Z Lebensm Unters Forsch (1983) 177:200 202

LebensmittelUntersuchung und-Forschung
@ J. F. Bergmann Verlag 1983

Zeitschrift fLir

Determination of Hemieellulose, Cellulose and Lignin Contents of Dietary Fibre and Crude Fibre of Several Seed Hulls. Data Comparison
Fulgencio Saura-Calixto, Jaime Cafiellas, J u a n G a r c i a - R a s o Department of Organic Chemistry, University of Palma de Mallorca, Palma de Mallorca, Spain

Bestimmung des HemiceUulose-, Cellulose- und Lignin-Gehaltes der Rohfaser versehiedener Sehalen. Datenvergleich Zusammenfassung. Der G e h a l t a n Hemicellulose, Cellulose u n d Lignin v o n ErdnuB-, Haselnul3-, S o n n e n b l u m e n s a m e n - , Kastanie-, Kiirbissamen-, Eichel-, u n d K o k o s n u B s c h a l e n wurde untersucht. Die Z u s a m m e n setzung der Paare S o n n e n b l u m e n s a m e n u n d Eichel, ErdnuB u n d K i i r b i s s a m e n u n d Haselnul3 u n d K a s t a n i e sind ~ihnlich. D a r a u s k a n n m a n folgern, d a b sie fihnliche Z e l l w a n d z u s a m m e n s e t z u n g e n haben. Grol3e M e n gen v o n Hemicellulose u n d niedrige v o n Cellulose u n d Lignin w u r d e n bei der B e s t i m m u n g der Rohfaser aufgel6st. Summary. The contents of hemicellulose, cellulose a n d lignin in neutral-detergent fibre, a n d acid-detergent fibre in hulls of hazelnuts, peanuts, coconuts, sunflower seeds, p u m p k i n seeds, acorns a n d chestnuts were determined. Similar cell-wall characteristics for sunflower-acorn, p e a n u t - p u m p k i n a n d hazelnut-chestn u t pairs can be deduced from their similar composition. High a m o u n t s of hemicellulose a n d lower ones of cellulose a n d lignin are dissolved in the process of determining crude fibre. The results are discussed.

commended the substitution of CF values for dietary fibre values in tables of food composition. On the other hand, the knowledge of the hemicelluloseand cellulose contents of vegetables may be important for industrial applications such as production of furfural, active carbons and other substances to increase the microbial growth in soils [9, 10] and for use in mixtures for animal feeding.

Experimental
Hulls of hazelnuts (Corylus avellana), peanuts (Arachis hypogaea), coconuts (Cocos nucifera), sunflower seeds (Helianthus annuus), pumpkin seed (Cucurbita pepo), chestnuts (castanea sativa), and acorns (Quercus ilex) were studied. Samples were homogenized and ground to particles of < 0.5 ram. Moisture was determinedby heating at 105 C to constant weight. Treatments with 0.255 N-H2SO4 and 0.13 N-NaOH were performed to determine CF, following AOAC methods [11]. NDF values were obtained by refluxingthe sampleswith sodium lauryl sulfate (pH 7.0) solution during 1 h. Hemicellulosecontents were determined as in loss-weight of the NDF residue when treated with acid detergent, following treatment with 72% HzSO4 and calcination at 550 C to obtain cellulose and lignin contents. Preparation of reagents and assay conditions were performed followingVan Soest procedures [3, 4]. The same method was used to obtain acid detergent fibre (ADF). CF were also treated with acid detergent, 72% H2SO4, and calcination in a similarfashion as for NDF in order to determine its contents of hemicellulose(H), cellulose(C) and lignin (L). Data obtained were the mean of at least four different determinations.

Results and Discussion

Dietary Fibre

Introduction
Fibre has long been considereda food fraction of very little nutritional interest. There is current evidence,however, that its components have a direct effect upon some biochemical and physiological processes. An adequate intake in the diet is now considered necessary. Studies of relationships of a lowered dietary fibre intake with several diseases such as diabetes, cancer of the colon, obesity, disorders in cholesterol metabolism and on its effects in mineral and micronutrient balance, protein digestibility,etc. have been the subject of many papers. Compilations of these are available in the literature [1, 2]. As is known, the use of crude fibre (CF) is not convenientin food analysis because some non-digestibleconstituents are dissolved and some digestiblecomponents remain in the residue during determination. More significant is dietary fibre, where the neutral-detergent fibre (NDF) residue, obtained by treating the vegetablematter with neutral detergent, remains the principal component of the cell walls. Van Soest methods [3, 4] are widely used for its determination, and other modifications have been proposed [5-8]. The FAO has re-

The contents of moisture, N D F , A D F , H, C a n d L for the samples studied are listed in Table 1. As can be observed, all samples have a high N D F c o n t e n t a n d for this reason m a y be considered a potential source dietary fibre. H contents of the sunflower (24.0%), hazelnuts (24.9%) a n d c o c o n u t (31.9%) are of the same order as the p r i m a r y matter to o b t a i n furfural. The contents of L (19.3 to 29.6) are higher t h a n c o r r e s p o n d i n g products used in a n i m a l feeding (e. g. wheat straw, 12%; alfalfa, 9%) a n d its use is only possible as part of n u t r i t i o n a l mixtures. Percentages of H, C a n d L in N D F are included in Table 2. Values of the same order for p e a n u t hulls appear in the literature [12, 13]. We have n o t f o u n d data c o n c e r n i n g other products studied.

F. Saura-Calixto et al.: Hemicelluose, Cellulose and Lignin Contents of Dietary Fibre

Table 1. NDF, ADF, Hemicellulose, Lignin and Lignin contents (% dry matter a)

201

Hull

Moisture % 9.4 _+0.8 10.5-+0.2 16.6_+0.4 22.4_+0.5 12.0_+0.3 6.40.8 11.0-+0.2

NDF % 89.9 1.0 82.7_+0.9 77.8 1.5 70.3 1.4 85.9 _+1.3 89.9 1.3 92.0_+1.0

Hemicellulose % 24.0_+0.7 16.3 -+0.6 20.5 _+0.9 19.9_+1.0 17.5 1.0 31.9_+0.9 24.9_+0.8

Lignin % 23.2 1.0 27.6 _+1.1 21.4 _+1.0 21.9 _+1.3 28.5 -+1.2 19.3 +0.8 29.6 _+1.0

Cellulose % 42.7 _+2.7 38.8 -+2.4 35.9 _+2.6 28.5 _+3.7 39.9 _+3.5 38.7_+3.0 37.5 _+2.8

ADF % 70.0 _+1.3 75.1 -+1.1 67.8 _+2.0 65.9 + 1.6 77.3 _+1.2 66.2_+1.0 74.6_+0.9

Sunflower seed Peanut Acorn Chestnut Pumpkin seed Coconut Hazelnut

a Average value-+standard deviation Table 2. Percentages of hemicellulose,lignin and cellulose in neutral detergent fibre (NDF) Hull Hemicellulose % 26.7 19.7 26.3 28.3 20.4 35.5 27.1 Lignin % 25.8 33.3 27.5 31.1 33.2 21.5 32.2 Cellulose % 47.5 47.0 46.2 40.6 46.4 43.0 40.7

Sunflower seed Peanut Acorn Chestnut Pumpkin seed Coconut Hazelnut

Table 3. Components of crude fibre (CF)

Hull

% Respect dry mattera Crude fibre Hemicellulose Lignin 6.9__0.5 4.5 -+0.3 5.0_+0.5 3.7_+0.3 8.9_+0.8 9.5 _ 0.7 8.7 0.6 20.4-+0.1 25.2 _+1.2 13.2_+0.9 9.8 _+0.9 28.0_+1.4 13.5 1.0 26.4 _+1.1 Cellulose 36.7_+0.9 32.5_+3.0 25.5_+2.4 18.3-+2.2 31.1-+3.2 24.6_+2.6 31.0_+3.1 H2SO4b residue 80.0_+0.8 82.5_+0.9 78.9_+0.7 77.9-+1.0 86.0_+0.9 81.7_+0.9 89.6_+1.0

% Respect crude fibre HemiLigniia cellulose 10.8 7.2 11.4 11.6 13.1 19.9 13.2 31.9 40.5 30.2 30.8 41.2 28.4 39.9 Cellulose 57.3 52.3 58.4 57.6 45.7 51.7 46.9

Sunflower s e e d Peanut Acorn Chestnut Pumpkin seed Coconut Hazelnut

64.0_+0.5 62.2 _+1.5 43.7-+ 1.0 31.8 _+1.0 68.0 1.1 47.6 _+0.9 66.1 _+1.4

a Average value _+standard deviation 0.255 N-H2SO4 (CF treatment)

F r o m the similar percentage of c o m p o n e n t s , it can be considered that the pairs sunflower-acorn, p e a n u t p u m p k i n , h a z e l n u t - c h e s t n u t have similar cell-wall characteristics. The cotents o f C are more u n i f o r m (44.5+3.0), while greater differences a p p e a r for L (29.2_+4.5) a n d H (23.3__5.3), The high H c o n t e n t gives a greater hardness to these samples, especially in coconuts, as in the case o f wood [14]. It m u s t be noticed that the difference between N D F a n d A D F does n o t coincides with the hemicellulose content, which is due to the presence in A D F of other c o m p o n e n t s cited in the literature, such as t a n n i n s a n d

pectins [15, 16]. Small a m m o u n t s of t a n n i n s , in particular, are also sometimes detected in N D F . As these a m o u n t s are n o t significant in N D F c o m p a r i n g with H, C or L contents a n d are also indigestible, their determin a t i o n was omitted.

Comparison of Dietary and Crude Fibre

Table 3 shows the contents of H, C a n d L in the CF. Values in C F are always m a r k e d l y lower t h a n in N D F . C o m p a r i n g the data in tables 2 a n d 3, it can be seen that H is the fraction m o s t p r o n e to loss in the process

202

F. Saura-Calixto et al.: Hemicellulose, Cellulose and Lignin Contents of Dietary Fibre 2. Symposium on Dietary Fiber, Houston, USA, 1980. J Agric Food Chem (1981) 29.'448-471 3. Van Soest PJ, Wine RH (1976) J Assoc Off Agric Chem 50:50 4. Van Soest PJ, Robertson JB (1979) Sistems of analysis for evaluating fibrous feeds. Presented at Proc Stand Analytical Methodology for Feeds. (Otawa) 5. Schaller D (1977) Food Prod Devel 11:70 6. Southgate DAT (1976) Determination of food carbohydrates. Applied Science Publ. London, pp 128-136 7. Jeltema MA, Zabik ME (1980) J Sci Food Agtic 31:820 81 Lintas C, Cappelloni M, Camovale, E (1983) European Conference on Food Chemistry. Proceedings Societ/t Chimica Italiana, Roma, pp. 351-356 9. Linares-Solana A, Lopez Gonzalez J, Molina Sabio M, Rodtiguez Reinoso F (1980) J Chem Tech Biotechnol 30:65 10. Nobile L (1971) Fr Patent 2047193 11. AOAC (1980) Official Methods of Analysis Association of Official Analytical Chemists. Washington DC 12. Crampton EW, Harris LE (1979) Nutticion animal aplicada, Actibia, Zaragoza (Spain), pp. 650-562 13. Collins JL, Post AR (1981) J Food Sci 46:445 14. Morey PR (1977) Como crecen lo firboles. Omega, Barcelona (Spain), pp 14-19 15 Belo PS, de Lumen BO (1981) J Agric Food Chem 29:370 16. Reed JD, McDowell RE, Van Soest PJ, Horvath PJ (1982) J Sci Food Chem 33:213

of determining CF, dissolving in amounts of 69.2 + 10.2%. Although lower, appreciable amounts of C (21.3_+10.6%) and L (22.4_+19.3%) are also dissolved. Pearson coefficients were 14 for H, 49.7 for C and 86 for L, indicating that the variation in the amounts dissolved increase in the order H, C and L. During treatment to obtain CF variable amounts (from 20% for pumpkin, to 50% for coconut) of NDF were dissolved. By treating the samples with 0.255 N-H2SO4 in a similar way for obtaining CF (but omitting the NaOH treatment), residues of higher weights than those corresponding to ADF were obtained in all cases. Considering the CF contents of the products studied against the contents of H, C and L in its NDF, the following equation was obtained: CF=0.18 H+2.14 C+2.00 L - 26.52, with a high correlation coefficient (r = 0.988) and low standard deviation (s= 0.94). This expression is in accord with the above statistical considerations.

References
1. F.A.O. (1980) Los carbohidratos en la nutrici6n humana. Informe conjunto FAO/OMS. Organizaci6n de las Naciones Unidas para ta Agricultura y la Alimentaci6n. Roma, pp. 71-79

Received April 14, 1983

Aus der Industrie

Eppendorf Varipette 4720
Eppendorf Gerdtebau Netheler + Hinz GmbH (Postfach 65 06 70, D-2000 Hamburg 65, Tel. 040/53801-1).

Mit der Eppendorf Varipette 4720 ist das Pipettieren im Milliliterbereieh genau so einfach und sicher wie mit der bewiihrten Varipette 4710 bereits im gl-Bereich. Start einer Vielzahl yon Glaspipetten deckt nur eine Varipette 4720 den gesamten Bereich yon 1 ml bis 10 ml liickenlos ab. Jedes gewlinschte Zwischenvolumen lggt sich miihelos und exakt re-

produzierbar an der vierstelligen Digitalanzeige kommarichtig einstellen. Da es weder Verluste durch Glasbruch noch zeitraubendes Spiilen gibt, macht sich die Anschaffung der Varipette bereits nach kurzer Zeit bezahlt. Die pipettierte F1/issigkeit kommt nicht mit der Varipette in Kontakt, sondern nut mit dem ,,varitip", einem Einmal-Verbrauchsartikel aus Kunststoff, der mit einer Klemmvorrichtung sicher aber leicht austauschbar mit dieser verbunden ist. Varitips gibt es in zwei Ausfiihrungen: varitips L mit besonders langem und schlankem Vorderteil zur Entnahme

aus enghalsigen Gef/iBen bzw. Megkolben mit max. 170 mm Eintauchtiefe sowie varitips P nach dem Prinzip der Direktverdr/ingung ffir alle iibrigen Anwendungen. Varitips werden nach Gebrauch einfach durch neue ersetzt. Das vermeidet Verschleppungsfehler und eriibrigt zeitraubendes Spfilen. Das Pipettieren mit der Vatipette 4720 ist besonders einfach und beschr~tnkt sich auf das Herunterdriicken des Druckknopfes zum Fiillen und Entleeren des varitip. Dabei ist nur eine Hand beteiligt, wghrend die andere frei bleibt.