Quantitative determination of non-starch polysaccharides in foods using Gas Chromatography with flame ionization detection

•The study provides a validated method for the measuring soluble and insoluble fibre in plant foods.•The method is applicable for foods that have less than 5% total fat.•Quantification as individual sugars can be achieved in 10 min.

A gas chromatographic method was developed for the quantitative determination of the monosaccharides of the soluble, insoluble fractions and the total non-starch polysaccharides (NSPs) content in foods with fat contents of less than 5%. Sample preparation involved enzymatic removal of starch and acid hydrolysis of the NSP to their constituent sugars. The alditol acetate derivatives were analysed on a wide bore capillary column with detection by flame ionization. The method was accurate, with recovery of spiked samples between 93.6% and 102.7% for intra-day analysis and between 93.2% and 104.7% for inter-day analysis. Repeatability was excellent; RSD values from 0.1 to 4.4% and 0.2 to 5.7% were observed from intra-day analysis and inter-day analysis, respectively. The peaks for all neutral sugars were sharp and separation was at baseline resolution with no interfering or co-eluting peaks.