An integrated procedure for the measurement of total dietary fibre (including resistant starch), non-digestible oligosaccharides and available carbohydrates


A method is described for the measurement of dietary fibre, including resistant starch (RS), non-digestible oligosaccharides (NDO) and available carbohydrates. Basically, the sample is incubated with pancreatic α-amylase and amyloglucosidase under conditions very similar to those described in AOAC Official Method 2002.02 (RS). Reaction is terminated and high molecular weight resistant polysaccharides are precipitated from solution with alcohol and recovered by filtration. Recovery of RS (for most RS sources) is in line with published data from ileostomy studies. The aqueous ethanol extract is concentrated, desalted and analysed for NDO by high-performance liquid chromatography by a method similar to that described by Okuma (AOAC Method 2001.03), except that for logistical reasons, d-sorbitol is used as the internal standard in place of glycerol. Available carbohydrates, defined as d-glucose, d-fructose, sucrose, the d-glucose component of lactose, maltodextrins and non-resistant starch, are measured as d-glucose plus d-fructose in the sample after hydrolysis of oligosaccharides with a mixture of sucrase/maltase plus β-galactosidase.

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The author thanks Patricia Rossiter and Anna Dragar for performing the RS analyses and HPLC of LMWNDO. TDF determinations were performed by Luzmila Ludena, Bread Research Institute Ltd., North Ryde, NSW, Australia.

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Correspondence to Barry V. McCleary.

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

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  • Total dietary fibre
  • Resistant starch
  • Non-digestible oligosaccharides
  • Available carbohydrates
  • Integrated method