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LC–MS/MS method validation for the quantitation of 1-kestose in wheat flour

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Abstract Fructan analysis is challenging due to several mono-, di-, and oligosaccharides as well as starch and proteins present in wheat grains which interfere with the analysis. So far, a… Click to show full abstract

Abstract Fructan analysis is challenging due to several mono-, di-, and oligosaccharides as well as starch and proteins present in wheat grains which interfere with the analysis. So far, a sensitive and fully validated LC–MS/MS method is missing although even small amounts of short-chain fructans such as 1-kestose are suggested to elicit gastrointestinal symptoms in patients suffering from irritable bowel syndrome. Therefore, the aim of this study was to validate a LC–MS/MS method for the detection of 1-kestose in a complex wheat matrix according to international guidelines. The chromatographic separation was performed on a C18 column coupled with a triple quadrupole MS in MRM mode using the transition m/z 503 → m/z 119 for the quantitation of 1kestose. Accuracy of 1-kestose quantitation in an aqueous solution was 105.5 %. However, the poor recovery of 64.1 % in a complex wheat matrix demonstrated the great impact of proteins and other constituents present in wheat. Nevertheless, the proposed method allows precise quantification of 1-kestose amounts ≥0.1 ppm. The robustness of the method was confirmed by the results being within 6.03 % of the target value. The validated method was successfully applied for the measurement of 10 different wheat samples with 1-kestose amounts between 7.0 and 50.2 ppm.

Keywords: quantitation kestose; wheat; method; method validation; validation quantitation

Journal Title: Journal of Food Composition and Analysis
Year Published: 2021

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