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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 GeH raudière, BP 71627, 44316 Nantes-03 (France)
R. Amadò: 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.
Keywords: dietary "bre; resistant starch; hydration methods; swelling; water retention
72
lwt/vol. 33 (2000) No. 2
Table 1 Characterization of substrates used for the ring tests on hydration properties
Property Pea hull Apple pulp Citrus pulp Novelose Eridania
incorporate modi"cations to make the methods more Food, Cergy Pontoise, France) was substituted for citrus
user-friendly. Measurements of water absorption in rela- pulp as an untested substrate.
tion to porosity were also made to relate swelling, WRC
and absorption to matrix structure.
Methods
Dietary ,bre analysis. Samples were analysed in tripli-
Materials and Methods cate for "bre content using an enzymatic}gravimetric
method (12).
Participating laboratories
Participation in the study was open to all members of Alcohol insoluble residues (AIR). These were prepared to
Pro"bre and outside interest was also encouraged. Par- characterize the relative contribution of polymeric ma-
ticipants were mainly members of the processing and terial from each test substrate. Samples (1 g dry weight)
physicochemistry group of Pro"bre and most undertook were extracted (]3) in boiling ethanol (30 mL; 5 min;
and completed the measurement of swelling and WRC. 80}85% v/v). Alcohol-insoluble material from each ex-
Measurements of water absorption and porosity was traction step was recovered by "ltration. Ethanolic
limited to participants with previous experience using the supernatants were discarded and the ethanol insoluble
methods involved. material was dried by solvent exchange, through abso-
lute ethanol (]2) and acetone (]2), to yield a dry white
powder.
Study protocol
The test substrates, chosen to cover a range of di!erent Solubility. Alcohol insoluble residues samples (300 mg)
"bre types, were characterized by a range of physical were suspended in distilled water (30 mL) and stirred for
properties which may be related to hydration properties, 3 h at room temperature (13). Each suspension was cen-
e.g. particle size (Table 1). Substrates were distributed to trifuged (3000]g), the supernatant discarded and the
participants with copies of the standardized experimental pellet washed (]2) in distilled water. Pellets were freeze
protocol(s) for swelling and water retention and schedule dried and water insoluble AIR determined from loss in
for the standardized reporting of results. Experimental sample weight during extraction.
protocols for each stage of the test were constructed,
based on published methods, to limit the number of Particle size. Median particle size was determined from
experimental variables in each protocol before proceed- particle size distributions generated using laser light
ing with the tests. di!raction (Malvern Mastersizer IP, MS15 for hydra-
Raw data were collected on dry weight and weights ted samples and PS65 for dry samples). Distributions
recorded at di!erent stages during each procedure. Data were made in triplicate for each sample, using 10}20 g
were screened for compliance with the experimental pro- sample weight for dry particle size distribution and 1}2 g
tocol and consistency between participants. Inconsisten- in an aqueous suspension for hydrated particle size
cies were checked through examination of raw data and, distribution (14).
if necessary, contact with the participant. All experi-
mental data complying with the set procedures were Surface area. Surface area was determined from nitrogen
included for analysis. adsorption isotherms, using a Micromeritics, Gemini III
The substrates used were commercial preparations. Dur- 2375 and Vacprep 061 LB system. Samples were de-
ing stage one, substrates were: pea hull (ID Food, Cergy gassed for 48 h, to a residual system pressure between 0.2
Pontoise, France); citrus pulp (Indulerida SA, Alguaire, and 0.5 KPa, prior to generating a Brunauer}Emmet}
Lleida, Spain); Novelose (National Starch and Chemical Teuer BET isotherm using nitrogen at 773 K (15).
Co., Neustadt, Germany); and Eridania (Eridania, Be-
ghin-Say, Vilvoorde, Belgium). For stage two, pea hull Swelling. The protocol, derived from the method of
and Eridania starch were retested and apple pulp (ID Kuniak and Marchessault (16), is outlined in Fig. 1. Test
73
lwt/vol. 33 (2000) No. 2
74
lwt/vol. 33 (2000) No. 2
known osmotic potential. Solutions of PEG were pre- for: pea hull, 67%; apple pulp, 41%; and citrus pulp, 17%
pared to cover an osmotic pressure range from of the sample. It is important to recognize the presence of
0}0.7 MPa. After equilibration the fresh weight of sample &water-soluble' material and its apparent concentration
recovered from the dialysis sacs was recorded, samples in samples if &absolute' values are required for hydration
were dried and the dry weight was used to determine properties, especially when calculation is based on the
water absorbed at each suction pressure. Pore size was original rather than the recovered sample weight, e.g.
estimated from suction pressure and surface tension swelling. In this study, testing methods of measurement
measurements (6, 21). was the major objective and these were evaluated in
conjunction with a spectrum of properties to more fully
characterize each "bre source.
Data analysis Particle size distribution (Table 1) showed median par-
The BCR HOSTAN3 Statistical Package, as used for the ticle size varied between substrates and that the particles
purposes of method certi"cation by the EU, was used for swelled when hydrated. Similarly, based on total sample
analysis of data for swelling and water retention. weight, there was an apparent ninefold range in surface
area of the substrates, from 180 m2/kg for citrus pulp to
1620 m2/kg for pea hull.
Results and Discussion
Substrate characterization Hydration properties
Substrates each had a low moisture content (Table 1) and The experimental data for the study on swelling and
there was good consistency between participants in re- WRC is summarized in Tables 2 and 3. Most participants
ported dry weights. Fibre analysis con"rmed substrates had some previous experience of measuring hydration
were typical "bre &concentrates', with apple pulp and properties and the relative precision of data submitted by
citrus pulp apparently rich in pectic polysacharides and laboratories with previous, little or no experience was
pea hull rich in cellulose, xylan and pectic polysacchar- similar. Data provided from laboratory speci"c methods
ide. Preparation of AIR distinguished the relative contri- (not shown) were also similar to data provided for the
bution of low molecular weight (ethanol soluble), water standard protocols. This gave reassurance that the
extractable and water-insoluble matrix material in each standard protocols were user-friendly and had not intro-
substrate, as supplied rather than after isolation of duced unforseen changes in the substrate response due to
nonstarch polysaccharides. The extractability of each experimental treatment.
sample can a!ect interpretation of results for hydration
properties. For example, the AACC method (10) was Swelling. The range of values for swelling (Table 2) was
developed for measuring total water retained by less than anticipated, due mainly to the low values for
a sample, with care taken to retain soluble material, citrus pulp and apple. Values were expected to be greater
whereas the current methods for WRC and swelling than 20 mL/g, considered typical for a fruit or vegetable
measure the (packed) matrix bulking potential. The resis- "bre concentrate (3). Di!erences could partly be at-
tant starches, Novelose and Eridania, were e!ectively free tributed to the presence of water soluble material, but
of alcohol soluble material and contained only negligible e!ects of processing and consequent matrix structure
water-extractable material. Pea hull was also rich in AIR, breakdown were probably more important. This also
most of which were water-insoluble. Apple pulp and emphasizes the need to consider processing history when
especially citrus pulp contained appreciable amounts of selecting "bre sources for diet therapy and in the inter-
alcohol soluble material and the water insoluble matrix pretation of health response. The statistical analysis
accounted for around 60% of the apple pulp but only showed data were normally distributed but that the vari-
around 40% of the citrus pulp. In comparison, the water ance between laboratories (S ) was higher than within
"
insoluble matrix recovered after "bre analysis accounted laboratory (S ; Table 2). Agreement within laboratory
8
Number of sets 19 13 14 19 19 16 11
Number of replicates 171 117 126 171 171 144 99
Overall mean (x6 ) 7.48 6.64 7.42 10.45 5.65 7.96 7.43
s individual values 0.77 0.79 1.15 1.21 0.86 0.67 1.05
9
s within lab. S 0.56 0.37 0.33 0.70 0.56 0.61 0.34
9 8
CV (%) 7.5 5.6 4.4 6.7 9.9 7.7 4.6
s between lab S 0.75 0.84 1.00 1.19 0.84 0.64 0.96
9 "
CV (%) 10.1 12.7 13.5 11.3 14.9 8.0 12.9
95% con"dence interval of x6 0.37 0.41 0.62 0.58 0.42 0.36 0.55
75
lwt/vol. 33 (2000) No. 2
Number of sets 16 13 13 17 17 13 11
Number of replicates 144 117 117 153 153 117 99
Overall mean (x6 ) 3.94 3.82 5.43 10.66 2.95 3.49 3.14
s individual values 0.46 0.40 1.18 2.34 0.47 0.73 0.26
9
s within lab. S 0.36 0.16 0.27 0.70 0.13 0.43 0.17
9 8
CV (%) 9.1 4.2 5.0 6.6 4.4 12.4 5.4
s between lab S 0.44 0.36 1.11 2.33 0.47 0.72 0.23
9 "
CV (%) 11.2 9.4 20.4 21.9 15.9 20.6 7.3
95% con"dence interval of x6 0.28 0.25 0.67 1.09 0.24 0.44 0.17
76
lwt/vol. 33 (2000) No. 2
Fig. 4 Water absorption measured using a Baumann apparatus. Values shown with error bars ($s ) are included to illustrate the
9
range of variation expected from the method. Inset shows the maintenance of equilibrium full absorption. s, pea; d, citrus; h,
Novelose
Fig. 5a Water absorption measured using suction pressure. Fig. 5b Estimation of pore size and pore volume in hydrated
Values were obtained through equilibrium dialysis against samples. Values were calculated from water absorbed against
polyethylene glycol (MW 10,000) solutions of known osmotic a known suction pressure (Fig. 5a) as the pore volume and with
potential. s, pea; d, citrus; h, Novelose pore radius r estimated from suction pressure (P) and surface
tension measurement (s) as r"2s/P (21). s, pea; d, citrus; h,
Novelose
therefore important for WRC measurement and it is
recommended that account is taken of &soluble' material of water absorption, after 30 min, for resistant starch and
in the pellet when calculating WRC if absolute values for pea was similar to the WRC measured, but for citrus
WRC are required. WRC was much greater than water absorption. This may
be related to di!erences in composition, particle and pore
Absorption and porosity. Rate of water absorption mea- size of the samples.
sured using a Baumann apparatus was relatively rapid Unlike the Baumann apparatus, when rate of absorption
for each substrate (Fig. 4). The resistant starch was ap- or wettability of a dry sample (19) is measured, suction
parently fully absorbed within 1 min. Pea and citrus were pressure is used to measure absorption or desorption of
extensively absorbed after 2 min, but absorption con- a hydrated sample at speci"ed suction pressures. As
tinued, albeit at a low rate, even after 30 min. The extent shown in Fig. 5a, at relatively low suction pressure water
77
lwt/vol. 33 (2000) No. 2
absorption by citrus pulp was high but only a slight France; C. Renard, F. Guillon, INRA, Nantes, France;
increase in suction pressure was required to reduce the G. Abraham, LMTA, UniversiteH de la Rochelle, France;
absorption capacity. The absorption capacity of resistant G. Dongowski, DIFE, Bergholz-RehbruK cke, Germany;
starch and pea hull was much lower than for citrus pulp. C. Niemann, IFLT, Technische UniversitaK t, Berlin,
With resistant starch and pea the contribution of water- Germany; U. Schlemmer, BFE, Karlsruhe, Germany; T.
soluble material to absorption pressure would be low. Sheehy, University College Cork, Ireland; D. Armstrong,
Absorption against a suction pressure will mainly depend H. Luyten and C. T. Ponne, ATO-DLO, Wageningen,
on the matrix potential of these samples (20, 22) and will The Netherlands; H. A. Schols, WAU, Wageningen, The
also apply to measurements made using the Baumann Netherlands; M. T. Amaral-Collaco, INETI, Lisbon,
apparatus (19). With citrus pulp the relatively high water- Portugal; F.-D. Saura-Calixto and L. Bravo, Instituto del
soluble component can generate a solute potential and Frio (CSIC), Madrid, Spain; M. Nyman, University of
contribute to the high absorption observed using suction Lund Chemical Centre, Sweden; P. Aman and R. Ander-
pressure. At higher suction pressures the extent of water sson, Swedish University of Agricultural Sciences, Up-
absorption becomes similar for all samples and similar to psala, Sweden; R. Amadò and E. Arrigoni, Swiss Federal
absorption measured using the Baumann apparatus. Institute of Technology, Zurich, Switzerland; M. Fischer,
This suggests that water absorption measured using the Nestlè Research Center, Lausanne, Switzerland; J.
Baumann apparatus mainly measures the pore volume of Robertson, Institute of Food Research, Norwich, UK.
the microcapillaries ((1 km) (21). Using a range of suc- The study was undertaken as part of the EU Concerted
tion pressures to measure pore volumes, the relative action PROFIBRE (Contract no. AIR3-CT94-2203).
contribution of micropores ((1 km) and macropores Financial assistance from the EU and support from
('1 km) to the water associated with the "bre matrix National Government sources is gratefully acknow-
and its relationship to swelling volume and WRC can be ledged.
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 References
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