Total Dietary Fiber Determined as Neutral Sugar Residues, Uronic Acid Residues, and Klason Lignin (The Uppsala Method): Collaborative Study

1995 ◽  
Vol 78 (4) ◽  
pp. 1030-1044 ◽  
Author(s):  
Olof Theander ◽  
Per Åman ◽  
Eric Westerlund ◽  
Roger Andersson ◽  
Dan Pettersson
Keyword(s):  
Dietary Fiber ◽  
Uronic Acid ◽  
Free Acid ◽  
Collaborative Study ◽  
Gravimetric Method ◽  
Insoluble Residue ◽  
Gas Liquid Chromatography ◽  
Neutral Sugar ◽  
Klason Lignin ◽  
Total Dietary Fiber

Abstract A joint AOAC/American Association of Cereal Chemists (AACC) collaborative study was conducted to determine by the Uppsala method the dietary fiber content and its composition in various foods. The method includes preparation of a residue by treatment with thermostable α-amylase and amyloglucosidase and then ethanol precipitation of solubilized dietary fiber components while leaving low-molecular weight carbohydrates in solution. After acid hydrolysis of residue, neutral polysaccharide residues are determined as alditol acetates by gas-liquid chromatography, uronic acid residues are determined by colorimetry, and ash-free acid-insoluble residue (Klason lignin) is determined gravimetrically. Total dietary fiber, including enzyme-resistant starch, is calculated as the sum of nonstarch polysaccharide residues and Klason lignin. Nine laboratories completed the study, analyzing in duplicate 8 unknown dried products that included 4 cereal products, green peas, potato fiber, carrots, and apples. Total dietary fiber contents of products tested ranged from 4.6 to 84.3%, with an average RSDR value of 8.4% (range, 4.8–11.1%). Total neutral polysaccharide residues ranged from 3.8 to 64.1%, with an average RSDR value of 7.5% (range, 5.4–10.5%). Individual neutral sugars (rhamnose, arabinose, xylose, mannose, galactose, and glucose) and uronic acid residues present at more than 1% generally had good RSDR values (3.3– 22.8%), whereas, as expected for Klason lignin, only the wheat bran sample with a high content (16%) had an excellent RSDR value (5.0%). The gas chromatographic-colorimetric-gravimetric method (Uppsala method) for determination of total dietary fiber (as neutral sugar residues, uronic acid residues, and Klason lignin) has been 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 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 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.

Enzymatic-Gravimetric Determination in Foods of Dietary Fiber as Sum of Insoluble and Soluble Fiber Fractions: Summary of Collaborative Study

1993 ◽  
Vol 76 (4) ◽  
pp. 923-925 ◽  
Author(s):  
Roger Mongeau ◽  
Rene Brassard
Keyword(s):  
Dietary Fiber ◽  
Collaborative Study ◽  
Gravimetric Method ◽  
Wheat Bread ◽  
Soluble Fiber ◽  
Total Dietary Fiber ◽  
Whole Wheat ◽  
Whole Wheat Bread ◽  
Relative Standard ◽  
Fiber Fractions

Abstract A collaborative study was conducted on an enzymatic- gravimetric method for determination of total dietary fiber in foods, in which soluble fiber and insoluble fiber are determined separately. Ten collaborators analyzed blind duplicate test samples from 5 food products: turnip, wheat bran, beans canned with tomato sauce, rice, and whole wheat bread. Repeatability and reproducibility relative standard deviations ranged from 1.48 to 14.73% and from 4.13 to 17.94%, respectively. The method was adopted first action by AOAC International.

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 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 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.

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