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History of Dietary Fiber Measurement

Fiber Measurement


Early days

The history of dietary fiber dates back to ancient Greece where it was known that bran cereals helped to prevent constipation. In the 1930s, J.H. Kellogg confirmed the positive effects of wheat bran on patients suffering with colitis and constipation but it was not until 1953 that Dr. Eben Hipsley coined the phrase “dietary fiber” in an article on pregnancy toxaemia.1

Throughout the 1970s, British researchers, Denis Burkitt and Hugh Trowell, became leaders in the field proposing the “dietary fiber hypothesis” and the concept of “Western diseases”. Having spent a significant time studying populations in sub-Saharan Africa, they reached the conclusion that the lack of unprocessed, high fiber foods in typical Western diets led to a higher incidence of certain conditions including heart disease and colorectal cancer.2,3,4
Hugh Trowell is credited with the first acceptable definition of dietary fiber.5,6

Dietary fiber consists of the remnant of edible plant cells polysacharides lignin and associated substances resistant to digestion by the alimentary enzymes of humans


Following on from this a number of research groups began to focus on improving the methodology available for the measurement of dietary fiber content; Southgate,7 Theander,8 Schweizer,9 Furda,10 Heckman,11 Baker,12 and Asp13 being the major contributors at this time. Their goal was to develop a method of analysis that could be used to quantify dietary fiber as defined by Trowell.

By 1985, Leon Prosky had successfully led a collaborative effort to reach consensus within the scientific community on dietary fiber methodology. This was accomplished through an interlaboratory study that resulted in the acceptance of AOAC 985.29 / AACC 32.05 as the reference method for the analysis of dietary fiber. 14,15 This method was widely welcomed by the food science community, servingDietary fiber assay kit as a reliable, reproducible analytical tool for the food and beverage industries. A series of related methods for the measurement of dietary fiber followed and were also approved by AOAC. The most useful of these was a simple extension of the Prosky method which allowed the measurement of soluble and insoluble dietary fiber separately (Lee method – AOAC 991.43).16

Scientific surveys in the early 1990s began to highlight a deficiency in the definition of dietary fiber.17,18 A growing body of evidence existed for the inclusion of resistant starch and non-digestible oligosaccharides in total dietary fiber because these food ingredients exhibited many of the health benefits claimed for dietary fiber. These components were not measured by the “gold standard” Prosky method (AOAC 985.29) or its soluble/insoluble extension – AOAC 991.43. The analytical community responded to this challenge by developing both entirely new methods and extensions to existing methods. For example, dietary fiber including non-digestible oligosaccharides could be measured using the Matsutani method (AOAC 2001.03)19 but the quantification of resistant starch posed a more serious problem.

Resistant Starch as a basis for the MCCleary Integrated Total Dietary Fiber method (AOAC 2009.01)

The Prosky method (AOAC 985.29) could never be used for the measurement ofMegazyme supply an enzyme assay kit , Catalogue Number K-RSTAR for the measurement of resistant starch according to AOAC 2002.02. resistant starch because the harsh incubation conditions (100ºC, pH 8.2) during enzymatic hydrolysis ensured that the starch content in the sample was completely gelatinised removing any ‘resistant’ component. Throughout the 1980s a number of research groups (Champ,20 Berry,21 Cummings,22 and Muir and O’Dea23) turned their attention to a method for the measurement of resistant starch and sought to develop a method using pseudo-physiological incubation conditions for the required enzymatic digestion step.  McCleary et al.24 ultimately developed a method employing pancreatic α-amylase in place of bacterial α-amylase at pH 6, 37ºC, which could successfully be used to reproducibly measure resistant starch. This was the only resistant starch method that survived the thoroughness of an interlaboratory evaluation and was accepted by AOAC as an official method (AOAC 2002.02).25

MegazymeFollowing intensive research, it was shown that the incubation step developed for the resistant starch method (with very minor modifications) was also suitable for the measurement of HMWDF. The mild, physiologically relevant, conditions employed ensured that the starch present in a sample was not gelatinised and could be accurately measured as a component in dietary fiber. The precipitation step for the isolation of HMWDF was used as in AOAC 985.29 to maintain the previous molecular weight cut-off and the HPLC analysis of the filtrate following this precipitation was performed as described in the Matsutani method (AOAC 2001.03) to guarantee correct measurement of non-digestible oligosaccharides.Megazyme supply an enzyme assay kit , Catalogue Number K-INTDF for the measurement of dietary fiber according to AOAC 2009.01, AOAC 2011.25. The amalgamation of all of these features resulted in the McCleary method26 for Integrated Total Dietary Fiber (AOAC 2009.01)27 and its soluble/insoluble method extension (AOAC 2011.25).28

The McCleary method is now the only method that correctly measures all components of dietary fiber as defined by CODEX Alimentarius.

CODEX Alimentarius definition of dietary fiber:   
  Dietary fibre denotes carbohydrate polymers with 10 or more monomeric units, which are not hydrolysed by the endogenous enzymes in the small intestine of humans and belong to the following categories: Edible carbohydrate polymers naturally occurring in the food consumed. Carbohydrate polymers, which have been obtained from food raw material by physical, enzymatic or chemical means and which have been shown to have a physiological benefit to health, as demonstrated by generally accepted scientific evidence to competent authorities. Synthetic carbohydrate polymers that have been shown to have a physiological benefit to health, as demonstrated by generally accepted scientific evidence to competent authorities. NOTES: (1) Includes also lignin and other compounds if quantified by AOAC 991.43. (2) Decision on whether to include carbohydrates with a degree of polymerization from DP 3 to 9 should be left to national authorities.


1Hiplsley, E. H. (1953) Dietary “Fibre” and Pregnancy Toxaemia Br. Med. J. 2(4833), 420–422. Link to article

2Trowell, H. (1972) Crude fibre, dietary fibre, and artheroschlerosis. Atheroscler. 16(1), 138-140. Link to article

3Trowell, H. (1972) Ischemic heart disease and dietary fibre. Am. J. Clin. Nutr. 25(9), 926-932. Link to article

4Burkitt, D. P., Walker, A. R. P., and Painter, N. S. (1972) Effect of dietary fibre on stools and transit times and its role in the causation of disease. Lancet 300(7792), 1408–1411. Link to article

5Trowell, H. C. (1974) Definition of dietary fibre. Lancet 303(7856), 503. Link to article

6Trowell, H. C., Southgate, D. A. T., Wolever, T. M. S., Leeds, A. R., Gassull, M. A., and Jenkins, D. J. (
1976) A. Dietary fiber redefined. Lancet 307(7966), 967. Link to article

7Southgate, D. A. T. (1977) The definition and analysis of dietary fibre. Nutr. Rev. 35(3), 31-37. Link to article

8Theander, O., and Aman, P. (1979) Studies on dietary fibres. I. Analysis and chemical characterization of water-soluble and water-insoluble dietary fibres. Swedish J. Agric. Research 9(3), 97. Link to journal homepage

9Schweizer, T. F., and Wursch, P. (1979) Analysis of dietary fiber. J. Sci. Food Agric. (30)6, 613-619. Link to article

10Furda, I. Simultaneous analysis of soluble and insoluble dietary fiber. In: The Analysis of Fiber in Foods. W. P. T. James and O. Theander, Eds. Marcel Dekker, New York, NY, 1981 Link to book

11Heckman, M.M., and Lane, S.A. (1981) Comparison of dietary fiber methods for food. J. AOAC Int.(64)6,1339-1343. Link to article

12Baker, D. Notes on the neutral detergent fibre method. In: The Analysis of Dietary Fiber in Food. W. P. T. James and O. Theander, Eds. Marcel Dekker, New York, NY, 1981Link to book

13Asp, N-G., Johansson, C-G., Hallmer, H., and Siljestrom, M. (1983) Rapid enzymatic assay of insoluble, and soluble dietary fiber. J. Agric. Food Chem. (31)3, 476-482. Link to article

14Prosky, L., Asp, N-G., Furda, I., DeVries, J. W., Schweizer, T. F., and Harland, B. F. (1985) Determination of total dietary fiber in foods and food products: Collaborative study. J. AOAC Chem.68(4), 677-679. Link to article

15AOAC Official Method 985.29, Total Dietary in Foods—Enzymatic-Gravimetric Method. Official Methods of Analysis, 16th ed. AOAC International, Gaithersburg, MD, 1995Link to book

16AOAC Method 991.43, Total, Insoluble and Soluble Dietary Fiber in Food—Enzymatic-Gravimetric Method, MES-TRIS Buffer. Official Methods of Analysis, 16th ed. AOAC International, Gaithersburg, MD,1995Link to book

17Lee, S. C., and Prosky, L. (1995) International survey on dietary fiber definition, analysis, and reference materials. J. AOAC Int. (78)1, 22-36. Link to article

18Cho, S. S., and Prosky, L. Summary of AOAC survey on complex carbohydrates/dietary fiber. In: Complex Carbohydrates/Dietary Fiber, S. S. Cho, L. Prosky, and M. Dreher, Eds. Marcel Dekker, New York, NY, 1999Link to book

19Gordon D. T., Okuma K. (2002) Determination of Total Dietary Fiber in Selected Foods Containing Resistant Maltodextrin by Enzymatic-Gravimetric Method and Liquid Chromatography: Collaborative Study. J. AOAC Int. (85)2, 435–444. Link to article

20ChampM. (1992)  Determination of resistant starch in foods and food products: interlaboratory study. EurJ. Clin. Nutr. 46(Suppl.2), S51-S62

21Berry, C. S. (1986) Resistant starch: Formation and measurement of starch that survives exhaustive digestion with amylolytic enzymes during the determination of dietary fibre. J.Cereal Sci(4)4 , 301-314. Link to article

22Englyst, H., Wiggins, H.S., and Cummings, J.H. (1982) Determination of the non-starch polysaccharides in plant foods by gas-liquid chromatography of constituent sugars as alditol acetatesAnalyst107, 307-318. Link to article

23Muir, J. G, O'Dea K. (1992) Measurement of resistant starch: factors affecting the amount of starch escaping digestion in vitro. AmJClinNutr56123-127 Link to article

24McCleary, B. V., Monaghan, D.  (2002) Measurement of resistant starch J AOAC Int. 85(3), 665-75. Link to article

25McCleary, B. V., McNally, M., Rossiter, P. (2002) Measurement of resistant starch by enzymatic digestion in starch and selected plant materials: Collaborative study. J. AOAC Int. 85, 1103–1111. Link to article

26McCleary, B. V. (2007) An integrated procedure for the measurement of total dietary fibre (including resistant starch), non-digestible oligosaccharides and available carbohydrates. Anal. Bioanal. Chem.  389(1), 291-308. Link to article

27McCleary, B. V., DeVries, J. W., Rader, J. I., Cohen, G., Prosky, L., Mugford, D. C., and Okuma, K. (2010) Determination of total dietary fiber (CODEX definition) by enzymatic-gravimetric method and liquid chromatography: Collaborative study. J. AOAC Int. (93)1, 221-233. Link to article

28McCleary, B. V., DeVries, J. W., Rader, J. I., Cohen, G., Prosky, L., Mugford, D. C., and Okuma, K. (2012). Determination of insoluble, soluble, and total dietary fiber (CODEX definition) by enzymatic-gravimetric method and liquid chromatography: Collaborative study. J. AOAC Int. (95)3, 824-844. Link to article