Lebensm.-Wiss. u.-Technol.

, 33, 72}79 (2000)

Hydration Properties of Dietary Fibre and Resistant Starch: a European Collaborative Study
James A. Robertson*, Francois D. de Monredon, Patrick Dysseler, Fabienne Guillon, Renato Amado ` and Jean-Francois Thibault

J. A. Robertson: Food Biopolymers Section, Institute of Food Research, Norwich Research Park, Colney, Norwich NR4 7UA (U.K.) F. D. de Monredon, F. Guillon, J-F. Thibault: Centre de Recherche Agro-alimentaire de Nantes, INRA, Rue de la Geraudiere, BP 71627, 44316 Nantes-03 (France) H ` R. Amado: Department of Food Science, Swiss Federal Institute of Technology, ETH-Zentrum, CH-8092, ` Zurich (Switzerland) P. Dysseler: Department of Food Science, Institut Meurice, CERIA, Avenue Emile Gryzon, B-1070, Brussels (Belgium) (Received May 17, 1999; accepted August 4, 1999)

Hydration properties related to the xbre matrix have been dexned and measured in 19 European laboratories using common methods and the substrates: resistant starches, pea hull, citrus pulp and apple pulp. Swelling and water retention capacity (WRC) were the major hydration properties studied. The objective was to derive standardized methods with an included estimate of experimental variation or statistical tolerance. Measurement of swelling and WRC were complemented by measurement of water absorption and porosity. Swelling ( 7 mL/g) and WRC (&4 g/g) were relatively low for resistant starches and pea hull. Swelling and WRC of citrus (&11 mL/g: & &11 g/g) and apple pulp (&7 mL/g:&5 g/g) were lower than expected, probably reyecting ewects of processing on matrix structure. Coezcient of variation was higher between laboratories than within laboratory. The relationship between swelling, WRC, absorption and porosity, as well as matrix ewects, are discussed. 2000 Academic Press Keywords: dietary "bre; resistant starch; hydration methods; swelling; water retention

Introduction Understanding the perceived health response to "bre in the diet has involved relating health markers to the physicochemical behaviour of "bre during gut transit. This has provided a range of methods of characterizing the physical and chemical properties of the "bre matrix (1}5) and determining how properties are a!ected under physiological conditions (3, 6}9). There is an identi"ed need to de"ne the properties of "bre precisely and also to standardize methods of measurement within the constraints of each de"nition (10; see also 5, 11) so that health-care industries and research organizations have acceptable methods available to them, with known statistical tolerance, to screen proposed "bre-based therapeutic products. Within the EU concerted action group, Pro"bre, clear de"nition and standards for measurement of properties
* To whom correspondence should be addressed. Fax:#44 (0) 1603 507723, E-mail: jim.robertson@bbsrc.ac.uk

were major considerations. For hydration properties, de"nitions arising from Pro"bre were: swelling, &the volume occupied by a known weight of "bre under the conditions used' is measured as settled bed volume; water retention capacity (WRC), &the amount of water retained by a known weight of "bre under the conditions used' is measured by centrifugation and is preferred to either water-holding capacity or water-binding capacity; water absorption, &the kinetics of water movement under de"ned conditions' is measured using a Baumann apparatus or using osmotic pressure/dialysis techniques; porosity, &the accessible volume and pore size' measurement involves pycnometry and solute exclusion techniques. A collaborative study was initiated to measure hydration properties, notably swelling and WRC, using substrates supplied to each laboratory by a common source. The major objective was to standardize methodology and to evaluate the levels of experimental variation expected from each method. The study was undertaken in two stages: stage 1 to test substrates, using standarized methods; and stage 2 to repeat the operation, but to

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Table 1 Characterization of substrates used for the ring tests on hydration properties
Property *Dry weight (g/kg) Dietary "bre (g/kg dry weight) (AIR) (g/kg dry weight) Water-insoluble (g/kg dry weight) Median particle size ( m) } dry } hydrated Speci"c surface area (N ads) (m/kg)  Mean s  Mean s  Pea hull 979.3 10.9 751.2 1.9 953.2 872.8 67 83 1620 Apple pulp 926.6 11.0 511.1 5.0 690.5 610.5 133 150 554 Citrus pulp 951.4 20.9 357.6 10.7 484.8 386.9 139 274 180 Novelose 952.2 14.8 * 999.6 996.7 40 64 421 Eridania 960.8 15.5 * 1000.2 998.3 84 150 334

*Substrates as received: mean and S of dry weight determinations reported by participants 

incorporate modi"cations to make the methods more user-friendly. Measurements of water absorption in relation to porosity were also made to relate swelling, WRC and absorption to matrix structure.

Food, Cergy Pontoise, France) was substituted for citrus pulp as an untested substrate.

Materials and Methods Participating laboratories Participation in the study was open to all members of Pro"bre and outside interest was also encouraged. Participants were mainly members of the processing and physicochemistry group of Pro"bre and most undertook and completed the measurement of swelling and WRC. Measurements of water absorption and porosity was limited to participants with previous experience using the methods involved.

Methods Dietary ,bre analysis. Samples were analysed in triplicate for "bre content using an enzymatic}gravimetric method (12). Alcohol insoluble residues (AIR). These were prepared to characterize the relative contribution of polymeric material from each test substrate. Samples (1 g dry weight) were extracted (;3) in boiling ethanol (30 mL; 5 min; 80}85% v/v). Alcohol-insoluble material from each extraction step was recovered by "ltration. Ethanolic supernatants were discarded and the ethanol insoluble material was dried by solvent exchange, through absolute ethanol (;2) and acetone (;2), to yield a dry white powder. Solubility. Alcohol insoluble residues samples (300 mg) were suspended in distilled water (30 mL) and stirred for 3 h at room temperature (13). Each suspension was centrifuged (3000;g), the supernatant discarded and the pellet washed (;2) in distilled water. Pellets were freeze dried and water insoluble AIR determined from loss in sample weight during extraction. Particle size. Median particle size was determined from particle size distributions generated using laser light di!raction (Malvern Mastersizer IP, MS15 for hydrated samples and PS65 for dry samples). Distributions were made in triplicate for each sample, using 10}20 g sample weight for dry particle size distribution and 1}2 g in an aqueous suspension for hydrated particle size distribution (14). Surface area. Surface area was determined from nitrogen adsorption isotherms, using a Micromeritics, Gemini III 2375 and Vacprep 061 LB system. Samples were degassed for 48 h, to a residual system pressure between 0.2 and 0.5 KPa, prior to generating a Brunauer}Emmet} Teuer BET isotherm using nitrogen at 773 K (15). Swelling. The protocol, derived from the method of Kuniak and Marchessault (16), is outlined in Fig. 1. Test

Study protocol The test substrates, chosen to cover a range of di!erent "bre types, were characterized by a range of physical properties which may be related to hydration properties, e.g. particle size (Table 1). Substrates were distributed to participants with copies of the standardized experimental protocol(s) for swelling and water retention and schedule for the standardized reporting of results. Experimental protocols for each stage of the test were constructed, based on published methods, to limit the number of experimental variables in each protocol before proceeding with the tests. Raw data were collected on dry weight and weights recorded at di!erent stages during each procedure. Data were screened for compliance with the experimental protocol and consistency between participants. Inconsistencies were checked through examination of raw data and, if necessary, contact with the participant. All experimental data complying with the set procedures were included for analysis. The substrates used were commercial preparations. During stage one, substrates were: pea hull (ID Food, Cergy Pontoise, France); citrus pulp (Indulerida SA, Alguaire, Lleida, Spain); Novelose (National Starch and Chemical Co., Neustadt, Germany); and Eridania (Eridania, Beghin-Say, Vilvoorde, Belgium). For stage two, pea hull and Eridania starch were retested and apple pulp (ID

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Fig. 2 Scheme of water retention capacity (WRC)

Fig. 1 Scheme of swelling

substrate (&100 mg dry weight in phase 1; &200 mg dry weight in phase 2) was hydrated in a known volume of distilled water (10 mL), containing 0.02% azide as a bacteriostat, in a calibrated cylinder (1.5 cm diameter) at room temperature. After equilibration (18 h), the bed volume was recorded and expressed as volume/g original substrate dry weight. Swelling of the water-insoluble matrix was measured, although water-extractable material may be present and contribute to the calculation of results. The low swelling ability of the pea and starch identi"ed problems in recording swelling in such samples, so for stage 2 sample weight was increased to 200 mg. =ater retention capacity. The protocol, derived from published methods (2}4, 17) is outlined in Fig. 2. Substrate (&3 g dry weight for pea and starch and &1 g for citrus and apple pulp) was hydrated in 30 mL distilled water, containing 0.02% azide as a bacteriostat, in a centrifuge tube at room temperature. After equilibration (18 h), samples were centrifuged (3,000;g; 20 min). The supernatant was decanted and the sample transferred to a weighed sinter to drain. Sample fresh weight was recorded prior to drying. WRC was calculated as the

amount of water retained by the pellet (g/g dry weight) after transfer to the sinter. Hence, WRC measures water retained by the insoluble matrix. Transfer of the sample to a sinter was identi"ed as a problem stage and major source of experimental variation so was modi"ed for stage 2. The modi"cations involved decanting the supernatant after centrifugation, carefully inverting the tube and leaving the pellet to drain in the tube. This removed the need for sample transfer after centrifugation. =ater absorption. Water absorption characteristics of the test substrates were measured using a Baumann apparatus and/or suction pressure measurements (18}21). The Baumann apparatus consists of a sintered glass plate connected to a horizontal graduated pipette level with the surface of the sinter. The pipette, "lled with distilled water, acts as reservoir to measure rate and extent of water absorption. Test substrate (100 mg) was carefully placed on the glass sinter and the volume of water absorbed recorded to determine absorption g\ dry weight. Suction pressure measurements involved dialysing samples against polyethylene glycol solutions (PEG; MW 10,000) of known osmotic pressure, determined by freezing point depression (20). Hydrated samples (up to 500 mg dry weight) were placed in dialysis sacs (Visking 24/32 Polylabo; 6000}8000 MWCO). Sacs were dialysed (72 h with stirring) against 100 mL of a PEG solution of

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known osmotic potential. Solutions of PEG were prepared to cover an osmotic pressure range from 0}0.7 MPa. After equilibration the fresh weight of sample recovered from the dialysis sacs was recorded, samples were dried and the dry weight was used to determine water absorbed at each suction pressure. Pore size was estimated from suction pressure and surface tension measurements (6, 21).

Data analysis The BCR HOSTAN3 Statistical Package, as used for the purposes of method certi"cation by the EU, was used for analysis of data for swelling and water retention.

for: pea hull, 67%; apple pulp, 41%; and citrus pulp, 17% of the sample. It is important to recognize the presence of &water-soluble' material and its apparent concentration in samples if &absolute' values are required for hydration properties, especially when calculation is based on the original rather than the recovered sample weight, e.g. swelling. In this study, testing methods of measurement was the major objective and these were evaluated in conjunction with a spectrum of properties to more fully characterize each "bre source. Particle size distribution (Table 1) showed median particle size varied between substrates and that the particles swelled when hydrated. Similarly, based on total sample weight, there was an apparent ninefold range in surface area of the substrates, from 180 m/kg for citrus pulp to 1620 m/kg for pea hull.

Results and Discussion Substrate characterization Substrates each had a low moisture content (Table 1) and there was good consistency between participants in reported dry weights. Fibre analysis con"rmed substrates were typical "bre &concentrates', with apple pulp and citrus pulp apparently rich in pectic polysacharides and pea hull rich in cellulose, xylan and pectic polysaccharide. Preparation of AIR distinguished the relative contribution of low molecular weight (ethanol soluble), water extractable and water-insoluble matrix material in each substrate, as supplied rather than after isolation of nonstarch polysaccharides. The extractability of each sample can a!ect interpretation of results for hydration properties. For example, the AACC method (10) was developed for measuring total water retained by a sample, with care taken to retain soluble material, whereas the current methods for WRC and swelling measure the (packed) matrix bulking potential. The resistant starches, Novelose and Eridania, were e!ectively free of alcohol soluble material and contained only negligible water-extractable material. Pea hull was also rich in AIR, most of which were water-insoluble. Apple pulp and especially citrus pulp contained appreciable amounts of alcohol soluble material and the water insoluble matrix accounted for around 60% of the apple pulp but only around 40% of the citrus pulp. In comparison, the water insoluble matrix recovered after "bre analysis accounted Hydration properties The experimental data for the study on swelling and WRC is summarized in Tables 2 and 3. Most participants had some previous experience of measuring hydration properties and the relative precision of data submitted by laboratories with previous, little or no experience was similar. Data provided from laboratory speci"c methods (not shown) were also similar to data provided for the standard protocols. This gave reassurance that the standard protocols were user-friendly and had not introduced unforseen changes in the substrate response due to experimental treatment. Swelling. The range of values for swelling (Table 2) was less than anticipated, due mainly to the low values for citrus pulp and apple. Values were expected to be greater than 20 mL/g, considered typical for a fruit or vegetable "bre concentrate (3). Di!erences could partly be attributed to the presence of water soluble material, but e!ects of processing and consequent matrix structure breakdown were probably more important. This also emphasizes the need to consider processing history when selecting "bre sources for diet therapy and in the interpretation of health response. The statistical analysis showed data were normally distributed but that the variance between laboratories (S ) was higher than within laboratory (S ; Table 2). Agreement within laboratory 

Table 2 Swelling of test substrates (ml/g)*statistics summary

Pea Sample Number of sets Number of replicates Overall mean (x)  s individual values  s within lab. S   CV (%) s between lab S  CV (%) 95% con"dence interval of x  I 19 171 7.48 0.77 0.56 7.5 0.75 10.1 0.37 II 13 117 6.64 0.79 0.37 5.6 0.84 12.7 0.41 Apple II 14 126 7.42 1.15 0.33 4.4 1.00 13.5 0.62 Citrus I 19 171 10.45 1.21 0.70 6.7 1.19 11.3 0.58 Novelose I 19 171 5.65 0.86 0.56 9.9 0.84 14.9 0.42 Eridania I 16 144 7.96 0.67 0.61 7.7 0.64 8.0 0.36 II 11 99 7.43 1.05 0.34 4.6 0.96 12.9 0.55

I"stage 1 test; II"stage 2 test. CV"coe$cient of variation

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Table 3 Water retention capacity of test substrates (g/g)*statistics summary

Pea Sample Number of sets Number of replicates Overall mean (x)  s individual values  s within lab. S   CV (%) s between lab S  CV (%) 95% con"dence interval of x  I 16 144 3.94 0.46 0.36 9.1 0.44 11.2 0.28 II 13 117 3.82 0.40 0.16 4.2 0.36 9.4 0.25 Apple II 13 117 5.43 1.18 0.27 5.0 1.11 20.4 0.67 Citrus I 17 153 10.66 2.34 0.70 6.6 2.33 21.9 1.09 Novelose I 17 153 2.95 0.47 0.13 4.4 0.47 15.9 0.24 Eridania I 13 117 3.49 0.73 0.43 12.4 0.72 20.6 0.44 II 11 99 3.14 0.26 0.17 5.4 0.23 7.3 0.17

I"stage 1 test; II"stage 2 test. CV"coe$cient of variation

and between laboratories was good, although the 95% con"dence interval of the overall mean indicated that experimental variation was relatively high. Increasing the sample weight to 200 mg had no apparent e!ect on the swelling measured. Recording swelling volume was considered easier when using 200 mg and up to 200 mg there was no apparent compaction of sample. Using graduated conical tubes rather than #at-base cylinders also helped when recording low swelling values and tube shape had no apparent e!ect on swelling volume. Standard deviations of the results indicate that modi"cations to the experimental protocol resulted in a slight reduction in experimental variation, which may be partly attributed to an increased familiarity with the method or may indicate that experimental variation is as low as can be expected within the general procedure. =ater retention capacity. Values of WRC (Table 3) were normally distributed and tended to be less than swelling values. Values for citrus and apple were also less than expected ('20 g/g expected) for fruit and vegetable "bre concentrates (1, 3, 5, 11). Modi"cations made to the protocol for stage 2 did not have a major e!ect on WRC, (pea stage 1, 3.9 g/g: stage 2, 3.8 g/g; Eridania stage 1, 3.5 g/g: stage 2, 3.1 g/g). The coe$cient of variance for S and for S was similar to that found for corresponding  samples for swelling but the 95% con"dence interval of the overall mean indicated that experimental variation was relatively high. The s for experimental data indicates  that modi"cations to the protocol for stage 2 resulted in a slight reduction in experimental variation. The e!ect was small and may be partly attributed to an increased familiarity with the method, as well as indicating that experimental variation is as low as can be expected within the procedure. The consistency of data both within laboratory and between laboratories was reassuring for method standardization. The major problem during stage 1 was the transfer of sample after centrifugation. Loss of sample occurred and problems arose in allowing for the water retained in the glass sinter. Results indicate that the method became easier to use during stage 2, although some problems were reported due to pellet loss from the centrifuge tube during draining procedures. Reducing the sample weight could help prevent such losses but may

Fig. 3 E!ect of sample weight on WRC (apple pulp). , single determinations made over a range of sample weights; , mean $s of values from study participants using 1 g or 3 g sample  weight. y"6.57!0.81x; R"0.899

a!ect pellet compaction during centrifugation (see Fig. 3). There may be a need in the future to consider modifying sample weight and/or centrifugal force to give e$cient pelleting and sample retention in the tube. When designing the protocol for WRC one of the criteria was to optimize sample weight to give reproducible results and allow for excess supernatant in the centrifuge tube. Hence, for expected high WRC samples, weight was restricted to 1 g but for low WRC samples 3 g were used. Several participants measured WRC of apple pulp at 1 g and at 3 g sample weight. The values obtained are shown in Fig. 3 against a background pro"le of WRC determined for a range of sample weights. Increasing sample weight led to a decrease in WRC and the values reported by participants were consistent with the observed background pro"le. The decrease in WRC with increased sample weight can in part be explained by the proportionate increase in the contribution from soluble material retained by the pellet at increased sample weight. The presence of soluble material is not a problem when swelling is being measured, since swelling g\ original sample is recorded. However, WRC measurement is based on the sample weight recovered and assumes this to be an insoluble matrix. The ratio of sample weight: solute volume is

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Fig. 4 Water absorption measured using a Baumann apparatus. Values shown with error bars ( s ) are included to illustrate the $  range of variation expected from the method. Inset shows the maintenance of equilibrium full absorption. , pea; , citrus; , Novelose

Fig. 5a Water absorption measured using suction pressure. Values were obtained through equilibrium dialysis against polyethylene glycol (MW 10,000) solutions of known osmotic potential. , pea; , citrus; , Novelose

Fig. 5b Estimation of pore size and pore volume in hydrated samples. Values were calculated from water absorbed against a known suction pressure (Fig. 5a) as the pore volume and with pore radius r estimated from suction pressure (P) and surface tension measurement (s) as r"2s/P (21). , pea; , citrus; , Novelose

therefore important for WRC measurement and it is recommended that account is taken of &soluble' material in the pellet when calculating WRC if absolute values for WRC are required. Absorption and porosity. Rate of water absorption measured using a Baumann apparatus was relatively rapid for each substrate (Fig. 4). The resistant starch was apparently fully absorbed within 1 min. Pea and citrus were extensively absorbed after 2 min, but absorption continued, albeit at a low rate, even after 30 min. The extent

of water absorption, after 30 min, for resistant starch and pea was similar to the WRC measured, but for citrus WRC was much greater than water absorption. This may be related to di!erences in composition, particle and pore size of the samples. Unlike the Baumann apparatus, when rate of absorption or wettability of a dry sample (19) is measured, suction pressure is used to measure absorption or desorption of a hydrated sample at speci"ed suction pressures. As shown in Fig. 5a, at relatively low suction pressure water

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absorption by citrus pulp was high but only a slight increase in suction pressure was required to reduce the absorption capacity. The absorption capacity of resistant starch and pea hull was much lower than for citrus pulp. With resistant starch and pea the contribution of watersoluble material to absorption pressure would be low. Absorption against a suction pressure will mainly depend on the matrix potential of these samples (20, 22) and will also apply to measurements made using the Baumann apparatus (19). With citrus pulp the relatively high watersoluble component can generate a solute potential and contribute to the high absorption observed using suction pressure. At higher suction pressures the extent of water absorption becomes similar for all samples and similar to absorption measured using the Baumann apparatus. This suggests that water absorption measured using the Baumann apparatus mainly measures the pore volume of the microcapillaries ((1 m) (21). Using a range of suction pressures to measure pore volumes, the relative contribution of micropores ((1 m) and macropores ('1 m) to the water associated with the "bre matrix and its relationship to swelling volume and WRC can be obtained (Fig. 5b). For example, water absorbed by starch is mainly in microcapillaries. The proportion of water in microcapillaries may be related to particle size since smaller particles, e.g. pea and starch, will have a higher packing density but particle composition and structure will also contribute the overall distribution of water.

France; C. Renard, F. Guillon, INRA, Nantes, France; G. Abraham, LMTA, Universite de la Rochelle, France; H G. Dongowski, DIFE, Bergholz-Rehbrucke, Germany; K C. Niemann, IFLT, Technische Universitat, Berlin, K Germany; U. Schlemmer, BFE, Karlsruhe, Germany; T. Sheehy, University College Cork, Ireland; D. Armstrong, H. Luyten and C. T. Ponne, ATO-DLO, Wageningen, The Netherlands; H. A. Schols, WAU, Wageningen, The Netherlands; M. T. Amaral-Collaco, INETI, Lisbon, Portugal; F.-D. Saura-Calixto and L. Bravo, Instituto del Frio (CSIC), Madrid, Spain; M. Nyman, University of Lund Chemical Centre, Sweden; P. Aman and R. Andersson, Swedish University of Agricultural Sciences, Uppsala, Sweden; R. Amado and E. Arrigoni, Swiss Federal ` Institute of Technology, Zurich, Switzerland; M. Fischer, Nestle Research Center, Lausanne, Switzerland; J. ` Robertson, Institute of Food Research, Norwich, UK. The study was undertaken as part of the EU Concerted action PROFIBRE (Contract no. AIR3-CT94-2203). Financial assistance from the EU and support from National Government sources is gratefully acknowledged.

References
1 EASTWOOD, M. A. AND MITCHELL, W. D. Physical properties of "ber: a biological evaluation. In: SPILLER, G. A. AND AMEN, R. I. (Eds), Fibre in Human Nutrition, Plenum Press, pp. 109}129 (1976) 2 MONGEAU, R. AND BRASSARD, R. Insoluble dietary "ber from breakfast cereals and brans: bile salt binding and water-holding capacity in relation to particle size. Cereal Chemistry, 59, 413}417 (1982) 3 THIBAULT, J-F., LAHAYE, M. AND GUILLON, F. Physicochemical properties of food plant cell walls. In: SCHWEIZER, T. F. AND EDWARDS, C. A. (Eds), Dietary Fibre2a Component of Food. Nutritional Function in Health and Disease. ILSI Europe London: Springer-Verlag, pp. 21}39 (1992) 4 OAKENFULL, D. G. Physical properties of dietary "bre. In: SAMMAN, S. AND ANNISON, G. (Eds), Dietary Fibre and Beyond2an Australian Perspectives, Vol. 1. Nutritional Society of Australia, Perth, Australia: Nutrition Society of Australia Occassional Publications pp. 47}56 (1993) 5 CHO, S., DEVRIES, J. W. AND PROSKY, L. The physicochemical properties of dietary "ber. In: Dietary Fiber Analysis and Applications, Gaithersburg, MD: AOAC International, pp. 119}138 (1997a) 6 ROBERTSON, J. A. Physicochemical characteristics of food and the digestion of starch and "bre during gut transit. Proceedings of the Nutrition Society, 47, 143}152 (1988) 7 EASTWOOD, M. A. AND MORRIS, E. R. Physical properties of dietary "bre that in#uence physiological function: a model for polymers along the gastrointestinal tract. American Journal of Clinical Nutrition, 55, 436}442 (1992) 8 EASTWOOD, M. A. The physiological e!ect of dietary "ber: an update. Annual Review of Nutrition, 12, 19}35 (1992) 9 SOUTHGATE, D. A. T. Physical form and physiological function of dietary "bre. In: GUILLON, F., AMADO, R., COLLACO, M. T., ANDERSSON, H., ASP, N. G., BACH-KNUDSEN, K. E., CHAMP, M., MATHERS, J., ROBERTSON, J. A., ROWLAND, I. AND VAN LOO, I. European Commission, pp. 16}21 (1998) 10 AACC Method 88-04 In: Approved Methods of the American Association of Cereal Chemists, 9th Edn, St Paul, MN: Eagen Press (1995)

Conclusion This study on the hydration properties of "bre using substrates common to all participants and standardized methods has helped to highlight and resolve problems associated with achieving consistent experimental data on hydration properties. The outcome of the tests includes standardized and more user-friendly experimental protocols which can be recommended for general use. The tests have also highlighted the need to consider other properties of the "bre matrix, for example, matrix &solubility', when evaluating hydration properties. Also, through the use of substrates common to each participant and standardized methods, the tests have clari"ed the precision of experimental data which can be expected when measuring hydration properties.

Acknowledgements The authors would like to thank the participants for their maintained and enthusiastic collaboration developed during the course of the study. Collaborators were: U. Pechanek, Institute of Food Industry, Vienna, Austria; B. Wepner, ILMT, University for Agricultural Sciences, Vienna, Austria; P. Dysseler, Institut Meurice, CERIA, Free University of Brussels, Belgium; N. Canibe, National Institute of Plant and Animal Science, Tjele, Denmark; A.-M. Aura and K. Autio, VTT Biotechnology, Espoo, Finland; A.-C. LeFebvre, ADRIA, Quimper,

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11 CHO, S., DEVRIES, J. W. AND PROSKY, L. Analytical methods for measuring the physicochemical properties of dietary "ber. In: Dietary ,ber analysis and applications, Gaithersburg, MD: AOAC International, pp. 139}145 (1997b) 12 LEE, S. C., PROSKY, L. AND DEVRIES, J. W. Determination of total, soluble and insoluble dietary "bre in foods*Enzymatic-Gravimetric Method, Mes-Tris Bu!er: collaborative study. Journal of the Association of O.cial Analytical Chemists International, 75, 395}416 (1992) 13 GOONERATNE, J., MAJSAK-NEWMAN, G., ROBERTSON, J. A. AND SELVENDRAN, R. R. Investigation of factors that a!ect the solubility of dietary "ber, as non-starch polysaccharides, in seed tissues of mung bean ( <igna radiata) and black gram (<igna mungo). Journal of Agricultural and Food Chemistry, 42, 605}611 (1994) 14 ANFOR (Association Franiaise de Normalisation), NF X11-666, Analyse granulometrique des poudres, Methode par H H di!raction. Paris, 11 pp. (1984) 15 AFNOR (Association Franiaise de Normalisation), NF X11-620, Determination de la surface speci"que des solides par adsorption de gaz a l'aide de la methode BET. Paris, 16 ` H pp. (1994) 16 KUNIAK, L. AND MARCHESSAULT, R. H. Study of crosslinking reactions between epichlorohydrin and starch. Starch, 4, 110}116 (1972)

17 ROBERTSON, J. A. AND EASTWOOD, M. A. An investigation of the experimental conditions which could a!ect the waterholding capacity of dietary "bre. Journal of the Science of Food and Agriculture, 32, 819}825 (1981a) 18 BAUMANN, H. Apparatur nach Baumann zur Bestimmung der Flussigkeitsaufnahme von pulvrigen Substanzen. GlasK technick und Instrumententechnick Fachzeitschrift fuK r das aboratorium, 11, 540}542 (1967) 19 ARRIGONI, E., CAPREZ, A., NEUKOM, H. AND AMADO, R. Determination of water uptake by an automated method. ebensmittel-=issenschaft und-echnologie, 20, 263}264 (1987) 20 ROBERTSON, J. A. AND EASTWOOD, M. A. A method to measure the water-holding properties of dietary "bre using suction pressure. British Journal of Nutrition, 46, 247}255 (1981b) 21 GUILLON, F., AUFFRET, A., ROBERTSON, J. A., THIBAULT, J.-F. AND BARRY, J.-L. Relationship between physical characteristics of sugar beet "bre and its fermentability by human feacal #ora. Carbohydrate Polymers, 37, 185}197 (1998) 22 DAINTY, J. The water relations of plants. In: WILKINS, M. B. (Ed.), Physiology of Plant Growth and Development. London: McGraw-Hill, pp. 421}452 (1969)

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