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SHERMA: JOURNAL OF AOAC INTERNATIONAL VOL. 84, NO.

5, 2001 1303

SPECIAL REPORT

Pesticide Residue Analysis (19992000): A Review


JOSEPH SHERMA Lafayette College, Department of Chemistry, Easton, PA 18042

The literature of pesticide residue analysis is reviewed selectively for the period 19992000. Analyses of a wide range of pesticide classes and sample types, as well as some related organic pollutants, are covered. Studies of exposure and monitoring as well as pesticide degradation, persistance, leaching, mobility, and metabolism studies are included.

he purpose of this selective review is to describe the present status of the field of pesticide residue analysis and advances in methodology and applications reported in the past 2 years. Coverage is provided for a broad variety of pesticides and samples, and more limited information is given on the analysis of several classes of organic pollutants related to pesticides. References are provided to review articles, journal papers, and abstracts of presentations at meetings as examples for the topics covered. The major sources of information were the primary analytical and chromatography journals, which were searched directly, and computer-based searches of Chemical Abstracts, Analytical Abstracts, and The Web of Science. This review updates the one published last year in this journal covering the years 19971998 (1). Current trends in the field of analytical chemistry during the past 2 years have included the lowering of detection limits of analytes for trace analysis, increasing automation to reduce analytical costs and improve precision, reduction of sample sizes, and use of coupled systems allowing cleanup, separation, detection, and confirmation. Trace analyses are being developed for more complex and dirty samples in which sample preparation is a key element, and fast gas chromatography (GC) and various combinations of GC and liquid chromatography (LC) with mass spectrometry (MS) are becoming more important. The mass spectrometer can be a universal detector for GC, and GC/MS is a legally accepted confirmation technique. In the scan mode, the detection capabilities of a mass spectrometer approximates the rather nonselective flame ionization detector (FID), while the selected ion monitoring (SIM) mode (also termed mass selective detection [MSD]) or MS/MS affords increased selectivity. The time of flight (TOF) mass spectrometer, which is the fastest detector, has sensitivity and resolution similar to the quadrupole; it is used more in LC (e.g., matrix-assisted laser desorption ionization

Received February 27, 2001. Accepted by RR February 27, 2001.

[MALDI]TOF for high molecular weight analytes) but is gaining popularity in GC. Fast GC uses shorter columns with smaller diameter packings and thinner stationary phase films, smaller sample volumes, and faster temperature programming for achieving separations and cleanup of the column. SIMMS is often used with fast GC because the ability to scan characteristic ions can make up for reduced resolution on the column. LC/MS is growing in applications, but coupling remains more difficult and buffer ions and mobile phase solvents cause worse backgrounds compared with GC/MS. Automated systems often include solid-phase extraction (SPE) and occasionally solid-phase microextraction (SPME) for sample cleanup. SPME, which makes use of a polymeric phase, such as poly(dimethylsiloxane), bonded or coated onto a fused-silica fiber (2), is being applied increasingly for sampling liquids and headspace vapors, including derivatization on the fiber, and advances in stirbar sorptive extraction (SBSE) are being reported. Programmed temperature GC inlets with large volume injection are being used more widely to increase sensitivity and eliminate concentration steps. Research on new sample preparation and injection techniques are promising for analysis of more labile and polar compounds by GC rather than LC. Many of these general analytical trends, and others, have been noted in the new pesticide analytical methods published in the last 2 years. Advances were reported in residue analysis by GC/MS with full ion scanning and SIM; GC/MSMS; GC with an on-column capillary inlet; GC with a temperature programmable preseparation column; GC with atomic emission and MS detectors (GCAED/MS; 3); thermal desorptionGC/MS (4); large volume injection (LVI)GC, GC/MS, and GC/MSMS (5); LVIGC with a flame photometric detector (FPD); fast GC; microcolumn (capillary) LC (6); coupled column LC (LCLC); LC with photodiode array (PDA) ultraviolet detection (LCPDAUV); LC/atmospheric pressure chemical ionization MS (APCIMS; 7); LC/ion trap (IT)MS and LC/ITMS/MS (8); micro LC/electrostatic ionization (ESI)/MSMS; LCPDAUV/MSMS (9); SPELCPDAUV/APCIMS (10); SBSE; microwave assisted extraction (MAE) with (11) and without (12) in situ derivatization; accelerated solvent extraction (ASE) combined with GC and LC as replacements for traditional blender and Soxhlet extractions (13, 14); in-tube SPME/LC (6); capillary electrophoresis (CE; 15); CE/MS (16, 17); chiral analysis of pesticides (18); immunoassay; and isotachophoresis. These and other pesticide analytical methods are covered in the references given below in the pertinent sections of this review.

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Sample Collection and Preparation The use of semipermeable membrane devices for sampling trace and ultratrace amounts of organic contaminants, including organochlorine (OC) pesticides, polychlorinated biphenyls (PCBs), polycyclic aromatic hydrocarbons (PAHs), polychlorinated dioxins, and dibenzofurans, in water, sediment, soil, and air was reviewed (19). The pesticide multiresidue methods used most often for surveillance and compliance monitoring of foods, risk assessment studies, and other surveys and routine analyses are based on the Luke et al. and U.S. FDA Pesticide Analytical Manual (PAM) methods using acetone extraction, methylene chloride partitioning, and dual-column GC or LC or other multiresidue methods involving GC/MS after liquidliquid extraction (LLE) and concentration without a cleanup step (see the section on pesticide monitoring below). Improvements in this methodology were reported (20) that involved modifying and adopting a published acetonitrile extraction method in order to eliminate methylene chloride hazardous waste and use of gravitySPE to simplify sample preparation and provide cleaner samples, new selective detectors, retention time locking (21), and GC/MS. Gel permeation chromatography (GPC) remains widely used for cleanup in pesticide residue analyses, e.g., after acetone extraction and ethyl acetate partitioning in the GC/ITMS determination of 19 fungicides in processed fruits and vegetables at 0.0050.05 mg/kg (22). Simazine, terbuthylazine, and their dealkylated chlorotriazine metabolites in soil were determined using sonication microextraction, GC with a nitrogenphosphorus (thermionic) detector (GCNPD), and GC/MSSIM (23). A semiautomatic module for the direct leaching and determination of 16 phenols (pesticide degradation products) in agricultural soils at concentrations of 505000 ng/g was described; soil extractions were done with alkaline aqueous solutions and solid-sorbent preconcentration in an acid medium, using XAD2 as sorbent (24). SPE has become very widely used in pesticide residue analytical methods for isolation, cleanup, and preconcentration of analytes (25). In addition to the most commonly used octadecyl-bonded silica (C18), different SPE sorbents in column and cartridge form are being applied more often, including strong and weak anion exchangers (26), Florisil (26), graphitized carbon black (e.g., ENVI-Carb), and polymeric materials (e.g., LiChrolut EN and Isolute ENV+; 27). It was shown that acidic and nonacidic herbicides could be recovered more efficiently from soils by extraction with hot water and collection on a Carbograph 4 SPE column on-line than by using Soxhlet and sonication extraction techniques (28). Graphitized carbon black cartridges (Carbopack B) were shown to be efficient and not cause compound decomposition when used for extraction of organophosphorus (OP) pesticides from large volumes of water (29). Double-disk SPE, using layered strong anion exchange (SAX) and C18 disks, was effective for the simultaneous cleanup and trace enrichment of herbicides and metabolites from water and soil extracts (30). Ion-pair SPE using a C8 cartridge conditioned with sodium hexanesulfonate

was used to extract diquat and paraquat from drinking water prior to reversed phase (RP)LCPDAUV (31). Restricted access media (RAM) columns have proven valuable for removal of humic acid interferences in the trace analysis of acidic samples in water samples at 0.51 g/L by LCLCUV. The RAM materials tested were SPS (Regis), ISRP (Pinkerton, Regis), Hisep (Supelco), and ADS (Merck) (32). A new enrichment technique, dynamic ion exchange SPE (DIESPE), was shown to be effective for sample preparation for GC/MS analysis of 16 acidic herbicides in environmental waters that were weakly acidic to neutral. DIESPE is based on adsorption of a long carbon chain surfactant, such as cetyltrimethylammonium bromide (CTAB), on the surface of C18 bonded silica, where the ionic functional groups of the surfactant act as ion exchange sites to attract ionized analytes from water. DIESPE gave higher recoveries for the acidic herbicides and were less affected by sample matrixes compared with conventional RPSPE (33). Selective extraction of triazine herbicides from complex aqueous samples was obtained using on-line SPE with coupled columns containing a molecularly imprinted polymer (MIP) and C18 silica prior to RPLC analysis (34). The optimization of SPME of several OC and OP pesticides was presented and the influence of variables discussed; the optimized method was applied to determination of the pesticides in ethanolwater mixtures used as food simulants (35). SPME was used also for the determination of herbicides in soil extracts and water samples (36). Focused open vessel (FOV)MAE, closed vessel (CV)MAE, and ASE with ethyl acetatecyclohexane (1 + 1) were used for extraction of OC pesticides from fish tissues before direct GPC without solvent exchange and GC with electron capture detection (ECD); the relative standard deviation (RSD) of each technique was typically <10%, but ASE was most convenient (37). A method for 10 chloroacetanilide pesticides and pyriminobac-methyl in crops using supercritical fluid extraction (SFE) cleanup on a trap column consisting of Extralut and Florisil or Bond Elut SAX and PSA, and GC/MSSIM was developed and compared favorably with the Japanese Bulletin method, in which pesticides are prepared by traditional solvent extraction and partitioning and Florisil column cleanup and determined by GCNPD (38). Addition of an appropriate chemical sometimes aids in quantitative recovery of pesticides by SFE [assisted SFE (ASFE)]. As an example, Na4EDTAASFE with carbon dioxide was used to determine 29 polar aromatic acids, phenols, and neutral compounds, including pentachlorophenol (PCP) and other pesticides, in soil (39). On-line SFE and aminopropyl SPE was used to determine the residues of 23 GC-amenable multiclass pesticides in cereals (40). Other new sample preparation methods are described in many of the pesticide analyses cited in the sections below.

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Gas Chromatography and Gas Chromatography/Mass Spectrometry GC remains the most widely used method for pesticide residue analysis, e.g., the classic Luke et al. method and its modifications (41). Most current published papers make use of capillary columns, although some official and regulatory methods still specify the older packed columns. The nature of the column is usually not specified when referring to GC in this review. MS is increasingly replacing traditional detectors such as FID (42), ECD, FPD, and NPD in newly developed methods. As examples of recent research, the following new methods were reported for pesticide analysis by GC: fluvalinate residues at 100500 g/kg in beeswax by dissolving the samples in hexane, partitioning with acetonitrile on an Extrelut diatomaceous earth disposable column, chromatographic cleanup on a Florisil cartridge eluted with diethyl etherhexane (1 + 1), and GCECD (43); binary and ternary mixtures of pesticides in wetland waters by GC at levels of 0.0201.0 ng/mL after preconcentration on a C18 cartridge using partial least squares analysis with sufficient sensitivity to measure residues at the maximum allowable concentrations specified in the European Union drinking water directive (44); 26 pesticides in honey at 0.021.6 mg/kg by ENV+ SPE and GCFPD and NPD (45); carbofuran and its metabolites in sugarcane and soil by derivatization with 1-fluoro-2,4-dinitrobenzene and GCNPD (46); malathion, coumaphos, and fluvinate in honey by GCECD and NPD (47); fungicides (48) and OP insecticides (49) in grapes, must, and wine by on-line microextraction and GCECD and NPD without cleanup; and LVI-short-column capillary GC (CGC) with programmable temperature vaporization (PTV) injection for improved detection limits in the analysis of pesticides in foods (50). GC/MS was used as part of the following new pesticide analytical determinations: 2 oxypyrimidine metabolites of diazinon in urine at 0.501.0 ppb using sample preparation by classical liquidliquid partitioning, SPE with ENV+ and silica gel columns, and GC/MSSIM and LC/ESIMSMS (51); 22 multiclass pesticide residues in mixed fruit and vegetable acetonitrile extracts by direct sample injection (DSI)GC/MSMS without cleanup (52); more than 100 pesticides at low ppb levels in fruits, vegetables, and milk by GC/MSMS using temperature programmed cold injection (TPCI) and only 2 injections per sample to screen for all the pesticides (53); hydroxyl-containing endocrine disruptors including PCP in water after derivatization with N-methyl-N-(tert.-butyldimethyltrifluoroacetamide; 54); and 17 pesticides in wine by SPE followed by direct injection GCMSD (55). Liquid Chromatography and Liquid Chromatography/Mass Spectrometry The majority of pesticide residue determinations are still performed on an RPLC system with a UV (fixed- or variablewavelength or PDA) or fluorescence (Fl; 56) detector, but MS is being reported increasingly for detection. As examples, sulfentrazone was determined in soil (57) and benzoylurea insecticides in apples and pears (58) by C18LCUV and azamethiphos in salmon tissue by C18LCFl (59). Opti-

mized, rapid separation of pesticides was demonstrated by use of 2 serially coupled columns with chemically diverse stationary phases that are independently temperature controlled (60). The following new analytical methods are examples of those reported for pesticide residue analysis by LC: triasulfuron herbicide in soil by LCUV with LC/MS confirmation after methanolphosphate buffer (pH 7; 2 + 1) extraction and cleanup on a silica adsorption SPE tube (61); glyphosate in plants by precolumn derivatization with 9-fluoroenylmethyl chloroformate and LCLCFl (62); and dithiocarbamate fungicides in fruits and vegetables by surface extraction followed by direct injection RP ion pair LC with UV and electrochemical detection in series (63). The use of LC/MS was reported for the following new pesticide residue analyses: 4 benzimidazole pesticides (carbendazim, thiabendazole, benomyl, and thiophanate-methyl) in fruits and vegetables at g/L levels by C18 LC/ESIMS after ethyl acetate extraction without cleanup (results of a 1998 residue monitoring program were given; 64); chlormequat in pears using water extraction and LC/ITMS in the single MS mode or ESIMS/MS with a triple quadrupole instrument (65); triazines, phenylureas, and acetanilides in brook, river, and sewage plant effluent water using on-line trace enrichment with custom-made polyacrylate-coated capillaries combined with LC/MSMS (66); pirimicarb and its desmethyl and desmethylformamido metabolites in fruits and vegetables at 0.0050.05 mg/kg by LC/ESIMS and MS/MS (67); 6 imidazolinone herbicides in soil at 2 ppb using 0.5M NaOH extraction, C18 and tandem strong anion-/strong cation-exchange SPE, desalting with an RP-102 SPE cartridge, and LC/ESIMSSIM (68); 120 pesticides and metabolites at <115 ng/g in soils with high organic content by C18 and amino SPE and GC/ITMS (69); phenylurea herbicides in various types of water samples at 0.020.8 g/L by LCLCUV, LCLC/MS, and LVILCLC/MS (results of an interlaboratory study are presented; 70); and urea pesticides in fruits and vegetables using SFE and LC/MS (71). Mass Spectrometry, Combination, and Hyphenated Methods Papers on MS, methods using both GC and LC, and hyphenated methods not included in other sections of this review are covered in this section. Developments in environmental MS in 19981999, including applications to pesticides in a variety of sample matrixes, were reviewed (72). Precise and rapid automated toxaphene quantitation was described using GC/MS with electron capture negative ionization; the method was implemented by a small QBasic program that compares peak area ratios with the predicted chlorine isotopic ion ratios (73). The use of MS with negative chemical ionization (MSNCI) in combination with SIM allowed sensitive and selective determination of polar and thermally unstable herbicides in soils by LC coupled to a particle beam interface and matrix-standard calibration to avoid quantitative errors due to transfer of matter through the interface (74).

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Exact masses of ions determined by high resolution MS (HRMS) provide unique elemental compositions useful for identification of compounds in mixtures of environmental contaminants or synthetic products for regulatory analysis only for low mass ions (<150 Da). Methods were described (75) for mass peak profiling from selected ion recording data to acquire additional MS data and a profile generation model for automated interpretation of the data that provides elemental compositions of ions with m/z values up to 600 based on incontestable properties of atoms, their exact masses, isotopic abundances, and valences. Dioxins formed by thermal reaction of phenols could be sensitively and selectively identified by supersonic jet-multiphoton ionizationTOF MS (76). LC/accelerator MS (AMS) was used to measure 14C-labeled atrazine metabolites in human urine after dermal exposure. Limits of quantitation were a remarkably low 14 amol (77). A method was described for 251 pesticide and degradation product residues in fruits and vegetables using acetonitrile extraction, salting-out, SPE on a C18 cartridge followed by coupled carbon and aminopropyl cartridges, GC/MSSIM, and LCFl for N-methyl carbamates (78). Fungicide and OP residues at 0.110 g/g were determined in oranges by extraction with sodium acetate and ethyl acetate, cleanup on tandem anion exchange and primary/secondary amine bonded silica SPE columns, and GCFPD for chlorpyrifos, methidathion, and methyl parathion or LCFl for biphenyl, benomyl (as methyl-2-benzimidazole carbamate [MBC]), o-phenylphenol, and thiabendazole (79). Size-exclusion chromatography (SEC) was coupled to RPLC/MS for the determination of trace levels of thifensulfuron-methyl and tribenuron-methyl in buffersolution extracts of cottonseed and cotton gin trash; the extracts underwent solvent exchange into methanol and were injected onto the SEC column without cleanup, and the entire analysis was completed in 30 min (80). A fully automated system for analysis of pesticides in water at 0.0051 g/L involved on-line extraction with PRP-1 cartridges followed by C18-LC-tandem PDAUV and postcolumn derivatizationFl detection (81). A method was described for identification and quantitation of 77 neutral, acidic, and basic pesticides, including some s-triazine metabolites, in organically highly loaded groundwater samples using mixed C18/EN SPE coupled to liquidliquid microextraction and RPLCPDA (82). Other Chromatographic Methods and Electrophoresis Advances in the techniques and applications of thin-layer chromatography (TLC) for pesticide analysis published and/or abstracted in the period from mid-1998 through mid-2000 were covered in a separate review in this journal (83). The following analyses by CE were reported during the past 2 years: paraquat and diquat in plant material (84); sulfonylurea herbicides in water (85) and soil (86); chlormequat chloride in formulations (87); enantiomeric and isomeric separation of 7 pesticides by cyclodextrin-modified

micellar electrokinetic chromatography (MEKC; 88); 18 plant protectants in raw and drinking waters by MEKC (89); carbamate insecticides by micellar capillary electrokinetic chromatography (CEC or capillary electrochromatography) with decanoyl-N-methylglucamide (MEGA 10)borate and sodium dodecyl sulfate (SDS) surfactants (90); 16 PAHs by CEC (91); and imazapyr, imazamox, imazapic, imazethapyr, imazaquin, and imazamethabenz (meta and para) in soil (92). Although papers such as these continue to be published, CE is not nearly as popular as GC and LC for pesticide residue analysis. Spectrophotometric Methods Despite the primary importance of chromatographic methods for pesticide analysis, new spectrophotometric analyses continue to be developed. These relatively simple methods based on older technology may be valuable for use in certain countries where expensive and complex instrumentation is not available readily for use. A trend has been to combine flow-injection (FI) with spectrophotometry. Examples of new spectrophotometric determinations include the following: ferbam in wheat grains and commercial sample by converting it to iron(II)-bathophenanthroline-tetraphenylborate complex, which was then adsorbed onto microcrystalline naphthalene and the absorbance measured at 534 nm against a reagent blank (93); and carbamate pesticides in formulated products and water samples by coupling with diazotized 2,4,6-trimethylaniline and FI-spectrophotometry at 550 nm (94). Immunochemical Methods Pesticide and industrial chemical residue analyses in a variety of samples have been described using enzyme-linked immunosorbent assay (ELISA) test kits (95), laboratory-developed competitive ELISA (96), direct competitive ELISA and flow injection immunoaffinity analysis (FIIAA; 97), plate ELISA (98), ASEELISA (99), and quenching fluoroimmunoassay (100), among other formats. James Lawrence, winner of the 1999 AOAC INTERNATIONAL Harvey W. Wiley Award, is developing reusable, pocket-size immunoaffinity cartridges and columns for use in a manner similar to SPE for selectively retaining a single pesticide or class of pesticides from a sample matrix, followed by elution with ethanol or methanol prior to determination (101). The application of commercial immunoaffinity cartridges to food analysis was described (102). The following immunochemical methods are additional examples of those reported in the review period: application of a newly isolated transgenic tobacco peroxidase as a chemiluminescent label for pesticide immunoassay using 2,4-dichlorophenoxyacetic acid (2,4-D) as a model compound (103); detection of simazine in water, milk, and juices based on use of oppositely charged water-soluble polyelectrolytes in ELISA and dot blot formats of the immunoassay (104); and determination of endothall in environmental water samples (105) and glyphosate in community water systems (106) by anion exchange SPE and a direct-competitive ELISA.

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Miscellaneous Analytical Studies, Methods, and Applications

Analysis of Compounds Related to Pesticides


PCBs, chlorinated dioxins, PAHs, and polybrominated aromatic hydrocarbons are industrial compounds that may appear in samples being analyzed for pesticides. An interesting article titled Dioxin Food Crisis in Belgium (115) explained how an analytical chemists idea of linking dioxins and PCBs allowed feed, meat, egg, and poultry samples to be analyzed much more quickly and inexpensively for PCBs rather than for dioxins. Based on the results obtained, the Belgian government decided that PCB-free products were dioxin free and could return to the market. The PCB GC method used was unvalidated and unpublished, but analytical expediency dictated its use; 50 samples could be screened per day per GC instrument at $150 per sample compared with the official government HRMS method for dioxins requiring $1700$1800 per sample and a long analysis time. Three certified reference materials of PCBs in pork fat were produced to support PCB analyses in Belgium (116). A method and quality assurance (QA) procedures for analysis of PCBs and OC pesticides in mussels, seal blubber, and bird and fish liver were described. The method included a wet, cold-blend or Soxhlet extraction; cleanup through a multilayer column containing 10% waterdeactivated aluminum oxide, activated silica, sulfuric acidimpregnated silica, and sodium sulfate; and dual-column GCECD using an autosampler (117). A mixture of PCBs and OC pesticides was analyzed in human serum by hexanediethyl ether extraction, fractionation on Florisil and silica gel columns, and dual-column CGCECD (118). PCB levels in human serum from the Housatonic River area (Massachusetts) were compared using hexaneethyl acetate extraction of methanol-denatured serum, micro silica gel column cleanup, and quantitation as total Aroclor 1260 by megabore and dual capillary column GCECD (119). The maternal body burden of dioxins, dibenzofurans, and OC pesticides in Japanese mothers was studied in an analysis of breast milk by CGCECD and HRGC/MS at ngpg/g levels (120). An approach was described for independent-matrix removal of PAHs from solid samples based on focused microwave-assisted Soxhlet extraction (FMASE) with on-line fluorescence monitoring. FMASE was shown to be as efficient as conventional Soxhlet extraction for extracting PAHs from soils but with a drastic reduction of both extraction time and organic solvent disposal (121).

Method Validation and Interlaboratory Studies


Virtually all newly published pesticide residue methods contain some degree of validation data, such as recovery, precision, limit of detection, limit of quantitation, selectivity, ruggedness, speed, simplicity, and/or cost. These values are for the most part not reported in this review. A joint U.S. Environmental Protection Agency (EPA)American Chemical Society (ACS) study of the analysis of water and soil samples for pesticides and other contaminants using prescribed cookbook methods developed by EPA in the 1970s and early 1980s versus newer techniques, developed by the participating laboratories, that meet certain analytical standards (performance based measuring systems, PBMS) was described (107). Results with spiked samples were mixed, and many laboratories were reluctant to participate and disrupt their regular operations to develop new analytical techniques, even though they might save time and money eventually. An overview was presented of a Canadian program for proficiency testing of environmental laboratories and site assessments based on ISO/IEC Guide 25 (108). In an interlaboratory study of the determination of the herbicides atrazine, bromacil, chlorpyrifos, and metolachlor from water samples after concentration on Empore SPE disks, average recoveries were >70% for all compounds except bromacil, the GC detection of which was problematic at some locations (109). Assays of urinary 3,5,6-trichloro-2-pyrinidol in the general Italian population by HRGCECD and HRGC/MS were validated by an interlaboratory study, and preliminary results were presented (110). After a 14-laboratory collaborative study of a multiresidue method for determining synthetic pyrethroid pesticides in agricultural products at 0.0951.9 mg/kg based on acetonitrilewater (2 + 1) or acetone extraction, partitioning with hexane and then acetonitrile, cleanup on a 5% water deactivated Florisil column with diethyl etherhexane (6 + 94) eluent, and GCECD, the method was adopted First Action by AOAC INTERNATIONAL (111). A related interlaboratory study involving GC/MS identification and quantitation of pyrethroids in agricultural products was also published (112). Charles Parfitt, Jr, AOAC INTERNATIONAL General Referee for Multiresidue Methods, reported on progress in the areas of comprehensive multiresidue methodology, pesticides in nonfatty foods using SFE and GC/MS, SFE of pesticide residues in foods, and synthetic pyrethroids during 1999 (113) and 2000 (114). Bernadette McMahon, AOAC INTERNATIONAL General Referee for Organohalogen Residues and Fumigants, reported on 5 topics in 1999 (113): chlorinated dioxins, methyl bromide, phosphine, PCBs in blood, and PCP residues in gelatin. AOAC INTERNATIONAL General Referee W. Harvey Newsome reported (114) that a collaborative study on glyphosate was completed and the report forwarded to the General Referee and Statistician for review.

Exposure and Monitoring Studies


A new monitoring system for 18 fungicides, 30 insecticides, 42 herbicides, and 10 degradation products found in polluted Japanese river waters was established based on SPE on a styrene-divinylbenzene copolymer; elution with acetone, hexane, and ethyl acetate; and GC/MS (122). Results of the following monitoring studies were reported for pesticide residues: 802 fruit and 1536 vegetable samples collected in the period 19911995 and analyzed using multiresidue methodology specified in the FDAs PAM (123); a total diet study to estimate intake of OC, carbamate,

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benzimidazole, and phenylurea residues in Kuwait using PAM GPC, GC, and LC methods (124); residues of 14 OC pesticides in medicinal plants sold in Coimbra, Portugal, using hexane extraction, Florisil SPE, and GCECD (125); benzoylphenylurea insecticides in pome fruit and fruiting vegetables as found during the Dutch pesticide monitoring program in 19951998 using C18LCPDAUV with an acetonitrilewater gradient after acetone extraction, partitioning with dichloromethanepetroleum ether, and amino-bonded SPE (126); OP pesticides on vegetables in Trinidad, West Indies, collected in 19961997 as determined by the Luke et al. extraction method and GCFPD (127); 52 pesticides in Egyptian fruits and vegetables collected in 1995 and analyzed according to the Luke et al. extraction method and GCECD and NPD (128); the effect of household preparations of vegetables, cereals, and fruits on the residues of OC, OP, and organonitrogen (ON) pesticides as determined by traditional solvent extraction and column cleanup methods and GCECD, FPD, and NPD (129); dietary intake of OC pesticides in foods from Hsinchu, Taiwan, as determined by hexane extraction, Florisil cartridge SPE, and GCECD (130); OC contaminants in microlayer and subsurface water of Alexandria Coast, Egypt, as determined by dichloromethane extraction, Florisil chromatographic cleanup, and GCECD with GC/MS confirmation (131); OC and OP pesticide and fungicide residues in 4128 food samples determined by GCECD, GCNPD, LCUV, and spectrophotometry (132) and chlormequat and mepiquat in grain determined by LC/MSMS (133; results from the Danish National Pesticide Survey); priority pesticides and other organic pollutants in river water from Portugal by GC/MS and LC/APCIMS (134); and pesticide residues in 300 citrus fruit samples from different countries using 2 different methods, one involving organic solvent extraction and the other SFE (135).

and atrazine mobility in soil using GCECD (145); persistence of hexaconazole fungicide in soils using hexane extraction and GCECD (146); and impact of redox conditions on metolachlor and metribuzin degradation in Mississippi flood plain soils determined by wide bore CGCECD (147).

Reviews and Additional New Analytical Studies


Reviews were published on the following topics: the analysis of fumigant residues, including the main current fumigants phosphine and methyl bromide and the new fumigants carbonyl sulfide and ethyl formate (148); determination of herbicide residues in cereals, fruits, and vegetables (149); pesticide residue determination in fruit and vegetables by GC/MS (150); and trends in environmental analysis, including pesticides (151). Dimethoxydithiophosphate (DDTP) in water at 5 ppb was determined indirectly as Bi(DDTP)3 by flow injection analysis using liquidliquid extraction and atomic absorption spectrometry with hydride generation of BiH3 (152). Screening of PCP-contaminated wood by thermodecomposition sampling and photoacoustic detection using a new instrument that requires no added chemicals and can be used in the field, such as at wood recycling plants, was reported (153). References
(1) Sherma, J. (1999) J. AOAC Int. 82, 561574 (2) Shurmer, B., & Pawliszyn, J. (2000) Anal. Chem. 72, 36603664 (3) Mol, H.G.J., Hankemeier, T., & Brinkman, U.A.T. (1999) LC-GC 17, 544, 546, 548550, 552, 554555 (4) Cuppett, C.M., Findeis, P.M., Klotz, J.C., Woods, L.A., & Strein, T.G. (1999) LCGC 17, 532, 534, 536, 538, 540, 542 (5) Lehotay, S. (2000) Fast Multiresidue Analysis of Pesticides, Presented at the 114th AOAC INTERNATIONAL Annual Meeting & Exposition, September 1014, Philadelphia, PA, Abstract No. B-1601 (6) Gou, Y., & Pawliszyn, J. (2000) Anal. Chem. 72, 27742779 (7) Martinez, K., Ferrer, I., & Barcelo, D. (2000) J. Chromatogr. A 879, 2737 (8) Steinheimer, T.R. (2000) Residues of Corn/Soybean Herbicides in Water: Enhancing Both Selectivity of Determination and Confirmation of Identity Using Liquid Chromatography with Ion Trap Mass Spectrometry/Mass Spectrometry, Presented at the Fall, 2000 National Meeting of the American Chemical Society, Division of Agrochemicals, Picogram and Abstracts, Issue No. 59, Abstract No. 13 (9) Jeannot, R., Sabik, H., Sauvard, E., & Genin, E. (2000) J. Chromatogr. A 879, 5171 (10) Santos, T.C.R., Rocha. J.C., & Barcelo, D. (2000) J. Chromatogr. A 879, 312 (11) David, M.D., Campbell, S., & Li, Q.X. (2000) Anal. Chem. 72, 36653670 (12) Tomy, G.T., & Stern, G.A. (2000) Anal. Chem. 72, 48604865 (13) Diserens, H., Schenk, G., & Perisset, A. (1999) Application of Accelerated Solvent Extraction (ASE) for the Determination of Pesticide Residues in Foods, Presented at the 113th

Degradation, Persistence, Leaching, Mobility, and Metabolism Studies


Pesticide analytical methods are used extensively in studies of pesticides on foods and in the environment. Examples of such studies include photodegradation of selected herbicides in water and soil as determined by GC (136); determination of acid metabolites of acetochlor residues in groundwater (137); determination of chloroacetanilide metabolites in water by LCPDAUV and LC/MS (138); fate of metolachlor under subirrigation in a sandy soil as determined by magabore CGCNPD (139); leachability of 5 herbicides in South Australian soils with analysis by C18 SPE and GCNPD (140); persistence, degradation, and leaching of coumaphos in soil with analysis by TLC, LCUV, and LC-scintillation counting of radioactive compounds in eluted fractions (141); the effect of storage temperature on degradation of methidathion in fortified orange and peach juices as determined by GCNPD (142); comparison of photodegradation of atrazine and desethylatrazine in water samples containing titanium hydroxide/hydrogen peroxide and ferric chloride/hydrogen peroxide as determined by C18 SPE, GCNPD, and GC/MS (143); degradation of parathion methyl on field sprayed apples and stored apples using ethyl acetate extraction and GCNPD (144); alachlor, metolachlor, simazine,

SHERMA: JOURNAL OF AOAC INTERNATIONAL VOL. 84, NO. 5, 2001 1309 AOAC INTERNATIONAL Annual Meeting & Exposition, September 2630, Houston, TX, Abstract No. F-1203 Covino, L., Ezzell, J., & Joyce, R. (1999) Determination of PCBs and Lipids in Marine Tissue Using Accelerated Solvent Extraction, Presented at the 113th AOAC INTERNATIONAL Annual Meeting & Exposition, September 2630, Houston, TX, Abstract No. G-201 Cavalier, T., Nejad, H., & Safarpour, M.M. (2000) Considerations in the Use of Capillary Electrophoresis in the Agrichemical Industry, Presented at the 114th AOAC INTERNATIONAL Annual Meeting & Exposition, September 1014, Philadelphia, PA, Abstract No. 1204 Safarpour, D., Picard, K., Zeng, M., & Katz, S. (2000) CE/ESIMS Applications to Formulated Products and Environmental Samples, Presented at the 114th AOAC INTERNATIONAL Annual Meeting & Exposition, September 1014, Philadelphia, PA, Abstract No. 1205 Krynitsky, A.J. (2000) Exploring CEUV and CE/MS as Alternatives for Analyzing More Polar Pesticides, Presented at the 114th AOAC INTERNATIONAL Annual Meeting & Exposition, September 1014, Philadelphia, PA, Abstract No. 1206 Vetter, W., & Luckas, B. (2000) Chemosphere 41, 499506 Petty, J.D., Orazio, C.E., Huckins, J.N., Gale, R.W., Lebo, J.A., Meadows, J.C., Echols, K.R., & Cranor, W.L. (2000) J. Chromatogr. A 879, 8395 Cook, J., Beckett, M.P., Reliford, B., Hammock, W., & Engel, M. (1999) J. AOAC Int. 82, 14191435 Cook, J., Engel, M., Wylie, P., & Quimby, B. (1999) J. AOAC Int. 82, 313326 Sannino, A., Bandini, M., & Bolzoni, L. (1999) J. AOAC Int. 82, 12291238 Navarro, S., Oliva, J., & Barba, A. (2000) J. AOAC Int. 83, 12391243 Crespin, M.A., Gallego, M., & Valcarel, M. (1999) Anal. Chem. 71, 26872696 Colume, A., Cardenas, S., Gallego, M., & Valcarel, M. (2000) J. Chromatogr. A 882, 193203 Schenck, F.J. (2000) Determination of Organochlorine and Organophosphorus Pesticide Residues in Milk Using a Solid-Phase Extraction Cleanup, Presented at the 114th AOAC INTERNATIONAL Annual Meeting & Exposition, September 1014, Philadelphia, PA, Abstract No. B-1301 Curtis, A.S., Putnam, R.A., Auclair, T.R., Corte-Real, L., Shrestha, P.S., & Clark, J.M. (1999) Analysis of Massachusetts Groundwater Monitoring Samples Using a Polymeric Solid-Phase Extraction Method, Presented at the Fall, 1999 National Meeting of the American Chemical Society, Division of Agrochemicals, Picogram and Abstracts, Issue No. 57, Abstract No. 161 Crescenzi, C., DAscenzo, G., Di Corcia, A., Nazzari, M., Marchese, S., & Samperi, R. (1999) Anal. Chem. 71, 21572163 Sabik, H., & Jeannot, R. (2000) J. Chromatogr. A 879, 7382 Ferrer, I., Barcelo, D., & Thurman, E.M. (1999) Anal. Chem. 71, 10091015 Fest, G.A., Ren, A., Obare, J., Glover, J., & Hajipour, G. (1991) EPA 549.1: Method Performance Extraction and Analysis of Diquat and Paraquat in Drinking Water by HPLC, Presented at the 113th AOAC INTERNATIONAL Annual Meeting & Exposition, September 2630, Houston, TX, Abstract No. F-1301 Hogendoorn, E.A., Djikman, E., Baumann, B., Hidalgo, C., Sancho, J.-V., & Hernandez, F. (1999) Anal. Chem. 71, 11111118 Li, N., & Lee, H.K. (2000) Anal. Chem. 72, 30773084 Bjarnason, B., Chimuka, L., & Ramstrom, O. (2000) Anal. Chem. 72, 21522156 Batlle, R., Sanchez, C., & Nerin, C. (1999) Anal. Chem. 71, 24172422 Hernandez, F., Beltran, J., Lopez, F.J., & Gaspar, J.V. (2000) Anal. Chem. 72, 23132322 Weichbrodt, M., Vetter, W., & Luckas, B. (2000) J. AOAC Int. 83, 13341343 Yoshi, K., Okada, M., Tsumura, Y., Nakamura, Y., Ishimitsu, S., & Tonogai, Y. (1999) J. AOAC Int. 82, 12391245 Guo, F., Li, Q.X., & Alcantara-Licudine, J.P. (1999) Anal. Chem. 71, 13091315 Valverde, A., Aguilera, A., Rodriguez, M., & Brotons, M. (2000) Evaluation of Supercritical Fluid Extraction-Aminopropyl Solid Phase In-Line Cleanup for Analysis of Pesticide Residues in Cereals, Presented at the 114th AOAC INTERNATIONAL Annual Meeting & Exposition, September 1014, Philadelphia, PA, Abstract No. B-1505 Sadlo, S. (2000) J. AOAC Int. 83, 214219 Bernal, J.L., Jiminez, J.J., del Nozal, M.-J., Higes, M., & Llorente, J. (2000) J. Chromatogr. A 882, 239243 Tsigouri, A., Menkissoglu-Spiroudi, U., Thrasyvoulou, A.T., & Diamantidis, G.C. (2000) J. AOAC Int. 83, 12251228 Gil Garcia, M.D., Galera, M.M., Espada, M.D.C.P., Frenich, A.G., & Vidal, J.L.M. (2000) J. AOAC Int. 83, 10681075 Jansson, C. (2000) J. AOAC Int. 83, 714719 Battu, R.S., Kalra, R.L., & Dhillon, R.S. (2000) J. AOAC Int. 83, 569578 Menkissoglu-Spiroudi, U., Diamantidis, G.C., Georgiou, V.E., & Thrasyvoulou, A.T. (2000) J. AOAC Int. 83, 178182 Navarro, S., Barba, A., Navarro, G., Vela, N., & Oliva, J. (2000) J. Chromatogr. A 882, 221229 Oliva, J., Barba, A., Vela, N., Melendreras, F., & Navarro, S. (2000) J. Chromatogr. A 882, 213220 Mastovska, K., Hahslova, J., & Krivankova, J. (2000) Incorporation of the PVT Injection Technique into a Multiresidue Method for the Analysis of Pesticides in Food Matrices, Presented at the 114th AOAC INTERNATIONAL Annual Meeting & Exposition, September 1014, Philadelphia, PA, Abstract B-1603 Yokley, R.A., Shen, N., & Cheung, M.W. (2000) J. AOAC Int. 83, 12291238 Lehotay, S.J. (2000) J. AOAC Int. 83, 680697 Sheridan, R.S., & Meola, J.R. (1999) J. AOAC Int. 82, 982990 Mol, H.G.J., Sunarto, S., & Steijger, O.M. (2000) J. Chromatogr. A 879, 97112 Soleas, G.J., Yan, J., Hom, K., & Goldberg, D.M. (2000) J. Chromatogr. A 882, 205212 Wehner, T.A., Morneweck, L.A., Hicks, M.B., & Payne, L.D. (2000) HPLC Fluorescence Method To Determine Residues of Emamectin Bebzoate and Its Metabolites on Vegetables, Presented at the Fall, 2000 National Meeting of

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1310 SHERMA: JOURNAL OF AOAC INTERNATIONAL VOL. 84, NO. 5, 2001 the American Chemical Society, Division of Agrochemicals, Picogram and Abstracts, Issue No. 59, Abstract No. 8 Ohmes, G.A., & Mueller, T.C. (1999) J. AOAC Int. 82, 12141216 Tsiropoulos, N.G., Aplada-Sarlis, P.G., & Miliadis, G.E. (1999) J. AOAC Int. 82, 213216 Pfenning, A.P., Roybal, J.E., Turnipseed, S.B., Gonzales, S.A., & Hurlbut, J.A. (1999) J. AOAC Int. 82, 12241228 Mao, Y., & Carr, P.W. (2000) Anal. Chem. 72, 27882796 Gennari, M., Ferraris, L., Negre, M., & Cignetti, A. (2000) J. AOAC Int. 83, 10761081 Hernandez, F., Hidalgo, C., & Sancho, J.V. (2000) J. AOAC Int. 83, 728734 van Lishaut, H., & Schwack, W. (2000) J. AOAC Int. 83, 720727 Fernandez-Alba, A.R., Tejedor, A., Aguera, A., Contreras, M., & Garrido, J. (2000) J. AOAC Int. 83, 748755 Mol, H.G.J., Van Dam, R.C.J., Vreeken, R.J., & Steijger, O.M. (2000) J. AOAC Int. 83, 742747 Hartmann, H., Burhenne, J., Mueller, K., Frede, H.G., & Spiteller, M. (2000) J. AOAC Int. 83, 762770 Startin, J.R., Sykes, M.D., Taylor, J.C., Hird, S.J., Jackson, K., Fussell, R.J., & Hill, A.R.C. (2000) J. AOAC Int. 83, 735741 Krynitsky, A.J., Stout, S.J., Nejad, H., & Cavalier, T.C. (1999) J. AOAC Int. 82, 956962 Mogadati, P., Louis, J.B., & Rosen, J.D. (1999) J. AOAC Int. 82, 705715 van der Heeft, E., Djikman, E., Baumann, R.A., & Hogendoorn, E.A. (2000) J. Chromatogr. A 879, 3950 Schwack, W. (2000) Analysis of Residues of Urea Pesticides in Fruits and Vegetables Using SFE and LC/MS, Presented at the 114th AOAC INTERNATIONAL Annual Meeting & Exposition, September 1014, Philadelphia, PA, Abstract No. B-1606 Richardson, S.D. (2000) Anal. Chem. 72, 44774496 Glassmeyer, S.T., Shanks, K.E., & Hites, R.A. (1999) Anal. Chem. 71, 14481453 Jiminez, J.J., Bernal, J.L., del Nozal, M.J., & Martin, M.T. (2000) J. AOAC Int. 83, 756761 Grange, A.H., & Sovocool, G.W. (1999) J. AOAC Int. 82, 14431457 Uchimura, T., & Imasaka, T. (2000) Anal. Chem. 72, 26482652 Buchholz, B.A., Fultz, E., Haack, K.W., Vogel, J.S., Gilman, S.D., Gee, S.J., Hammock, B.D., Hui, X., Wester, R.C., & Maibach, H.I. (1999) Anal. Chem. 71, 35193525 Fillion, J., Sauve, F., & Selwyn, J. (2000) J. AOAC Int. 83, 698713 Yamazaki, Y., & Ninomiya, T. (1999) J. AOAC Int. 82, 14741478 Stry, J.J., Amoo, J.S., George, S.W., Hamilton-Johnson, T., & Stetser, E. (2000) J. AOAC Int. 83, 651659 Patsias, J., & Papadopoulou-Mourkidou, E. (1999) J. AOAC Int. 82, 968981 Vandecasteele, K., Gaus, I., Debreuck, W., & Walraevens, K. (2000) Anal. Chem. 72, 30933101 Sherma, J. (2001) J. AOAC Int. 84, 993999 Krynitsky, A.J. (1999) The Analysis of More Polar Pesticides by Capillary Electrophoresis, Presented at the 113th AOAC INTERNATIONAL Annual Meeting & Exposition, September 2630, Houston, TX, Abstract No. 701 Hickes, H., & Watrous, M. (1999) J. AOAC Int. 82, 15231533 Menne, H.J., Janowitz, K., & Berger, B.M. (1999) J. AOAC Int. 82, 15341541 Fang, L., & Zeng, M. (1999) Quantitative Methods for Analysis of Chlormequat Chloride and Other Ionic Compounds in Formulated Pesticide Products Using Capillary with Indirect UV Detection, Presented at the 113th AOAC INTERNATIONAL Annual Meeting & Exposition, September 2630, Houston, TX, Abstract No. 708 Shea, D., Penmetsa, K.V., & Leidy, R.B. (1999) J. AOAC Int. 82, 15501561 Stutz, H., & Malissa Jr, H. (1999) J. AOAC Int. 82, 15101522 Tegeler, T., & El Rassi, Z. (1999) J. AOAC Int. 82, 15421549 Vallano, P.T., & Remcho, V.T. (1999) J. AOAC Int. 82, 16041612 Nejad, H., Cavalier, T., Safarpour, M.M., Picard, G., Krynitsky, A.J., & Stout, S.J. (2000) Capillary Electrophoresis Determinative and LC/MS Confirmatory Method for Imazapyr, Imazamox, Imazapic, Imazethapyr, Imazaquin, and Imazamethabenz (meta and para) Residues in Soil, Presented at the 114th AOAC INTERNATIONAL Annual Meeting & Exposition, September 1014, Philadelphia, PA, Abstract No. 1201 Malik, A.K. (2000) J. AOAC Int. 83, 971975 Alvarez-Rodriguez, L., Esteve-Romero, J., Escrig-Tena, I., & Alvarez-Coque, M.C.G. (1999) J. AOAC Int. 82, 937947 Chen, A.W. (2000) ELISA Method in Determination of Sulfentrazone and the Acid Metabolite in Water Samples, Presented at the Spring, 2000 National Meeting of the American Chemical Society, Division of Agrochemicals, Picogram and Abstracts, Issue No. 58, Abstract No. 124 Watanabe, T., Shan, G., Leeman, W.R., Gee, S.J., & Hammock, B.D. (2000) Residue Analysis of Permethrin in Food by Enzyme Immunoassay, Presented at the Spring, 2000 National Meeting of the American Chemical Society, Division of Agrochemicals, Picogram and Abstracts, Issue No. 58, Abstract No. 119 Kraemer, P.M. (2000) Developments and Optimizations of Two Different Immunoassay Formats for Isoproturon: ELISA and FIIAA, Presented at the Spring, 2000 National Meeting of the American Chemical Society, Division of Agrochemicals, Picogram and Abstracts, Issue No. 58, Abstract No. 121 Cullen, S.J., Van Emon, J.M., Robbins, K.-L., & Reed, A.W. (2000) Immunoassays for Food Analysis, Presented at the Spring, 2000 National Meeting of the American Chemical Society, Division of Agrochemicals, Picogram and Abstracts, Issue No. 58, Abstract No. 114 Chuang, J.C., Hart, K., Chang, J.S., Reed, A.W., & Van Emon, J.M. (2000) Evaluation of Analytical Methods for Determining Pesticides in Baby Food and Adult Duplicate-Diet Samples, Presented at the Spring, 2000 National Meeting of the American Chemical Society, Division of Agrochemicals, Picogram and Abstracts, issue No. 58, Abstract No. 109 Matveeva, E.G., Kennedy, I.M., Shan, G., Gee, S.J., & Hammock, B.D. (2000) Homogeneous Fluoroimmunoassay for

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SHERMA: JOURNAL OF AOAC INTERNATIONAL VOL. 84, NO. 5, 2001 1311 the Detection of Esfenvalerate Metabolite, Presented at the Spring, 2000 National Meeting of the American Chemical Society, Division of Agrochemicals, Picogram and Abstracts, Issue No. 58, Abstract No. 113 Anonymous (1999) Inside Laboratory Management, June, 3133 Rejeb, S.B., Cleroux, C., Querry, J., Streng, C., Lawrence, J.F., Khayat-Frydman, C., Le Goffic, F., & Sarl, A. (2000) Evaluation of Commercially Available Immunoaffinity Cartridges for Selective Extraction of Pesticides in Food, Presented at the 114th AOAC INTERNATIONAL Annual Meeting & Exposition, September 1014, Philadelphia, PA, Abstract No. B-1504 Dzgoev, A.B., Gararyan, I.G., Lagrimini, L.M., Ramanathan, K., & Danielsson, B. (1999) Anal. Chem. 71, 52585261 Yazynina, E.V., Zherdev, A.V., Dzantiev, B.D., Izumrudov, V.A., Gee, S.J., & Hammock, B.D. (1999) Anal. Chem. 71, 35383543 Bhullar, B.S., Mestemacher, M.A., & Sangha, J.S. (1999) Development of an Enzyme Immunoassay for Measurement of Endothall in Environmental Water Samples, Presented at the Fall, 1999 National Meeting of the American Chemical Society, Division of Agrochemicals, Picogram and Abstracts, Issue No. 57, Abstract No. 162 Bhullar, B.S., Mestemacher, M.A., & Sangha, J.S. (1999) Development of an Ultrasensitive Enzyme Immunoassay for the Analysis of Glyphosate in Community Water Systems, Presented at the Fall, 1999 National Meeting of the American Chemical Society, Division of Agrochemicals, Picogram and Abstracts, Issue No. 57, Abstract No. 135 Hogue, C. (2000) Chem. Eng. News (C&EN), June 12, 3233 Leblanc, M.D., & Wilson, R.G. (1999) Overview of the Standards Council of Canada (SCC)/Canadian Association of Environmental Analytical Laboratories Accreditation Program for Environmental Laboratories, Presented at the 113th AOAC INTERNATIONAL Annual Meeting & Exposition, September 2630, Houston, TX, Abstract No. A-102 Mueller, T.C., Senseman, S.A., Wauchope, R.D., Clegg, C., Young, R.W., Southwick, L.M., Riley, M.B., Moye, H.A., Dumas, J.A., Mersie, W., Mattice, J.D., & Leidy, R.B. (2000) J. AOAC Int. 83, 1327 Aprea, C., Betta, A., Catenacci, G., Lotti, A., Magnaghi, S., Barisano, A., Passini, V., Pavan, I., Sciarra, G., Vitalone, V., & Minoia, C. (1999) J. AOAC Int. 82, 305312 Pang, G.-F., Cao, Y.-Z., Fan, C.-L., Zhang, J.-J., & Li, X.-M. (1999) J. AOAC Int. 82, 186212 Pang, G.-F., Can, Y.-Z., Fan, C.-L., Zhang, J.-J., Li, X.-M., Mu, J., Wang, D.-N., Liu, S.-M., Song, W.-B., Li, H.-P., Wong, S.-S., Kubinec, R., Tekel, J., & Tahotna, S. (2000) J. Chromatogr. A 882, 231238 General Referee Reports (1999) J. AOAC Int. 82, 503507 General Referee Reports (2000) J. AOAC Int. 83, 488490 Erickson, B.E. (1999) Anal. Chem. 71, 541A543A Schimmel, H., Sejeroe-Olsen, B., Konieczka, P., Harbeck, S., Mertens, I., Bester, K., Kramer, G.N., & Pauwels, J. (2000) The Certification of European Reference Materials for PCBs in Pork Fat in the Frame of the Belgian Dioxin Crisis, Presented at the 114th AOAC INTERNATIONAL Annual Meeting & Exposition, September 1014, Philadelphia, PA, Abstract No. B-1506 (117) Cleemann, M., Paulsen, G.B., Storr-Hansen, E., & Fromberg, A. (1999) J. AOAC Int. 82, 11751184 (118) Najam, A.R., Korver, M.P., Williams, C.C., Burse, V.W., & Needham, L.L. (1999) J. AOAC Int. 82, 177185 (119) Reddick, J.A., Bosworth, L.J., Servizio, P., Nassif, J., Timperi, R., Burse, V.W., Najam, A.R., Williams, C.C., & Korver, M.P. (1999) Comparison of PCB Levels in Human Serum Using Megabore and Dual Capillary Columns with Electron Capture Detection, Presented at the 113th AOAC INTERNATIONAL Annual Meeting & Exposition, September 2630, Houston, TX, Abstract No. A-201 (120) Nakagawa, R., Hirakawa, H., Iida, T., Matsueda, T., & Nagayama, J. (1999) J. AOAC Int. 82, 716724 (121) Garcia-Ayuso, L.E., Luque-Garcia, J.L., & Luque de Castro, M.D. (2000) Anal. Chem. 72, 36273634 (122) Tanabe, A., Mitobe, H., Kawata, K., Sakai, M., & Yasuhara, A. (2000) J. AOAC Int. 83, 6177 (123) Ripley, B.D., Lissemore, L.I., Leishman, P.D., Denomme, M.A., & Ritter, L. (2000) J. AOAC Int. 83, 196204 (124) Sawaya, W.N., Al-Awadhi, F.A., Saeed, T., Al-Omair, A., Ahmad, N., Husain, A., Khalafawi, S., Al-Omirah, H., Dashti, B., Al-Amiri, H., & Al-Saqer, J. (1999) J. AOAC Int. 82, 14581465 (125) Lino, C.M., Guarda, L.M.C., & Silveira, I.N. (1999) J. AOAC Int. 82, 12061213 (126) Heimstra, M., Toonen, A., & De Kok, A. (1999) J. AOAC Int. 82, 11981205 (127) Chang Yen, I., Bekele, I., & Kalloo, C. (1999) J. AOAC Int. 82, 991995 (128) Dogheim, S.M., Gad Alla, S.A., El-Marsafy, A.M., & Fahmy, S.M. (1999) J. AOAC Int. 82, 948955 (129) Ramesh, A., & Balasubramanian, M. (1999) J. AOAC Int. 82, 725737 (130) Doong, R.-A., Lee, C.-Y., & Sun, Y.-C. (1999) J. AOAC Int. 82, 677682 (131) Mohammed, A., & Abd-Allah, A. (1999) J. AOAC Int. 82, 391398 (132) Juhler, R.K., Lauridsen, M.G., Christensen, M.R., & Hilbert, G. (1999) J. AOAC Int. 82, 337358 (133) Juhler, R.K., & Vahl, M. (1999) J. AOAC Int. 82, 331336 (134) de Almeida Azevedo, D., Lacorte, S., Vinhas, T., Viana, P., & Barcelo, D. (2000) J. Chromatogr. A 879, 1326 (135) Anastassiades, M., & Scherbaum, E. (2000) Pesticide Residues in Citrus Fruit Analyzed between June 1996 and May 2000, Presented at the 114th AOAC INTERNATIONAL Annual Meeting & Exposition, September 1014, Philadelphia, PA, Abstract No. B-1605 (136) Albanis, T.A., & Konstantinou, I.K. (1999) Photodegradation of Selected Herbicides in Various Natural Waters and Soil-Sorbed Phase Under Environmental Conditions, Presented at the Spring, 1999 National Meeting of the American Chemical Society, Division of Agrochemicals, Picogram and Abstracts, Issue No. 56, Abstract No. 082 (137) Harradine, K.J., & Seymour, M.P. (1999) Use of LC/MSMS for the Simultaneous Determination of Sulfonic Acid and Oxanilic Metabolites of Acetochlor Residues in Water, Presented at the Fall, 1999 National Meeting of the American Chemical Society, Division of Agrochemicals, Picogram and Abstracts, Issue No. 57, Abstract No. 144

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