time moderate-tem-
Acid Orange 12 to determine protein in frozen dairy desserts. perature hydrolysis for foods by Lucas et al. @OM) who found
A method for the determination of cresol red index in oilseed the two procedures equivalent. A procedure for pretreating
residues has been published by the British Standards Insti- all amino acids with sodium hypochlorite has been developed
tution (11M). Immunoturbidimetry has been applied to the by Ishida et al. (63M) so that proline and hydroxyproline may
determination of proteins in foods by Gombocz et al. (40M). be determined with the other amino acids by HPLC of the
Proteins in fish or meat meals have been determined by phthalaldehyde derivatives. Reversed-phaseHPLC has been
Wright et al. (130M) by low-resolution pulsed NMR and by used by Kozukue et al. (70M) for the analysis of DNP de-
Rutar et al. (99M)and O’Donnell et al. (91M) by magic-angle rivatives of amino acids. Dansyl derivatives of amino acids
sample-spinning carbon-13 NMR. Heating a food sample with from food hydrolyzates have been determined by HPLC by
aluminum to form aluminum nitride followed by complexo- Khayat et al. (67M) and Hughes et al. (57M) who use po-
metric determination of the aluminum has been used by stcolumn reaction after HPLC. High-performancethin-layer
Vdovenko et al. (121M) to determine total nitrogen in food chromatography has been used by Yang (133M) to determine
products. Near-infrared spectroscopy has been compared with 20 amino acid phenylthiohydantoin derivatives in 1 h. A
dye binding by Biston et al. (8M) for estimating protein in review of the various isotachophoresis methods for amino acids
oat groats, both procedures compared satisfactorily with and peptides has been written by Holloway et al. (51M).
Kjeldahl. Descriptions of the use of NIR for protein and other Photometric determination of lysine, methionine, cysteine,
consituents in meats have been published by Hauser et al. and tryptophan after enzymic release has been described by
(47M) and Kruggel et al. (73M). The applications of NIR Hob (52M). Sulfur amino acids in protein hydrolysates have
analysis for protein in grains have been discussed by DeGroen been determined by Mackey et al. (83M) by reversed-phase
(20M) for barley and malt, by Hruschka et al. (55M) for chromatography of the Dns derivatives. Oxidized sulfur amino
ground wheat, by Williams et al. (127M) for hard wheat, and acids have been separated by Raymond et al. ( 9 6 m by ion
by Krischenko et al. (72M) for the analysis of grain and grain exchange chromatography. An arginine decarboxylase plug
products. Tkachuk (115M)has applied this procedure to the flow reactor has been utilized by Valle-Vega et al. (118M)to
analysis of whole wheat kernels. Conversion factors for protein measure L-arginine, and the same authors (119M) have de-
in milk have been calculated by DeLange et al. (21M),for food scribed an arginase-urease electrode for the same determi-
and agricultural samples by De Rham (23M),and for soybean nation. Betaine in sugar and wine has been determined by
protein products by Morr (86M). Vide et al. (122M)by liquid chromatography. A stopped-flow
A procedure for the assessment of protein digestability has method for the determination of cysteine and reduced glu-
been described by Gauthier et al. (34M), using enzyme hy- tathione has been described by Inouye et al. (61M) based on
drolysis and simultaneous dialysis. A review of procedures the reaction of the acids with 5,5’-dithiobis(2-nitrobenzoic
for the detection and estimation of collagen has been published acid). Thiols have been separated by Nakamura et al. (89M)
by Etherington et al. (28M). A method for the determination by anion exchange chromatography and postcolumn deriva-
of a suitable value for the colla en to protein ratio in chopped tization with o-phthalaldehydeand taurine. Specially purified
meats has been described by jailler (92M) using a modified L-methionine y-lyase has been used to determine L-cysteine
hydroxyprolineprocedure. Trinitrobenzene sulfonic acid and by Tanaka et al. (113M),methionine interferes. Monosodium
ninhydrin methods have been compared by Clegg et al. (16M) lutamate in foods has been determined by rapid HPLC by
for the assessment of protein degradation in cheese, and the bporns (108M). Methods for available lysine include an L-
TNBS method was preferred. Unreduced glutenin has been lysine enzyme electrode described by Skogberg (106M), an
extracted from wheat flour with sodium dodecyl sulfate by automated enzyme-photometric procedure by Holz (54M),
Danno (17M). The use of ion-exchange resins has been sug- a rapid dye-binding procedure with C.I. Acid Orange 12 by
gested by Satyanarayana et al. (103M) as an efficient means Hurrell et al. (59M),the use of the guanidination reaction by
of extracting proteins from oilseed flours. Ultra-thin-layer Maga (84M),and fluorimetric assay by Goodno et al. (41M)
electrophoresis has been applied by Georg et al. (37M,38M) using o-phthalaldehyde and P-mercaptoethanol. Lysine and
to the separation of legume seed proteins. Polyacrylamide nitrogen have been measured by Gill (36M) using infrared
gel electrophoresis has been described by Lauriere et al. (75M) reflectance, and good correlations with conventionalmethods
for the analysis of cereal prolamins and by De La Vigne (22M) obtained. Lysinoalanine has been determined by Fritsch et
for the analysis of cheese proteins and peptides. High-reso- al. (30M), in foods by use of an amino acid analyzer after
lution gel chromatography has been shown by Rutschmann hydrolysis, and detection with ninhydrin. Other methods for
et al. (IOOM) to separate protein fractions on a preparative lysinoalanine include HPLC which has been described by
scale. Bovine skim-milk proteins have been analyzed by Wood-Rethwill et al. (129M) and an amino acid analzyer
Dimenna et al. (25M)using high-performancegel-permeation technique with fluorimetric detection by Fritsch et al. (31M)
chromatography, and Barth (5M) has chromatographed hy- for both lysinoalanine and 2,3-diaminopropionicacid, and a
drolyzed plant proteins by using a high-performance size- method by Ishida et al. (62M) for lysinoalanine and lanthione
exclusion technique. Size-exclusion HPLC has also been using gas chromatography after esterification. Direct pho-
applied by Diosady et al. (26M) to the characterization of whey tometric determination of methionine and cyst(e)ine in en-
proteins. Reversed-phase HPLC has been used by Hancock zymic hydrolysates has been described by Holz (53M). Gas
et al. (45M)for the analysis of peptide and protein mixtures, chromatography has been used by Apostolatos et al. (2M) for
and improved peptide separations were obtained by deacti- the determination of methionine in proteins and plant ma-
vation of the hydroxysilyl groups on the column (46M). terials. The determination of methionine with L-methionine
Dipeptide mixtures have been analyzed by Lin et al. (78M) y-lyase has been described by Tanaka et al. (114M). Fluo-
by ion-pair HPLC and identified by gas chromatography-mass rometry has been used by Jones et al. (64M) to determine
spectrometry. The different ratios of sulfhydryl/disulfide 3-methylhistidine in meat products after hydrolysis and
groups in whey protein and a-casein has been used by fluorescamine treatment. Selenocystine, cystine, and cysteine
Mrowetz et al. (87M) to determine whey protein in mixtures. have been determined by Grier et al. (42M) by cathodic
Quantitative isoelectric focusing has been applied by Munroe stripping voltammetry. Methods for tryptophan include direct
et al. (88M) to the separation of wort and beer proteins. fluorescence or fluorescence after reaction with formaldehyde
Rattenbury (95M) has edited a book on amino acid analysis. which has been described by Steinhart ( I I I M ) , colorimetry
Two-dimensional TLC and HPLC have been described by with an iron chloride-copper chloride mixture suggested by
Barcelon (4M) as a means of separating free amino acids as Hu et al. (56M), and spectrophotometry and HPLC which
their 5-dimethylaminonaphthalene-1-sulfonyl derivatives. have been compared by Devries et al. (24M). The effect of
HPLC has also been used by Camerlynck et al. (14M)for the variations in hydrolysis techniques on the determintion of
determination of free amino acids in vegetable tissues as the tryptophan has been examined by Lucas et al. (81M).
phenylthiohydantoin derivatives. The free amino acid pool A creatinine-specific enzyme electrode has been described
of the potato has been analyzed by Golan-Goldhirsh et al. by Guilbault et al. (43M) using creatinase. Primary and
(39M)and y-aminobutyric acid and ornithine were positively secondary amines in marine organisms have been determined
identified by GC-MS. A method for total a-amino acids in by Lin et al. (77M) by conversion to the “dabsyl” derivatives
orange juice has been described by Drawert et al. (27M) using and HPLC after reaction with dinitrofluorobenzene. Aliphatic
the reaction with ninhydrin and titrimetric determination of secondmy amines have been determined by Bellati et al. (7M)

182R ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983


FOOClS

by HPLC after reaction with dinitrofluorobenzene. Glass VITAMINS


capillary as chromatography has been described by Hamano Improved and rapid methods for the individual vitamins
et al. (44bfor the detection of secondary amines in foods and for mixtures of vitmins represent the majority of methods
after formation of benzenesulfonyl chloride derivatives. described in the literature in the past 2 years. Methods for
Amines in pure-milk bacteria cultures have been determined vitamin A in fortified milk powders have been described hy
by Hladik et al. (49M) by TLC after formatipn of the 2,4- Woollard et al. (82w1, for vitamin A and @-carotenein pizza
dinitrophenyl derivatives. Volatile amines in wnes have been by Kame1 et al. (28N),and for vitamin A, carotene, and vi-
detected by Daudt et al. (18M) by gas chromatography with tamin A isomers in cheese by Stancher et al. (68N),all w e
a nitrogen detector after distillation and derivatization with HPLC for the measurement of the vitamins after various
trifluoracetic anhydride. Careful attention to conditions for cleanup steps. Wi gins et al. (81N)have determined vitamins
extraction has been described by Kim (68M) as providing an
improved method for the determination of trimethylamine
t
A and D in foods y HPLC after preliminary separation on
a dry alumina column. Direct injection of a diluted oil solution
and trimethylamine oxide. Trimethylamine in egg has been has been used by Vincenzini Foppa (79N) for the determi-
determined by Hobson-Iprohock @OM) by GC after freeze- nation of vitamins A and E by HPLC. Gel permeation
drying. An improved method for the analysis of trimethyl- chromatography, followed by reversed-phase HPLC chro-
amine in fish has been described by Bullard et al. (13M) who matography has been developed by Landen (37N) for thLe
recommend the cold method of extraction to help eliminate determination of retinyl palmitate and a-tocopherol acetate
interferences. Three methods for volatile bases in fishery in infant formulas. Simple HPLC methods for vitamins A,
products have been compared by Gallardo et al. (33M) and E, and B6 in oil have been described by Capuano et al. (7Aq
problems due to sample hydrolysis noted. Biogenic amines who determine A and E by one system and B, by another. Thie
have been determined by Zee et al. (134)in beer by automated use of different methanol-containing mobile phases has been
ion exchanger, by Peckaiiek et al. (93M), in cheese and fish proposed by Landen (36N) for the HPLC determination of
on an amino acid analyzer, by Hurst et al. (60M), in chocolate several fat-soluble vitamins, including vitamin A esters, CY-
by HPLC, and in wine by HPLC by Froehlich et al. (32M). tocopherol acetate, and vitamins D2 and D3. In a review by
This technique has also been applied by Scudamore (I05M) Parrish (55N) methods for the determination of vitamin 13
to the determination of 2-aminobutane in potatoes. Gas in foods are discussed. Vitamin D in the unsaponifiables of
chromatography has beein used by Yamamoto et al. (132M) margarine has been determined by Van Niekerk et al. (77AT)
for the analysis of putriescine, cadaverine, spermine, and by repeated chromatography on HPLC systems. Two-step
spermidine in foods after reaction with ethyl chloroformate HPLC has been described by Okano et al. (53") as a proce-
and by Staruszkiewicz et al. ( 1 1 O M ) to the determination of dure for vitamin D2in fortified dried milk. Another procedure
putrescine, cadaverine, and histamine using their perfluoro- for vitamin D in milk, margarine, and infant formuals has been
propionyl derivatives. An automated fluorimetric method for proposed by Thompson et al. (72N) using preliminary column
histamine in fish has been proposed by Luten (82M). Hist- clarification followed by HPLC. Mouillet et al. (49N) have
amine has also been determined in fish by Rubach et al. (98M) determined vitamin I& and D3 in the unsaponifiables of milk
by capillary isotachophoresis, and by Volk et al. (124M) by also by HPLC. A single column HPLC procedure for vitamin
HPLC of methanol extracts. Methods for histamine and D, and D3 in milk has been described by Muniz et al. (501\r?
tyramine in dairy products have been described by Suhren after preparation of the unsaponifiables and aluminum oxide
et al. (112M) using fluorometric detection. Tyramine in columm cleanup. Vitamin D3 sulfate has been found in milk
fermented food products has been determined by Yamamoto by Asano et al. ( I N ) by extraction, precipitation as the barium
et al. (131M) using gas chromatography, by Santos-Buelga et salt, and TLC and HPLC. Vitamin D2 and D3and their
al. (102M) using sand column chromato raphy and fluoro- isomers have been resolved by Zonta et al. (84N) in the
metry, and by Kostyukovskii et al. ( 7 1 3 using TLC of the presence of other fat-soluble vitamins by HPLC.
didansyl derivative. Tyrosine has been determined in potatoes The determination of tocopherols by HPLC has been de-
by Samotus et al. (101M)using a modified Millon's reaction. scribed by Rugraff et al. (64N) who have separated four to-
Aromatic amines in synthetic food colors have been deter- copherols, by Manz et al. (46N) using fluorimetric detection,
mined by Hunziker et a1 (58M) using HPLC. and by Gerz et al. ( 2 2 w who have separated tocopherols and
A method for ammonia is cheese after deproteinization has tocotrienols, and Cooirs et al. (9N) describe a similar separa-
been described by Behririger et al. (6M), and four methods tion. Other HPLC methods have been proposed by Deldime
for determining ammonia in meat roducts have been studied et al. (13") also for tocopherols and tocotrienols and Taylor
by Gerhardt et al. (35M). Methofs for caffeine using HPLC' et al. (70N) who have analyzed a number of edible oils for
have been described by F'errara et al. (29M) and applied to these constituents. Cortesi et al. (ION) have separated the
decaffeinated coffee by Lehmann et al. (76M) for coffee and tocopherols from the unsaponifiables by TLC followed b:y
caffeine containing foods using extraction, clarification, and HPLC. A standard method for tocopherols in oils has been
UV measurement, by Ballassat-Millet et al. (3M) for tea and published by IUPAC (27N) consisting of a TLC separation
cola using HPLC, and by <Juergenset al. (65M) for cocoa who followed by colorimetry or GC determination of the individual
compared spectrophotometric and HPLC measurement of tocopherols. Tocopherols have been determined by po-
theobromine and caffeine. Chromatographicmode sequencing larography using a micro-flow-through detector by Loeliger
has been applied by Reid et al. (97M) to the analysis of et al. (41N). A chemiluminescence technique has been de-
caffeine and theobromine in beverages. HPLC with electro- veloped by Yurchenko et al. (83N) for tocopherols in oila.
chemical detection has been used by Sontag et al. (107M) for HPLC has been used by Tanabe et al. (69N) for preliminary
the determination of caffeine, theobromine, and theophylline separation of tocotrienols, followed by TLC purification and
in tea, coffee, cocoa, and beverages. The structure of theo- mass spectrometric detection.
bromine derivatives from cocoa powder after fumigation with Procedures for determining vitamin K have been reviewed
ethylene oxide has been determined by Pfeilsticker et al. (94M) by Parrish (56N). Reiflectance spectrometry after TLC sep-
by TLC, UV, and mass spectrometry. Identification of 7 - aration has been applied by Ersoy et al. (17N) to the deter-
methylxanthine in cocoa iroducts has been achieved by Ale0 mination of vitamin K, a-tocopherol,and @-carotenein spinach
et al. ( I M ) , by HPLC andUV. Total content of purine com- extracts. Manual and semiautomatic methods for vitamin K,
pounds in foods has been measured by Vojir et al. (123M)after have been described by Hassan (24N),based on reactions with
digestion, conversion to xanthines, and enzymic determination. piperidine and malononitrile with no interference from vitamin
Hypoxanthine in fish has been determined by Wartheson et K1 and K2. A simple colorimetric test with sodium ethoxide
al. (126M) by an HPLC pirocedure. Quaternary alkaloids in for vitamin K1 in vegetable oil has been presented by Hughes;
mushrooms have been identified by Unger et al. ( 1 17M) by (26N). Phosphatidylcholine has been determined in soy
chromatography/secondary ion mass spectrometry. An en- lecithin by HPLC by Rhee et al. (58N) and by Nasner et al.
zymic peak shift technique has been applied by Kusuwi et al. (51N). Press et al. (5710 have compared HPLC determination
(74M) to the measurement of 5'-ribonucleotides in foods. and proton-nuclear magnetic resonance determination of
Acid-soluble nucleotides 1 n milk have been determined by phosphatidylcholine in soya lecithin and found good corre.
Hernandez et al. (48M) by improved enzyme methods which lation. Four ion-exchange resins and nine enzymes have been
agreed well with an ion-exchange chromatographic procedure. evaluated for use in the AOAC thiamin method by Ellefsori
Potato glycoalkaloidshave been analyzed by King (69M) by et al. (16N) who found Bio-Rex 70 resin and Rhozyme SI
GLC of the alkaloid components. enzyme satisfactory. The use of thiamine pyridinylase to

ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983 183R;


FOODS

prepare a thiamine-free blank solution has been proposed by by Matsumoto et al. (48N) for determining L-ascorbic acid
Kennedy et al. (32"). Thiamine in meat has been determined in food. An amperometric enzyme electrode has been used
by Kurzawa et al. (35N) by the induced sodium azide-iodine by Macholan et al. (45N) to measure ascorbic acid in flowing
reaction which is claimed to be as sensitive as the thiochrome streams. Kelly et al. (31N) have used the decrease in ab-
reaction. The use of benzenesulfonyl chloride to prepare sorbance after ascorbate peroxidase treatment as a means of
blanks for the AOAC thiamine method has been proposed by estimating ascorbic acid. A similar procedure has been de-
Soliman (67N), and the procedure has been automated. scribed by Tono et al. (73N). Titration with potassium 2-
HPLC for thiamine and riboflavine has been described by iodosobenzoate has been described by Verma (78N) for as-
Bognar (5N) using spectrofluorimetricdetection for riboflavine corbic acid, and procedures for analyzing mixtures containing
and for thiamine after conversion to thiochrome. Another cysteine, glutathione or methionine were listed. A similar
HPLC method for thiamine and riboflavin described by titrant, phenyl iodosoacetate, has been used by Vaidya et al.
Kamman et al. (29N) determines both vitamins by UV de- (74N) for the determination of vitamin C in fruits. Dithio-
tection at 254 nm. Riboflavin and flavin mononucleotide have threitol has been used by Beutler et al. (4N) to reduce deh-
been analyzed in foodstuffs by HPLC with fluorometric de- ydroascorbic acid to ascorbate which is determined by colo-
tection by Lumley et al. (43N). rimetry of the tetrazolium salts. Both L-ascorbic acid and
Niacin, riboflavine, and thiamine in foods have been de- dehydroascorbic acid have been determined by Rubach et al.
termined by Skurray (66N) using HPLC with spectrophoto- (62N) using isotachophoresis. A procedure for choline in plant
metric determination for niacin and fluorometric detection protein sources has been described by Atwal et al. (2N) using
for riboflavine and thiamine which is first oxidized to thio- a variation of the reineckate method. A review of automated
chrome. Ion-pair HPLC has been described by Kitayama et methods for the analysis of water soluble vitamins using the
al. (33N) as a method for the separation of nicotinamide and AutoAnalyzer I1 has been published by Roy (61N). Appli-
nicotinic acid in foods. The polarographic behavior of nico- cation of pyrolysis gas chromatography after thin-layer
tinamide has been studied by Kobori et al. (34N) and been chromatography to the determination of some water-soluble
found useful for the detection of small amounts of the vitamin vitamins has been described by Lyle et al. (44N).
in foods. A symposium on methods in vitamin B, nutrition
edited by Leklem et al. (39N) included chemical, enzyme, and MISCELLANEOUS
automated methods. Vitamin B6 has been determined by A review is given of the scope of the application of 13C mass
HPLC by Gregory et al. (23N) after formation of derivatives spectrometry in food analysis (28P). The application of
with semicarbazide and by Lim (40") who has compared, chemiluminescence of a Cypridina luciferin analogue to im-
HPLC, GC, and microbiological methods and found HPLC mobilized enzyme sensors for determining hydrogen peroxide,
to be the most satisfactory procedure. Two columns have been xanthine, hypoxanthine, glucose, cholesterol, or uric acid is
used by Vanderslice et al. (75N)to measure low concentrations presented by Kobayashi et al. (18P) along with optimized
of B, vitamins in food extracts, and the procedure has been conditions for analysis and a review is given of analytical
automated (76N). Spectrophotometry has been proposed by applications of immunochemicalprocedures for food analysis
Marzo (47N) as a means of determining pyridoxine in oils. (16P). HPLC procedures are provided for the analysis of plant
Folic acid in fortified foods has been determined by HPLC hormones from soy (IOP)and for the analysis of several un-
by Hoppner et al. (25N) using reversed-phase chromatography conjugated pterins from various foods (19P). Gradient HPLC
after extraction and purification on a DEAE column, and procedures are reported for the estrogens genistein and da-
folacin derivatives have been determined by Day et al. (12N) idzein, their glycosides, genistin and daidzin, and also for
by HPLC and postcolumn fluorogenic oxidative derivatization. coumestrol (20P),and Ettre (8P) reviews special sampling
In situ paired-ion HPLC has been described by Reingold et techniques (i.e., purge and trap and equilibrium headspace
al. (59N) to separate biologically significant forms of folate. methods) which permit the extension of the lower detection
Pantothenic acid in foods has been determined by Tesmer limits of gas chromatography. Analytical methods are given
et al. (71N) by GC after extraction and hydrolysis to pan- (26P) for separating and determining the main constituents
tolactone. A multitude of methods have been published this in chewing gum (waxes, alkanes, glycerides, rosin derivatives,
period on the determination of ascorbic acid. Isocratic HPLC polyvinyl derivatives, and elastomers) and Noble et al. (21P)
has been described by Dennison et al. (14N) for the deter- provide a novel method for the routine determination of
mination of ascorbic acid and combined ascorbic acid- protein, fat, and lactose in milk by use of a liquid scintillation
dehydroascorbic in beverages and by Carnevale (8N)for as- counter. Arneth (3P) describes simple and rapid methods for
corbic acid, sorbic, and benzoic acid in citrus juices. Phos- determining moisture, fat, and protein in meat and meat
phate-containingeluants for HPLC have been used by Watada products.
(80N) for the determination of ascorbic acid in vegetables, by
Shaw et al. (65N) for measuring ascorbic acid in tropical fruits, ACKNOWLEDGMENT
by Rose et al. (60N) to determine ascorbic and dehydro-
ascorbic acid, and by Lookhart et al. (42N) to determine The authors wish to thank Ms. J a y m E. Maher for typing
ascorbic acid in flours, and bread dough, by Geigert et al. and collating this manuscript.
(20N) to measure L-ascorbic acid and D-isoascorbicacid in fruit
juices, and Doner et al. (15N) have applied the procedure to LITERATURE CITED
the separation of ascorbic acid, erythorbic acid, dehydro-
ascorbic acid, dehydroerythorbic acid, dioxogulonic acid, and ADDITIVES
dioxogluconicacid using UV and refractive index detection.
HPLC with 6-alanine-sodium chloride elution has been (IA) Aifonso, F. C.; Martin, G. E.; Dyer, R. H., J . Assoc. Off. Anal. Chem.
1980, 63,1310.
proposed by Floridi et al. (19N) for the determination of (2A) Ang, K. P.; Kwik, W. L.; Mok, K. F., J . Singapore Natl. Acad. Sci.
ascorbic acid in foods and good agreement found with other 1979, 8 ,72; Chem. Abstr. 1982, 96,33446K.
methods. Reductones have been measured by HPLC by (3A) Archer, A. W., Anal. Chim. Acta 1981, 128, 235.
Obata et al. (52N) using sodium nitrate as eluant. Ion-pair (4A) Austin, R. E.; Wyatt, D. M., J . Am. Oil Chem. SOC. 1980, 57, 422.
HPLC has been applied by Rueckemann (63N) to the de- (5A) Bajardi, M. L.; Giannoia, L. I.; Giammona, G . , Riv. SOC.Ital. Sci. Aii-
ment. 1982, 1 1 , 105; Chem. Abstr. 1982, 97, 143207m.
termination of L-ascorbic acid in fruits and vegetables, by (6A) Brieskorn, C. H.; Mahimeister, K., Z . Lebensm .-Unters. Forsch. 1980,
Parolari (54N) to analysis of meat for ascorbic acid, by Au- 171,348.
gustin et al. (3N) to the determination of ascorbic acid in (7A) Burkhardt, R., Dtsch. Lebensrn.-Rundsch. 1981, 77,97.
potato products, by Coustard et al. ( 1 1 N ) to the separation (EA) Chretien, D.; Perez, L.; Sudraud, P., Connaiss. Vigne Vin. 1979, 13,
of ascorbic and isoascorbic acids, and by Keating et al. (30N) 311; Anal. Abstr. 1981, 4 0 , 3F79.
(9A) Coillnae, A,; Noirfalise, A,, Anal. Chim. Acta 1980, 121, 337.
to the same two vitamins using precolumn derivatization. (IOA) I b i d , 1981, 132,201.
Ascorbic, dehydroascorbic,and diketogulonicacids have been ( I l A ) Cornet, J. P.; Van de Haar, G., Chromatogr. Sci. 1982, 20, 343;
resolved by Finley et al. (18N) on two HPLC columns with Chem. Abstr. 1982, 97,37598e.
phosphate buffers as eluants. Polarography as a means of -
112AI DeSiena. A.: Jacobs. E.: Romaanoii. R.. J . Assoc. Off. Anal. Chem.
1981, 6 4 , 226.
determining ascorbic acid has been described by Valenta et ~

al. (38N) who use carbon paste and platinum electrodes, by (13A) Fang, C.; Yi, Q. Pan, K., Fenxi Huaxue 1981, 9 ,595; Chem. Abstr.
1982, 96,120994f.
Gerhardt et al. (21N) by differential pulse polarography, and (14A) Faugere, J. G., Ann. Faisif. Expert. Chim. 1979, 72,227; Anal.
by Branco (6nr). An ascorbate electrode has been proposed Abstr. 1980, 39,3F19.

184R ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983


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ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983 185R1


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186R ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983


FOODS

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1R7iP3n
.'-r.
(58D) Piergiovanni, L.; Volonterlo, G. Rlv. Ktlc. Enol. 1980, 33,289; Anal. (1OF) Bernard, J. L.; Sims, L. G., Ind. ResJDev. 1980, 22, 81; Cheni.
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(70D) Unterhalt, B. 2.Lebensni-Unters. Forsch. 1980, 170,425. Anal. Abstr. 1981, 4 0 , 3F87.
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1980, 306; Anal. Abstr. 1982, 42,3F53. (24F) Cortesi, N.; Ponziani, A.; Fedeli, E., Rlv. Ital. Sostanze Grasse 198.1,
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(40F) Gilbert, J.; Startin, J. R., J. Chromatogr. 1980, 189, 86. (99F) Stefanov, K.; Selzova, K., Maslo-Sapunena Prom-st. lS81, 77, 19;
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190R ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983


FOODS

(37G) Jennings, W. G.; Shibamoto, T., “Qualltative Analysis of Flavor and (92G) Vernin, G., “Chemistry of Heterocyclic Compounds in Flavors and
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15, 143; Chem. Abstr. 1982, 97, 71040b. (6H) Brause, A. R.; Raterman, J. M., J. Assoc. Off. Anal. Chem. 1982, ($5,
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(58G) Noda, Y.; Nakano, M., Nippon Shoyu Kenkyusho Zasshi 1979, 5, 299; (14H) Dikeman, E.;Pomeranz, Y.; Lai, F. S.,Cereal Chem. 1982, 59, 139.
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(59G) Oberdieck, R., Dtsch. Lebensm.-Rundsch. 1981, 7 7 , 63; Anal.
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(17H) Douglas, F. W., Jr.; Tobias, J.; Groves, M. L.; Farreii, H. M., Jr.; Ed-
(60G) Okamoto, M.; Ohtsuka, K.; Imai, J.; Yamada, F., J. Chromatogr. mondson, L. F., J. Dairy Sci. 1982, 65, 339.
1981, 219, 175.
(18H) Fincke, A., Dtsch. Lebensm-Rundsch. 1980, 76, 187.
(61G) Ohta, N.; Kuwata, G.; Akahori, H.; Watanabe, T., Nippon Shokuhin (l9H) Ibid., 1980, 7 6 , 3134.
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(62G) Parliment, T. H.; Spencer, M. D., J. Chromatogr. Scl. 1981, 19, 435. ’ 1982, 9 6 , 5111d. .
(63G) Petro-Turza, M.; Szarfoldi-Szaima, I., Acta Aliment. 1982, 1 1 , 75; (21H) Hadorn, H., CCB 1980, 5,26; Chem. Abstr. 1981, 9 4 , 289631.
Chem. Abstr. 1982, 97, 54079d. (22H) Herrmann, A.; Loetscher, E.; Wagmann, M., Mitt. Geb, Lebensmittel-
(64G) Pickenhagen, W.; Veiiur, A,; Passerat, J. P.; Ohioff, G., J. Sci. Food unters. Hyg. 1982, 73, 121; Chem. Abstr. 1982, 9 7 , 48982.
Agric. 1981, 32, 1132. (23H) Hlchcock, C. H. S.;Bailey, F. J.; Crimes, A. A.; Dean, D. A. G.; Davis,
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(66G) Postei, W.; Meier, B., 2.Lebensm.-Unters. Forsch. 1981, 173, 85; (24H) Hohfeld, K.; Pietsch, H. P., Nahrung 1981, 25, K23; Chem. Abstr.
Anal. Abstr. 1982, 42, 2F43. 1981, 95, 95557k
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(68G) Radtke-Granzer, R.; Piringer, 0. G., Dtsch. Lebensm.-Rundsch. 1981, 73.
77, 203. (26H) Human, J.; Khuyat, A., J. Food Sci. 1981, 46, 868.
(69G) Reindi, 6.; Stan, H. J., J. Agric. Food Chem. 1982, 30, 849. (27H) Iida, H.; Tokunaga, T.; Nakamura, K., Tokai-ku Suisan Kenkyusho
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(74G) Schreier, P., “3rd Weurrnan Symposium Proceedings of the Interna- (30H) Jebsen Haave, I.J.; Aaivik, E., Arch. Lebensmittelhyg. 1980, 31, 16;
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(75G) Ibid., J. Agric. Food Chem. 1980, 28, 926. Toxlcol. 1981, 74, 5291; Anal. Abstr. 1982, 43, 4F28.
(76G) Shankaranarayana, M. L.; Abraham, K. 0.; Raghavan, 6.; Natarajan, (32H) Juarez, M.; Martinez-Castro, I., Grasas Aceites (Seville) 1981, 32, 913;
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(79G) Sponhoiz, W. R., Z. Lebensm.-Unters. Forsch. 1982, 458. (34H) Kaffka, K. J.; Kuicsar, F., Acta Allment. 1982, 1 1 , 47.
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(82G) Tateo, F.; Redaeiil, V., IUv. SOC. Ital. Sci. Ailment. 1980, 9 , 427; 1981, 173, 468.
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(846) Toth, L., Fleischwirtschaff 1980, 60, 461; Anal. Abstr. 1981, 41, (39H) King, N. L.; Kurth, L.,J. Food Sci. 1982, 47, 1608.
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(85G) Ibid. 1980, 60, 728; Anal. Abstr. 1981, 41, 1F28.
(86G) Tressi, R.; Gruenewald. K. G.; Silwar, R.; Chem., Mikrobloi., Technol. (41H) Krzynowek, J.; Wiggin, K., J. Assoc. Off. Anal. Chem. 1981, 64,
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(42H) Kuhlmann, F., Dtsch. Lebensm.-Rundsch. 1979, 76, 390.
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(88G) Varga-Puchony, 2.; Vigh, G.; Hiavay, J.; Petro-Turza, M.; Szarfoldi- (44H) Leegwater, D. C.; begwater, J. A., J. Sci. Food Agric. 1981, 3.?,
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(90G) Ibid., Lebensm.-Wiss. ‘Technol. 1980, 13, 78; Anal. Abstr. 1981, Geb. Lebensmittelunters. Hyg. 1980, 71, 206; Anal. Abstr. 1981, 40,
4 1 , 2F83. 1C44.
(91G) Ibid., Z. Lebensm-Unters. Forsch. 1981, 172, 460; Anal. Abstr. (46H) McHard, J. A,; Fouik, S. J.; Jorgensen, J. L.; Bayer, S.; Winefordner, ,J,
1982, 42, 1F55. D., ACS Symp. Ser. 1980, No. 143, 363.

ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983 191 R


FOODS

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1288. . . - , 435.
172. . - -.
(45L) Puech, J. L., Bull. Llalson-Group8 Polyphenols 1980, 465; Anal. Abstr. (31M) Ibld., 1981, 773,101.
1982, 42,2F46. (32M) Froehlick, D.; Battaglia, R., Mltt. Geb. Lebensmlttelunters. Hyg. 1980,
(46L) Rajakyla, E., J . Chromatogr. 1981, 278, 695. 77,38; Anal. Abstr. 1980, 39,3F63.
(47L) Reschke, A.; Herrmann, K., 2. Lebensm.4nter.s. Forsch. 1981, (33M) Gailardo, J. M.; Lopez-Benito, M.; Pastoriza, L.; Gonzalez, P., I n f .
773,458. Tec. Inst. Invest. Pes9. (Barcelona) 1979, 65, 15; Anal. Abstr. 1981,
(48L) Richardson, R. K.; Gray, I. K., N.Z.J Dalry Scl. Technol. 1981, 76, 40, 2F26.
179; Chem. Abstr. 1981, 95, 1487829. (34M) Gauthier, S. F.; Vachon, C.; Jones, J. D.; Sovoie, L., J . Nutr. 1982,
(49L) Roberts, G. R., Fernando, R. S. S.; Ekanayake, A,, J . FoodScl. Tech- - . . .-.
, 9 , 1718
1, 1
no/. 1981, 78,118; Chem. Abstr. 1981, 95,95695d. (35M) Gerhardt, U.; Quang, T., Fleischwirtschaft 1979, 59,946; Anal. Abstr.
(50L) Roston, D. A.; Kisslnger, P. T., Anal. Chem. 1981, 53, 1695. 1980, 39,6F30.
(51L) Ibid., J . Li9. Chromatcgr. 1982, 5 , 75; Anal. Abstr., 1982, 43, 3G5. (36M) Gill, A. A.; Starr, C.; Smith, D. B., J . Agric. Scl. 1979, 93,727; Anal.
(52L) Ibld., Anal. Chem. 1982, 5 4 , 429. Abstr. 1981, 40, 5G3.
(53L) Saio, K.; Hondo, M., Shokuhln Sogo Kenkyusho Kenkyu Hokoku 1979, (37M) Goerg, A,; Postel, W.; Westermeier, R.. Z . Lebensm-Unters Forsch.
4 8 ; Chem. Abstr. 1981, 94,82281r. 1982, 774,282.
(54L) Schultz, J. C.; Baidwin, I.T.; Nothnagle, P. J., J . Agrlc. Food Chem. (38M) Ibld., 1982, 774,286.
1981, 29,823. (39M) Golan-Goidhirsh, A,; Hogg, A. M.; Wolfe, F. H., J . Agric. FoodChem.
(55L) Schulz, J . M.; Herrmann, K., J . Chromatogr. 1980, 795,95. 1982, 30,320.
(56L) Schulze, W. G.; Ting, P. L.; Henckel, L. A.; Goldsteln, H., J . A m . SOC. (40M) Gombocz, E.; Hellwig, E.; Petuely, F., Z . Lebensm-Unters. Forsch,
Brew. Chem. 1981, 39, 12; Anal. Abstr. 1982, 42,6F50. 1981. 772.355.
(57L) Somers, T. C.; Zlemells, G., J . Scl. Food Agric. 1980, 37,600. f4lM)- Goodno. C. C.: Swaisaood. H. E.: Catianani, G. L.. Anal. Blochem.
I

(58L) Sponholz. W. R.; Wuensch, B.; Dlttrlch, H. H.. Z . Lebensm-Unters. ' 1601, 115,203.
Forsch. 1981, 772,264. (42M) Grier, R. A,; Andrews, R. W., Anal. Chlm. Acta 1981, 724,333.
(59L) Tanabe, K.; Tanaka, A.; Kato, A., Yukagaku 1981, 30, 512; Chem. (43M) Guilbault, G. G.; Chen, S. P.; Kuan, S. S.,Anal. Lett., Part B 1980,
Abstr. 1981, 95, 1310490. 73,1607; Anal. Abstr. 1981, 4 7 , 3D184.
(60L) Tangkongchitr, U.; Seib, P. A.; Hoseney, R. C., Cereal Chem. 1981, (44MI Hamano. T.: Mltsuhashi, Y.: Matsukl, Y., Agric. Biol. Chem. 1981,
58,226. ~ 4 5 , 2237.
(61L) Tonogai, Y.; Ito, Y.; Iwaida, M., BunsekiKagaku 1982, 37,E69; Anal. (45M) Hancock, W. S.; Capra, J. D.; Bradley, W. A,; Sparrow, J. T., J .
Abstr. 1982, 43,4F6. Chromatogr. 1981, 206, 59.
(62L) Trombella, B.; Ribeiro, A., A m . J . Enol. Vitlc. 1980, 37,294; Anal. (46M) Hancock, W. S. Sparrow, J. T., Ibid. 1981, 206, 71.
Abstr. 1981, 47,5F57. (47M) Hauser, E.; Weber, U., Flelschwirtschaft 1980, 6 0 , 482; Anal. Abstr.
(63L) Turner, N. A., J . Scl. Food Agrlc. 1980, 37, 171. 1981, 41,2F27.
(64L) Uppstrom, 6.; Svensson, R., J . Scl. Food Agrlc. 1980, 37,651. (48M) Hernandez, A. G.; Sanchez-Medina, F., J . Sci. Food Agric., 1981,
(65L) Ushijima, S.; Hamada, T.; Kanbe, C., Nlppon Shoyu Kenkyusho Zasshl 32, 1123.
1982, 8 , 58; Chem. Abstr. 1982, 97,22202~. (49M) Hiadik, J.; Curda, L.; Pokluda. Z., Prum. Potravin 1982, 33,101; Anal.
(66L) Vaidehita, M. T.; Carballido, A.; Melgar, M. J., An. Bromatol. 1980, Abstr. 1982, 43,3F50.
32,381; Chem. Abstr. 1982, 96,3346313. (50M) Hobson-Frohock, A., J . Food Technol. 1979, 74, 441.
(67L) Verzele, M.; Dewaeie, C., J . A m . SOC.Brew. Chem. 1981, 39,67; (51M) Holloway, C. J.; Pingoud, V., flectrophoresis, 1981, 2 ,3.
Anal. Abstr. 1982, 43, 2F41. (52M) Holz, F., Z . Tlerphysiol., Tierernaehr. Futtermittelkd., 1981, 46,72;
(68L) Vora, P. S..J . Assoc. Off. Anal. Chem. 1982, 65, 572. Chem. Abstr. 1981, 95,131045~.

194R ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983


FOCIDS

(53M) Ibld. Z . , Pflanzenzuechf. 1982, 88 103; Chem. Absfr. 1982, 96, (111M) Steinhart, H., Landwlrtsch. Forsch., Sonderh. 1979, 36, 301;
197970~. Chem. Abstr. 1981, 9 4 , 28951a.
(54M) Ibld., Landwlrtsch. forsch. 1980, 33,272; Anal. Abstr. 1982, 42, (112M) Suhren, G.; Heeschen, W.; Tolle, A., Mllchwlssenschaff 1982, 37,
102. 143.
(55M) Hruachka, W. R.; Norrls, K. H., Appl. Spectrosc. 1982, 36, 261; (113M) Tanaka, H.; Imahara, H. Esaki, N.; Soda, K., Agr. Blol. Chem. 1081,
Chem. Absfr. 1982, 97,4 7 5 2 ~ . 45, 1021.
(56M) Hu, Y.; Tong, X., Fenxl Huaxue 1981, 9 ,436; Chem. Abstr. 1982, (114M) Ibld., Anal. Lel't., Part 6 1981, 14, 111; Anal. Absfr. 1981, 4 1 ,
96, 1209924. 3D206.
(57M) Hughes, G. J.; Winterhalter, K. H.; Boller, E.; Wilson, K. J., J. Chro- (115M) Tkachuk, R., Cereal Foods World 1981, 26, 584.
matogr. 1982, 235,417. (116M) Ugrlnovits, M., Mlff. Geb. Lebensmlffelunfers,Hyg. 1980, 71,'124;
(58M) Hunziker, H. R.; Misorez, A., Mlff. Geb. Lebensmlffelunters Hyg. Anal. Abstr. 1980, 33,3F7.
1981, 72,216; Anal. Ab&. 1982, 42, 1F14. (117M) Unger, S.E.; Vincze, A.; Cooks, R. G.; Chrisman, R.; Rothman, L. D.,
(59M) Hurrell, R. F.; Lerman, P.; Carpenter, K. J., J. Food Scl. 1979, 44, Anal. Chem. 1981, 53,976.
1221. (118M) Vaile-Vega, P.; Young, C. T.; Swalsgood, H. E., J. Food Scl. 1080,
@OM) Hurst, W. J.; Toomey, P. B., Analysf (London) 1981, 106, 394. 45, 1003.
(61M) Inouye, K.; Matsumoto, M., Toyo Soda Kenkyu Hokoku 1981, 25, 13; (119M) Ibld., 1980, 45, 1026.
Anal. Abstr. 1982, 42,6D186. (120M) Van Ginkel, J. H.; Sinnaeve, J. Analyst (London) 1980, 105, 1'199.
(62M) Ishida, N.; Tajima, M.; Kenmochi, K.; Matsuura, S.,Shokuhln Sogo (121M) Vdovenko, M. E.; Maklakova, A. V.; Marchevskaya, Y. M.; Osadlchii,
Kenkyusho Kenkyu Hokoku 1979, 90;Chem. Abstr. 1981, 94,8 2 2 8 2 ~ . V. D., Tezlsy Dokl. . Resp. Konf. Anal. Khlm, 1st 1979, 98; Chtsm.
(63M) Ishlda, Y.; Fujlta, T.; Asai, K., J . Chromafogr. 1981, 204, 143. Absfr. 1980, 93,202782n.
(64M) Jones, D.; Shoriey, D.; Hitchcock, C., J. Scl. Food Agrlc. 1982, 33, (122M) Vialle, J.; Kolosky, M.; Rocca, J. L., J. Chromatogr. 1981, 204,4129.
677. (123M) VoJlr, F.; Petueiy, F., Lebensmlftelchem. Gerlchtl. Chem. 1982, 36,
(65M) Juergens, U.; Von Grundherr, K.; Elosczyk, G., Lebensmlffelchem. 73; Chem. Absfr. 1982, 9 7 , 125799b.
Gerlchfl. Chem., 1980, 34, 109; Anal. Abstr. 1981, 4 1 , 5F20. (124M) Volk, K.; Gemmer, H., Flelschwlrtscbaff 1982, 62, 588; Chism.
(66M) Kaltwasser, E.; Thalacker, R., Flelschwlrtschaft 1980, 6 0 , 1678; Absfr. 1982, 97,222189.
Chem. Absfr. 1980, 93,237039~. (125M) Von Lengerken, (2.; Von Lengerken, J.; Eggers, G., Flelsch 1979, 33,
(67M) Khayat, A.; Redenz, P. K.; Gorman, L. A., Food Technol. (Chicago) 76; Anal. Abstr. 1980, 39,5F38.
1982, 36,46. (126M) Warthesen, J. #J.; Waletzko, P. T.; Busta, F. F., J. Agrlc. Food
(68M) Kim, D., Chungang Uihak 1979, 37, 37; Chem. Abstr. 1981, 95, Chem. 1980, 28, 1308.
1310422. (127M) Wllllams, P. C.; Cordelro, H. M., Cereal Foods World, 1981, '124.
(69M) King. R. R., J. Assoc. Off. Anal. Chem. 1980, 63,1226. (128M) Williams, P. C.; McEachern, L. W., Lab. Pracf. 1981, 30, 125;
(70M) Kozukue, N.; Kozukue, E., J. FoodScl. 1982, 47, 1584. Chem. Abstr. 1981, $ 4 , 137891b.
(71M) Kostyukovskil, Y. L.; Metlamed, D. B., Zh. Anal. Khlm. 1981, 36, 134; (129M) Wood-Rethwlll, J. C.; Warthesen, J. J., J . Food Scl. 1980, 45,1637;
Anal. Absfr. 1981, 4 1 , 3F3. Chem. Abstr. 1980, i93.
(72M) Krishchenko, V. P.; Bolling, H., Agrokhlmiya 1982, 124;Chem. Absfr. (130M) Wright, R. G.; Miiward, R. C.; Coles, E. A., Food Technol. (Chicago)
1982, 97, 125770k. 1980.34. 47.
(73M) Kruggel, W. (3.; Field, R . A,; Riley, M. L.; Radloff, H. D.; Horton, K. M., (131Mj~Ya&moto, S.; Wakabayashi, S.; Makita, M., J. Agrlc. Food. Chom.
J. Assoc. Off. Anal. Chern. 1981, 64, 692. 1980. 28. 790.
(74M) Kusuwl, S.; Shlmizu, M.; Nlshimura, S.;Murakoshi, A.; Takegawa, M.; (132M) Yamamoto, S.;Itano, H.; Kataoka, H.; Makita, M. Ibld. 1982, 30,
Tanaka, J., Shokuhin Elseigaku Zasshl 1980, 21, 373; Chem. Abstr. 435.
1981, 94,822652. (133M) Yang, C., Hoppe-Seyler's 2. Physlol. Chem. 1980, 367, 1599;
(75M) Lauriere, M.; Mosse, J., Anal. Blochem. 1982, 122,20. Anal. Absfr. 1981, 4 7 , 613206.
(76M) Lehmann, G.; Haug, I.; Schioesser, R., Z . Lebensm-Unfers. Forsch. (134M) Zee, J. A.; Simard, R. E.; Roy, A., Can. Inst. Food S o . Technol. J .
1981, 172987. 1981, 14, 71.
(77M) Lin, J.; Lai, C., Anal. Chem. 1980, 52,630.
(78M) Lin, S.; Smlth, L. A.; Caprloll, R. M., J . Chromafogr. 1980, 197,31. VITAMINS
(79M) Liuzzo, J. A.; Wong, C. M.; Coll, M., J. Agric. FoodChem. 1982, 30, (1N) Asano, T.; Hasegawa, T.; Suzukl, K.; Masushige, S.;Nose, T.; Suzuki,
340 T. Nutr. Rep. I n t . 1981, 24, 451; Chem. Abstr. 1981, 95, 218929t.
(8OM)-'Lucas, B.; Sotelo, A., Anal. Biochem. 1982, 123,349. (2N) Atwal, A. S.; Eskln, N. A. M.; Vaisey-Genser, M. Cereal Chem. W80,
(81M) Ibld., 1980, 109, 192. 57,368.
(82M) Luten, J. B., J. Food. Scl. 1981, 4 6 , 958. (3N) Augustin, J.; Beck, C.; Marousek, G. I.J. Food Scl. 1981, 4 6 , 312.
(83M) Mackey, L. N.; Beck, 7'.A,, J. Chromafogr. 1982, 240,455. (4N) Beutler, H. 0.; Beinstlngl, G. Dtsch. Lebensm-Rundsch 1982, 78,9.
(84M) Maga, J. A., J. Food. Scl. 1981, 4 6 , 132. (5N) Bognar, A. Dtsch. Lebensm-Rundsch 1981, 77,431.
(85M) McGIII, D. L., J . Assoc. Off. Anal. Chem. 1981, 6 4 , 29. (6N) Branca, P. Boll. Chlm. Unlone Ital. Lab. Prov. Parte Scl. 1980, 6 ,
(88M) Morr, C. V., !J. Food Sci. 1982, 47, 1751; Chem. Absfr. 1982, 87, 143; Anal. Abstr. 1981, 4 1 , 5F12.
17. (7N) Capuano, A.; Daghotte, A. Rlv. Ital. Sostanze Grasse 1980, 57,285;
(87M) Mrowetz, G.; Thomasow, J., Mllchwlssenchaff 1980, 35,675. Anal. Abstr. 1981, 40, 2F72.
(88M) Munroe, J. H.; Swltala, I<.J.; Cutala, A. J., J. A m . SOC.Brew. Chem. (EN) Carnevale, J. Food Technol. A M . 1980, 32,302; Anal. Abstr. 1981,
1979, 37, 164; Anal. Absfr. 1981, 4 0 , 2F60. 4 7, 4F62.
(89M) Nakamura, H.; Tamura, Z.,Anal. Chem. 1981, 53,2190. (9N) Coors, U.; Montag, A. Chem. Mlkroblol., Technol. Lebensm 1981, 7 ,
(90M) Nkonge, C.; Ballance, Q. M., J . Agrlc. Food Chem. 1982, 30,4'16. 21; Chem. Abstr. 1981, 95,409402.
(91M) O'Donnell, D. J.; Ackerman, J. J. H.; Maclel, G. E., J. Agrlc. Food (10N) Cortesi, N.; Fedeli, E. Rlv. Ital. Sostanze Grasse, 1980, 57, 16; Anal.
Chem. 1981, 29,514. Abstr. 1980, 39,3F68.
(92M) Paiiler, F. M., Ann. Falslf. Expert. Chlm. 1979, 72,335; Anal. Absfr. (11N) Coustard, J. M.; Sudraud, G. J. Chromatogr. 1981, 219,338.
1980, 39,6F26. (12N) Day, B. P.; Gregory, J. F., I11 J. Agrlc. Food Chem. 1981, 29,374.
(93M) Pechanek, U.; Blalcher, G.; Pfannhauser, W.; Woidlch, H.,2. Le- (13N) Deldime, P.; Lefebvre, G.; Sadin, Y.; Wybauw, M. Ref. Fr. Corps Gkas
bensm-Unfers. Forsch. 1980, 177,420. 1980, 27,279; Anal. Abstr. 1981, 4 1 , 4F83.
(94M) Pfeilsticker, K.; Leyendecker, A., Z . Lebensm-Unters. Forsch . 1980, (14N) Dennlson, D. E.; Brawley, T. G.; Hunter, G. L. K. J . Agrlc. b o d
171. 174. Chem. 1981, 29, 927.
(95M) Rattenbury, J. M., "Amlno Acid Analysis"; Ellis Horwood Ltd.: London, (15N) Doner, L. W.; Hicks, K. B. Anal. Blochem. 1981, 115,225.
Dist. bv Wllev. 1981.
(16N) Ellefson, W. C.; Richter, E.; Adams, M.; Baillies, N. T. J. Assoc. Off.
(96M) Raymond, M. L.; Dunmlre, D. L., J. Chromatog. Scl. 1981, 19, 144. Anal. Chem. 1981, 64, 1336.
(97M) Reid, S.J.; Good, T. J., J . Agrlc. Food Chem. 1982, 30, 775. (17N) Ersoy, L.; Duden, 13. Lebensm. Wiss. Technol. 1980, 73,201.
(98M) Rubach, K.; Offlzorz, IP.; Breyer, C., Z . Lebensm-Unfers. Forsch. (18N) Finiey, J. W.; Duang, E. J. Chromatogr. 1981, 207,449.
1981, 172,351.
(19N) Florldi, A.; Coli, R.; Fldanza, A. A.; Bourgeois, C. F.; Wlggins, R. A.
(99M) Rutar, V.; Bllnc, R.; Ehrenberg, L., J. Magn. Reson. 1980, 4 0 , 225; Int. J . Vitam. Nutr. Res. 1982, 52, 193; Chem. Abstr. 1982, -97,
Anal. Abstr. 1981, 4 1 , 4F29. 108598t.
(100M) Rutschmann, M.; Kuehn, L.; Dahlmann, B., Relnauer, H., Anal. Bio- (20N) Geigert, J.; Hlrano, D. S.;Neidleman, S.L. J. Chromatogr. 1981, 206,
chem. 1982, 124, 134. 396.
(101M) Samotus, B.; LeJa, M.; Sclgalskl, A.; Dullnski, J.; Siwanowicz, R., J. (21N) Gerhardt, U.; Wlndmueller, R . Fleischwirtschaft 1981, 61, 1389; Anal.
Scl. FoodAgrlc. 1982, 33,617. Abstr. 1982, 43,4F47.
(102M) Santos-Buelga, C.; Nogales-Alarcon, A.; Marine-Font, A.. J. Food. (22N) Gertz, C.; Herrmainn, K. Z . Lebensm-Unters. Forsch. 1982, 174,
Scl. 1981, 46, 1'794. 390.
(103M) Satyanarayana, B. L.; Guruprasad, A. S.; Dinanath V., J. Sci. Food (23N) Gregory, J. F., 111; Manley, D. B.; Kirk, J. R. J. Agrlc. Food Chsm.
Aorlc. 1981. 32. 717. 1981, 29, 921.
(104h) Schlllak, R., Chem. Anal. (Warsaw) 1980, 25, 181; Anal. Abstr. (24N) Hassan, S. S. M. J . Assoc. Off. Anal. Chem. 1981, 6 4 , 611.
1981, 40, 2F19.
(25N) Hoppner, K.; Lampi, B. J. Li9. Chromatogr. 1982, 5, 953.
(105M) Scudamore. K. A., Analyst (London) 1980, 705,1171. (26N) Hughes, D. E. J. Pharm. Scl. 1982, 71,834.
(106M) Skogberg, D. J., Dlss. Absfr. Inf. 6 .1981, 4 7 , 3375. (27N) International Unloin of Pure and ADDlled Chem.. Pure ADD/.
(107M) Sontag, G.; Kral, K., Mikrochlm Acta 1980, 2 , 39; Chem. Absfr. 1982, 54, 233.
.. . . Chem.
1981, 94,45679k. (28N) Kamel, B. S.;Bueno, M. Lebensm-Wiss. Technol. 1980, 13, 134.
(108M) Sporns, P.. J . Assoc. Off. Anal. Chem. 1982, 65, 567. (29N) Kamman, J. F.; Labuza, T. P.; Warthesen, J. J. J . Food Scl. 1980,
(109M) Stamm, H.; Gertz, C., Lebensmlffelchem. Gerlchtl, Chem. 1980, 34, 45. 1497.
70; Anal. Abstr. 1981, 4 7 , 3F18. (30N) .Keating, R. W.; Haddad, P. R. J. Chromafogr. 1982, 245, 249.
(llOM) Staruszkiewicz, W. F., Jr.; Bond, J. F., J. Assoc. Off. Anal. Chem. (31N) Kelly, G. J.; Latzko, E. J. Agric. Food Chem. 1980, 28, 1320.
1981, 64, 584. (32N) Kennedy, C. A.; MlcCleary, B. V. Analyst (London) 1981, 106, 3.44.

ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983 195 R


Anal. Chen?. 1983,55, 196R-202R

(33N) Kitayama, Y.; Inoue, M.; Tamase, K.; Imou, M.; Hasulke, A,; Sasakl, (75N) Vanderslice, J. T.; Maire, C. E., J. Chromafogr. 1980, 196, 176.
M.; Tanlgawa, K. Hyo to Shokuryo 1982, 35, 121; Chem. Absfr. 1982, (76N) Vandersllce, J. T.; Brown, J. F.; Beecher, G. R.; Maire, C. E.; Brown-
9 7 , 143228~. lee, s. G., J . Chromafogr. 1981, 2 1 6 , 338.
(34N) Koborl. S.; Kawakami, S. Ufsunorniya Daigaku Kyoikugakubu Kiyo, (77N) Van Nleklrk, P. J.; Smit, S. C. C., J. Am. 011Chem. SOC. 1980, 5 7 ,
Dal-2 bu 1980, 30, 67; Chem. Absfr. 1981, 9 5 , 167204t. 417.
(35N) Kurzawa, J.; Wojclechowski, J. Fleischwirfschaft 1980, 60, 1896; (78N) Verma, K. K.. Talanfa, 1982, 2 9 , 41.
Anal. Absfr. 1982, 4 2 , 1F28. (79N) Vlncenzlnl Foppa, G. F., Riv. Ifal. Sosfanze Grasse 1981, 58, 296;
(36N) Landen, W. O., Jr. J. Chromafogr. 1981, 211. 155. Anal. Abstr. 1982, 4 2 , 1F80.
(37N) Ibid., J . Assoc. Off. Anal. Chem. 1982, 65,610. (EON) Watada, A. E., HortSclence 1982, 17, 334; Chem. Absfr. 1982, 9 7 ,
(38N) Lechlen, A.; Valenta, P.; Nuernberg, H. W.; Patriarche, G. J. Fresenl-
us’ 2.Anal. Chem. 1982, 3 7 1 , 105; Anal. Absfr. 1982, 4 3 , 4E51.
90 509c .
(81N) Wiggins, R. A.; Zal, E. S.; Lumley, I., Chromafogr. Scl. 1982, 2 0 ,
(39N) Leklem, J. E.; Reynolds, R. D. “Methods in Vitamin 6-6 Nutrition”; 327.
Plenum Press: New York, 1981. (82N) Woollard, D. C.; Wooiiard, G. A., N.Z. J. Dairy Sci. Technol. 1981,
(40N) Llm, K. L. Diss. Absfr. Inf. 8 1982, 4 2 , 4021. 16, 99.
(41N) Loeiiger, J.; Saucy, F. 2.Lebensm-Unters. Forsch. 1980, 170, 413. (83N) Yurchenko, N. I.; Bogusiavskaya, L. V.; Gol’denberg, V. I., Kinef.
(42N) Lookhart, G. L.; Hail, S. B.; Finney, K. F. CerealChem. 1982, 5 9 , 69. Katal. 1979, 2 0 , 1434; Anal. Absfr. 1981, 4 0 , 3F91.
(43N) Lumley, I.D.; Wlgglns, R. A. Anaiysf (London) 1981, 106, 1103. (84N) Zonta. F.; Stancher, B.; Blelawny, J., J. Chromafogr. 1982, 2 4 6 , 105.
(44N) Lyle, S. J.; Tehranl, M. S. J. Chromatogr. 1982, 2 3 6 , 31.
(45N) Macholan, L.; Londyn, P.; Flscher, J. Collect. Czech. Chem. Com- Y I SCELLANEOUS
mun. 1981, 4 6 , 2871; Anal. Absfr. 1982. 42. 6D9. (1P) Ailvin, B., Kem. Tidskr. 1980, 9 2 , 24; Anal. Absfr. 1981, 4 1 , 1F1.
(46N) Manz, U.; Phlllpp, K. Inf. J . Vitam. Nuh. Res. 1981, 5 1 , 342; Anal. (2P) Aivarez, R., J . Assoc. Off. Anal. Chem. 1980, 6 3 , 806.
Absfr. 1982, 4 3 , 4619. (3P) Arneth, W., Fleischwirfschaft 1982, 6 2 , 974; Chem. Absfr. 1982, 9 7 ,
(47N) Marzo, S. Riv. Ifal. Sosfanze Grasse 1981, 5 8 , 115; Anal. Absfr. 143227t.
1981, 4 1 , 4F84. (4P) Baites, W.; Czedik-Eysenberg, P. B.; Pfannhauser, W., “Recent Devel-
(48N) Matsumoto, K.; Yamada, K.; Osajlma, Y. Anal. Chem. 1981, 53, opments In Food Analysis: Proceedings of the First European Conference
1974. in Food Chemistry (EURO FOOD CHEM I)”; Verlag Chemie, 1982.
(49N) Mouillet, L.; Luquet, F. M.; Gagnepaln, M. F. Sorgue, Y. LaR 1982, 6 2 , (5P) Bjarnoe, 0. C., J. Assoc. Off. Anal. Chem. 1981, 6 4 , 1392.
44; Chem. Abstr. 1982, 9 6 , 1795300. (6P) Ibld. 1982, 65, 696.
(50N) Munlz. J. F.; Wehr, C. T.; Wehr, H. M. J. Assoc. Off. Anal. Chem. (7P) Egan, H.; Kirk, R. S.; Sawyer, R., “Pearson’s Chemical Analysis of
1982, 65, 791. Foods”; Churchill Livingstone: Edinburgh, U. K., 1981.
(51N) Nasner, A.; Kraus, L. Fette, Seifen, Anstrichm. 1981, 8 3 , 70. (8P) Ettre, L. S., Chromafogr. Newsl. 1981, 9 , 46.
(52N) Obata, H.; Tsuchlhashl, W.; Tokuyama, T. Agric. 8iol. Chem. 1980, (9P) Frank, J. F.; Birth, G. S., J. Dairy Sci. 1982, 85, 1110.
4 4 , 1435. (1OP) Hardin, J. M.; Stutte, C. A., J . Chromafogr. 1981, 2 0 8 , 124.
(53N) Okano, T.; Takeuchi, A,; Kobayashl, T. J. Notr. Sci. Vlfaminol. 1981, (11P) Iwamoto, M.; Norris, K. H.; Kimura, S., Nippon Shokuhin Kogyo Gak-
2 7 , 539; Chem. Absfr. 1982, 9 6 , 102584t. kalshl1981, 2 8 , 85; Chem. Absh. 1881, 9 4 , 155103a.
(54N) Parolarl, 0. Ind. Conserve 1982, 5 7 , 19; Chem. Absfr. 1982, 9 7 , (12P) Kaffka, K., Prum. Pofravln 1981, 3 2 , 634; Anal. Absfr. 1982, 4 3 ,
70903~. 5F7.
(55N) Parrlsh, D. B. CRC Crlf. Rev. Food Sci. Nufr. 1979, 12, 29. (13P) Kaffka, K. J.; Norris, K. H.; Kulcsar, F.; Draskovits, I., Acta Aliment.
(56N) Ibid. 1980, 13, 337. 1982, 1 1 , 271.
(57N) Press, K.; Sheeley, R. M.; Hurst, W. J.; Martin, R. A. J . Agric. Food (14P) Kaffka, K. J.; Norrls, K. H.; Peredl, J.; Balogh, A,, ibid. 253.
Cham. i-9- a- -,
i . -29.
- 1096. (15P) Kaffka, J. K.; Norris, K. H.; Rosza-Kiss, M., IbM. 199.
(58N)-Rhee. J. S.; ShiniM. G. JAOCS J . Am. Oil. Chem. S O ~1982, . 59, (16P) Kas, J.; Fukal, L.; Rauch, P. Chem. Lisfy, 1981, 7 5 , 963; Anal. Absfr.
98. 1982, 4 3 , 5F1.
(59N) Reingoid, R. N.; Plcciano, M. F. J. Chromatogr. 1982, 2 3 4 , 171. (17P) King, R. D., “Developments in Food Analysls Techniques-2”; Applied
(60N) Rose, R. C.; Nahrwold, D. L. Anal. 8iochem. 1981, 114, 140. Science: London, 1980.
(61N) Roy, R. B. Top. Autom. Chem. Anal. 1979, 1 , 138. (18P) Kobayashi, T.; Saga, K.; Shimlzu, S.; Goto, T., Agrlc. 8/01. Chem.
(62N) Rubach, K.; Breyer, C. Dtsch. Lebensm-Rundsch. 1980, 7 6 , 228. 1881, 4 5 , 1403; Anal. Absfr. 1982, 4 2 , 2D11.
(63N) Rueckemann, H. 2.Lebensmdnters. Forsch. 1980, 177, 357. (19P) Kohashl, M.; Tomita, K.; Iwai, K., ibid. 1980, 4 4 , 2089; Anal. Absfr.
(64N) Rugraff, L.; Demanze, C.; Karlesklnd, A. Ind. Allment. Agric. 1981, 1981, 4 0 , 4F6.
9 8 , 305; Anal. Absfr. 1982, 4 3 , 3F77. (20P) Murphy, P. A. J . Chromafogr. 1881, 217, 166.
(65N) Shaw, P. E.; Wllson, C. S., 111 J. Agric. FoodChem. 1982, 30, 394. (21P) Noble, R. C.; Shand, J. H.; West, I.G., J. Dairy Sci. 1981, 6 4 , 14.
(66N) Skurray, G. R. FoodChem. 1981, 7 , 77. (22P) Osborne, B. G.; Douglas, S.; Fearn. T., J . Food Technol. 1982, 17,
(67N) Soiiman, A. J. Assoc. Off. Anal. Chem. 1981, 64, 616. 355.
(68N) Stancher, B.; Zonta, F. J . Chromafogr. 1982, 236,217. (23P) Shenk, J. S.; Landa, I.; Hoover, M. R.; Westerhaus, M. O., Crop Sci.
(69N) Tanabe, K.; Yamaoka, M.; Kato, A. Yukagaku 1981, 30, 116; Chem. 1981, 2 1 , 355; Anal. Absfr. 1982, 4 3 , 1G18.
Absfr. 1981, 9 4 , 155064~. (24P) Sloman, K. G.; Foitz, A. K.; Yeranslan, J. A., Anal. Chem. 1981, 53,
(70N) Taylor, P.; Barnes, P. Chem. Ind. (London) 1981, 722. 242R.
(71N) Tesmer, E.; Leinert, J.; Hoetzel, D. Nahrung 1980, 2 4 , 697; Chem. (25P) Stewart, K. K. “Nutrient Analysls of Foods: The State of the Art for
Absfr. 1980, 9 3 , 237032~. Routine Analysls”; Assoc. Off. Anal. Chem.: Arllngton, VA, 1980.
(72N) Thompson, J. N.; Hatina, G.; Maxwell, W. B.; Duval, S., J . Assoc. Off. (26P) Tessler, A.; Delaveau, P.; Hoffelt, J., 2. Lebensm-Unters. Forsch.
Anal. Chem. 1982, 65, 624. 1982, 174, 132; Anal. Ab&. 1982, 4 3 , 3F26.
(73N) Tono, T.; Fujlta, S., Agric. Biol. Chem. 1981, 4 5 , 2947. (27P) Watson, C. A,, Anal. Proc. (London) 1982, 19, 12.
(74N) Vaidya, S. K.; Damodaran, C., Farmaco, .Ed. Praf. 1882, 3 7 , 9; Anal. (26P) Winkler. F. J.; Schlmldt, H., 2.Lebensm-Unfers Forsch. 1980, 171,
Absfr. 1982, 4 3 , 3E43. 85.

Geological and Inorganic Materials

Carleton B. Moore” and Julle A. Canepa

Department of Chemistry, Arizona State University, Tempe, Arlzona 85287

This review discusses publications describing methods for analysis in the application reviews and many of the funda-
analysis of geological and inorganic materials during the period mental reviews especially emission spectrometry, ion exchange
November 1980 through November 1982. The topical chromatography, and ion selective electrodes. The citations
boundaries of the inorganic and geological materials are of this review may well, by necessity, include some of those
somewhat diffuse since closely related topics are reviewed in listed in other reviews, but for the most part they have been
both the fundamental and application reviews. These related selected from the many thousands available to give the reader
reviews include air pollution, fertilizers, ferrous metallurgy, an overview of recent advances in each analytical technique
nonferrous metallurgy, surface characterization, and water reviewed together with mentions of particularly interesting
196 R 0003-2700/83/0355-196R$01.50/0 0 1983 American Chemical Society

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