Determination of Insoluble, Soluble, and Total Dietary Fiber (CODEX Definition) by Enzymatic-Gravimetric Method and Liquid Chromatography: Collaborative Study

2012 ◽  
Vol 95 (3) ◽  
pp. 824-844 ◽  
Author(s):  
Barry V McCleary ◽  
Jonathan W DeVries ◽  
Jeanne I Rader ◽  
Gerald Cohen ◽  
Leon Prosky ◽  
...  
Keyword(s):  
Dietary Fiber ◽  
Collaborative Study ◽  
Gravimetric Method ◽  
Water Soluble ◽  
Official Method ◽  
Soluble Dietary Fiber ◽  
Total Dietary Fiber ◽  
Food Ingredients ◽  
Aoac Official

Abstract A method for the determination of insoluble (IDF), soluble (SDF), and total dietary fiber (TDF), as defined by the CODEX Alimentarius, was validated in foods. Based upon the principles of AOAC Official MethodsSM 985.29, 991.43, 2001.03, and 2002.02, the method quantitates water-insoluble and water-soluble dietary fiber. This method extends the capabilities of the previously adopted AOAC Official Method 2009.01, Total Dietary Fiber in Foods, Enzymatic–Gravimetric– Liquid Chromatographic Method, applicable to plant material, foods, and food ingredients consistent with CODEX Definition 2009, including naturally occurring, isolated, modified, and synthetic polymers meeting that definition. The method was evaluated through an AOAC/AACC collaborative study. Twenty-two laboratories participated, with 19 laboratories returning valid assay data for 16 test portions (eight blind duplicates) consisting of samples with a range of traditional dietary fiber, resistant starch, and nondigestible oligosaccharides. The dietary fiber content of the eight test pairs ranged from 10.45 to 29.90%. Digestion of samples under the conditions of AOAC 2002.02 followed by the isolation, fractionation, and gravimetric procedures of AOAC 985.29 (and its extensions 991.42 and 993.19) and 991.43 results in quantitation of IDF and soluble dietary fiber that precipitates (SDFP). The filtrate from the quantitation of water–alcohol-insoluble dietary fiber is concentrated, deionized, concentrated again, and analyzed by LC to determine the SDF that remains soluble (SDFS), i.e., all dietary fiber polymers of degree of polymerization = 3 and higher, consisting primarily, but not exclusively, of oligosaccharides. SDF is calculated as the sum of SDFP and SDFS. TDF is calculated as the sum of IDF and SDF. The within-laboratory variability, repeatability SD (sr), for IDF ranged from 0.13 to 0.71, and the between-laboratory variability, reproducibility SD (sR), for IDF ranged from 0.42 to 2.24. The within-laboratory variability sr for SDF ranged from 0.28 to 1.03, and the between-laboratory variability sR for SDF ranged from 0.85 to 1.66. The within-laboratory variability sr for TDF ranged from 0.47 to 1.41, and the between-laboratory variability sR for TDF ranged from 0.95 to 3.14. This is comparable to other official and approved dietary fiber methods, and the method is recommended for adoption as Official First Action.

scholarly journals Determination of Total Dietary Fiber in Selected Foods Containing Resistant Maltodextrin by Enzymatic-Gravimetric Method and Liquid Chromatography: Collaborative Study

2002 ◽  
Vol 85 (2) ◽  
pp. 435-444 ◽  
Author(s):  
Dennis T Gordon ◽  
Kazuhiro Okuma ◽  
J W DeVries ◽  
K Fukuhara ◽  
W Jacob ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Dietary Fiber ◽  
Average Molecular Weight ◽  
Collaborative Study ◽  
Gravimetric Method ◽  
Soluble Dietary Fiber ◽  
Total Dietary Fiber ◽  
Resistant Maltodextrin ◽  
Standard Deviations

Abstract A method was developed for determination of total dietary fiber (TDF) in foods containing resistant maltodextrin (RMD) which includes nondigestible carbohydrates that are not fully recovered as dietary fiber by conventional TDF methods such as AOAC 985.29 or 991.43. Because the average molecular weight (MW) of RMD is 2000 daltons, lower MW soluble dietary fiber components do not precipitate in 78% ethanol; therefore, RMD is not completely quantitated as dietary fiber by current AOAC methods. The accuracy and precision of the method was evaluated through an AOAC collaborative study. Ten laboratories participated and assayed 12 test portions (6 blind duplicates) containing RMD. The 6 test pairs ranged from 1.5 to 100% RMD. The method consisted of the following steps: (1) The insoluble dietary fiber (IDF) and high MW soluble dietary fiber (HMWSDF) were determined by AOAC 985.29. (2) Ion exchange resins were used to remove salts and proteins contained in the AOAC 985.29 filtrates (including ethanol and acetone). (3) The amount of low MWRMD (LMWRMD) in the filtrates were determined by liquid chromatography. (4) The TDF was calculated by summation of the IDF, HMWSDF, and LMWRMD fractions having nondigestible carbohydrates with a degree of polymerization of 3 and higher. Repeatability standard deviations (RSDr) were 1.33–7.46%, calculated by including outliers, and 1.33–6.10%, calculated by not including outliers. Reproducibility standard deviations (RSDR) were 2.48–9.39%, calculated by including outliers, and 1.79–9.39%, calculated by not including outliers. This method is recommended for adoption as Official First Action.

scholarly journals Total Dietary Fiber (CODEX Definition) in Foods and Food Ingredients by a Rapid Enzymatic-Gravimetric Method and Liquid Chromatography: Collaborative Study, First Action 2017.16

2019 ◽  
Vol 102 (1) ◽  
pp. 196-207 ◽  
Author(s):  
Barry V McCleary ◽  
N Ames ◽  
J Cox ◽  
S Iilians ◽  
Y Jin ◽  
...  
Keyword(s):  
Dietary Fiber ◽  
Collaborative Study ◽  
Gravimetric Method ◽  
Soluble Dietary Fiber ◽  
Total Dietary Fiber ◽  
Plant Materials ◽  
Food Ingredients ◽  
Insoluble Dietary Fiber ◽  
The Past ◽  
Aoac Method

Abstract A method for measurement of total dietary fiber (TDF) has been validated. This method is applicable to plant materials, foods, and food ingredients as consumed, consistent with the 2009 CODEX definition (ALINORM 09/32/REP), and measures insoluble dietary fiber (IDF) and soluble dietary fiber (SDF), comprising SDF that precipitates in the presence of 78% ethanol (SDFP) and SDF that remains soluble in the presence of 78% ethanol (SDFS). The method is an update of AOAC Method 2009.01 and addresses each of the issues identified by analysts in using that method over the past 8 years. A total of 13 laboratories participated in the study, with all laboratories returning valid assay data for most of the 16 test portions (8 blind duplicates) consisting of samples with a range of content of traditional dietary fibers, resistant starch, and nondigestible oligosaccharides. The dietary fiber content of the eight test pairs ranged from 6.90 to 60.37 g/100 g. TDF was calculated as the sum of IDF plus SDFP measured gravimetrically and SDFS measured by HPLC. The repeatability SD ranged from 0.27 to 0.76 g/100 g, and the reproducibility SD ranged from 0.54 to 3.99 g/100 g. The RSDr ranged from 1.22 to 6.52%, and the RSDR ranged from 2.14 to 10.62%.

Determination of Soluble Dietary Fiber in Foods and Food Products: Collaborative Study

1994 ◽  
Vol 77 (3) ◽  
pp. 690-694 ◽  
Author(s):  
Leon Prosky ◽  
Nils-Georg Asp ◽  
Thomas F Schweizer ◽  
Jonathan W Devries ◽  
Ivan Furda ◽  
...  
Keyword(s):  
Dietary Fiber ◽  
Collaborative Study ◽  
Gravimetric Method ◽  
Food Products ◽  
Green Beans ◽  
Soluble Dietary Fiber ◽  
Total Dietary Fiber ◽  
Insoluble Dietary Fiber ◽  
Relative Standard

Abstract A collaborative study was conducted to determine the soluble dietary fiber (SDF) content of foods and food products by using a combination of enzymatic and gravimetric procedures. The method was basically the same as that employed for determining total dietary fiber (TDF), 985.29, and the method for insoluble dietary fiber (IDF), 991.42. Ten laboratories were each sent 13 test samples (6 blind duplicates and 1 standard [green beans] containing 29-33% TDF, 19-23% IDF, and 8-13% SDF) and were instructed to assay for IDF, SDF, and TDF independently. Included in the package were the 3 enzymes, namely alpha-amylase, amyloglucosidase, and protease, and the filter aid Celite, which was thought to be the major cause of high reproducibility relative standard deviation (RSDR) values for SDF obtained in a previous collaborative study. The foods to be analyzed were apricots, carrots, chickpeas, onions, raisins, and the sugar beet fiber Fibrex™. IDF, TDF, and SDF were calculated as the weight of residue minus the weight of protein and ash on a dry weight basis. RSDR values of the IDF results averaged 8.02%, with only 1 food having an RSDR >10%. The RSDR values for the TDF results averaged 4.97%, and all foods had an RSDR <7%. Although the RSDR values for SDF averaged 14.17%, 4 of the 6 foods had an RSDR <10%, and 1 of the 2 remaining foods that had a high RSDR had an SDF content of only 1.2%. In all cases, the RSDR values of the SDF content of the foods were less than the values for the same foods analyzed in a previous collaborative trial. The enzymatic-gravimetric method for the determination of SDF was adopted first action by AOAC INTERNATIONAL.

Determination of Total, Soluble, and Insoluble Dietary Fiber in Foods—Enzymatic-Gravimetric Method, MES-TRIS Buffer: Collaborative Study

1992 ◽  
Vol 75 (3) ◽  
pp. 395-416 ◽  
Author(s):  
Sungsoo C Lee ◽  
Leon Prosky ◽  
Jonathan W De Vries
Keyword(s):  
Dietary Fiber ◽  
Collaborative Study ◽  
Gravimetric Method ◽  
Tris Buffer ◽  
Total Dietary Fiber ◽  
Method Performance ◽  
Insoluble Dietary Fiber ◽  
Heat Stable ◽  
Assay Precision

Abstract A joint AOAC/AACC (American Association of Cereal Chemists) collaborative study of methods for the determination of soluble, insoluble, and total dietary fiber (SDF, IDF, and TDF) was conducted with 11 participating laboratories. The assay Is based on a modification of the AOAC TDF method 985.29 and the SDF/IDF method collaboratively studied recently by AOAC. The principles of the method are the same as those for the AOAC dietary fiber methods 985.29 and 991.42, Including the use of the same 3 enzymes (heat-stable α-amylase, protease, and amyloglucosldase) and similar enzyme Incubation conditions. In the modification, minor changes have been made to reduce analysis time and to Improve assay precision: (1) MES-TRIS buffer replaces phosphate buffer; (2) one pH adjustment step Is eliminated; and (3) total volumes of reaction mixture and filtration are reduced. Eleven collaborators were sent 20 analytical samples (4 cereal and grain products, 3 fruits, and 3 vegetables) for duplicate blind analysis. The SDF, IDF, and TDF content of the foods tested ranged from 0.53 to 7.17, 0.59 to 60.53, and 1.12 to 67.56 g/100 g, respectively. The respective average RSDR values for SDF, IDF, and TDF determinations by direct measurements were 13.1, 5.2, and 4.5%. The TDF values calculated by summing SDF and IDF were in excellent agreement with the TDF values measured independently. The modification did not alter the method performance with regard to mean dietary fiber values, yet It generated lower assay variability compared with the unmodified methods. The method for SDF, IDF, and TDF (by summing SDF and IDF) has been adopted first action by AOAC International.

scholarly journals Determination of Total Dietary Fiber in Selected Foods Containing Resistant Maltodextrin by a Simplified Enzymatic-Gravimetric Method and Liquid Chromatography: Interlaboratory Study in China

2008 ◽  
Vol 91 (3) ◽  
pp. 614-621 ◽  
Author(s):  
Boqiang Fu ◽  
Jing Wang ◽  
Jean Michel Roturier ◽  
Zhiyu Tang ◽  
Huan Li ◽  
...  
Keyword(s):  
Dietary Fiber ◽  
Interlaboratory Study ◽  
National Standard ◽  
Official Method ◽  
Total Dietary Fiber ◽  
Modified Method ◽  
Resistant Maltodextrin ◽  
Aoac Official ◽  
Aoac Official Method

Abstract An interlaboratory study was conducted in China to validate the modified AOAC Official Method 2001.03 for the determination of total dietary fiber (TDF) in foods containing resistant maltodextrin (RMD), which will be adopted as the National Standard Method of China. The kind of buffer solution, the volume of filtrate evaporation, the volume of eluent for desalting and residual solution after evaporation, etc. were modified, which had been proved to have acceptable accuracy and precision in the routine assay. TDF contents in 3 representative foods and 2 kinds of RMD ingredient (i.e., NUTRIOSE 06 and NUTRIOSE 10) were measured using the modified method in 6 eligible laboratories representing commercial, industrial, and governmental laboratories in China. The results of the interlaboratory study indicated that the intralaboratory repeatability, interlaboratory reproducibility, and precision of the modified method are adequate for reliable analysis of TDF in food containing RMD, as well as resistant dextrin. Compared to AOAC Official Method 2001.03, the modified method is time- and cost-saving.

scholarly journals Determination of Total Dietary Fiber (CODEX Definition) by Enzymatic-Gravimetric Method and Liquid Chromatography: Collaborative Study

2010 ◽  
Vol 93 (1) ◽  
pp. 221-233 ◽  
Author(s):  
Barry V McCleary ◽  
Jonathan W De Vries ◽  
Jeanne I Rader ◽  
Gerald Cohen ◽  
Leon Prosky ◽  
...  
Keyword(s):  
Molecular Weight ◽  
Dietary Fiber ◽  
Resistant Starch ◽  
Collaborative Study ◽  
Gravimetric Method ◽  
Low Molecular Weight ◽  
Total Dietary Fiber ◽  
Aoac Method ◽  
Standard Deviations

Abstract A method for the determination of total dietary fiber (TDF), as defined by the CODEX Alimentarius, was validated in foods. Based upon the principles of AOAC Official MethodsSM 985.29, 991.43, 2001.03, and 2002.02, the method quantitates high- and low-molecular-weight dietary fiber (HMWDF and LMWDF, respectively). In 2007, McCleary described a method of extended enzymatic digestion at 37C to simulate human intestinal digestion followed by gravimetric isolation and quantitation of HMWDF and the use of LC to quantitate low-molecular-weight soluble dietary fiber (LMWSDF). The method thus quantitates the complete range of dietary fiber components from resistant starch (by utilizing the digestion conditions of AOAC Method 2002.02) to digestion resistant oligosaccharides (by incorporating the deionization and LC procedures of AOAC Method 2001.03). The method was evaluated through an AOAC collaborative study. Eighteen laboratories participated with 16 laboratories returning valid assay data for 16 test portions (eight blind duplicates) consisting of samples with a range of traditional dietary fiber, resistant starch, and nondigestible oligosaccharides. The dietary fiber content of the eight test pairs ranged from 11.57 to 47.83. Digestion of samples under the conditions of AOAC Method 2002.02 followed by the isolation and gravimetric procedures of AOAC Methods 985.29 and 991.43 results in quantitation of HMWDF. The filtrate from the quantitation of HMWDF is concentrated, deionized, concentrated again, and analyzed by LC to determine the LMWSDF, i.e., all nondigestible oligosaccharides of degree of polymerization 3. TDF is calculated as the sum of HMWDF and LMWSDF. Repeatability standard deviations (sr) ranged from 0.41 to 1.43, and reproducibility standard deviations (sR) ranged from 1.18 to 5.44. These results are comparable to other official dietary fiber methods, and the method is recommended for adoption as Official First Action.

Determination of Total Dietary Fiber in Foods and Products with Little or No Starch, Nonenzymatic-Gravimetric Method: Collaborative Study

1994 ◽  
Vol 77 (3) ◽  
pp. 687-689 ◽  
Author(s):  
Betty W Li ◽  
Maria S Cardozo
Keyword(s):  
Standard Deviation ◽  
Dietary Fiber ◽  
Fruits And Vegetables ◽  
Simple Procedure ◽  
Collaborative Study ◽  
Gravimetric Method ◽  
Total Dietary Fiber ◽  
Freeze Dried ◽  
Relative Standard

Abstract A collaborative study was conducted to validate a nonenzymatic-gravimetric method for the determination of total dietary fiber (TDF) of samples containing little or no starch such as most fruits, and vegetables and many purified polysaccharides. This simple procedure involves suspension of freeze-dried, ground samples in deionized water and incubation at 37°C for 90 min, followed by pre-cipitation with 4 volumes of 95% ethanol. The weight of the dilute alcohol-insoluble residues after correcting for crude protein and ash corresponds to the TDF content of the sample. Six samples in blind duplicate (apples, apricots, cabbage, carrots, onions, and soy fiber) were sent with Celite to 10 laboratories. The reproducibility relative standard deviation (RSDr) of the TDF values for 9 laboratories ranged from 2.92 to 6.25%. The repeatability standard deviation (RSDr) for the 9 laboratories ranged from 1.50 to 2.70%. The method has been adopted first action by AOAC INTERNATIONAL.

Determination of Insoluble and Soluble Dietary Fiber in Foods and Food Products: Collaborative Study

1992 ◽  
Vol 75 (2) ◽  
pp. 360-367 ◽  
Author(s):  
Leon Prosky ◽  
Nils-Georg Asp ◽  
Thomas F Schweizer ◽  
Jonathan W Devries ◽  
Ivan Furda
Keyword(s):  
Dietary Fiber ◽  
Collaborative Study ◽  
Dry Weight ◽  
Food Products ◽  
Soluble Dietary Fiber ◽  
Total Dietary Fiber ◽  
Brussels Sprouts ◽  
Insoluble Dietary Fiber ◽  
Relative Standard

Abstract A collaborative study was conducted to validate a method to determine the Insoluble dietary fiber (IDF) and soluble dietary fiber (SDF) contents of foods and food products by using a combination of enzymatic and gravimetric procedures. The method was basically the same as that for determining total dietary fiber, which was adopted as final action by AOAC and further modified to Include changes in the concentration of buffer and base and substitution of hydrochloric acid for phosphoric acid. Thirty-nine collaborators were each sent 7 test samples In a staggered design for duplicate blind analysis. They were also sent a standard containing 4.3-5.4% IDF and 1.5-2.7% SDF. The 22 foods that were analyzed for IDF and SDF were cabbage, carrots, French beans, kidney beans, butter beans, okra, onions, parsley, chick peas, brussels sprouts, barley, rye flour, turnips, soy bran, wheat germ, raisins, Callmyrna figs, prune powder, Black Mission figs, apple powder, peach powder, and apricot powder. Both IDF and SDF values were calculated as the weight of residue minus the weight of protein and ash reported on a dry weight basis. The reproducibility relative standard deviation (RSDR) of the IDF results ranged from 3.68 to 19.44% for the foods analyzed; almost half the test samples had an RSDR <10%. The RSDR values for the SDF results were somewhat higher. Approximately 50% of the foods analyzed had an RSDR >20%, and 45% had an RSDR between 10 and 20%. An RSDR approaching 45% was calculated for the 2 test samples with the lowest SDF content, 1.35 and 1.90%. Raisins and prune powder had high RSDR values for both SDF and IDF. A major reason for high RSDR values seems to be filtration problems, which are avoidable by analyzing 0.5-0.25 g test samples. The method for the determination of SDF requires further study, but the method for the determination of IDF was adopted first action by AOAC International.

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