2014Journal of AOAC InternationalRequires access

Screening Multimycotoxins in Food-Grade Gums by Stable Isotope Dilution and Liquid Chromatography/Tandem Mass Spectrometry

Kai Zhang, Jon W. Wong, Zhengwei Jia, Marta Václavíková, Mary W Trucksess, Timothy H. Begley

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Abstract

Stable isotope dilution with LC/MSIMS was used to determine the following 11 mycotoxins in food grade gums: aflatoxins B1, B2, G1, and G2; deoxynivalenol; fumonisins B1, B2, and B3; ochratoxin A; T-2 toxin; and zearalenone. Samples were fortified with 11 [13C]-uniformly labeled internal standard ([13C]-IS) mycotoxins that corresponded to the 11 target mycotoxins and extracted by acetonitrile-water (4 + 1, v/v), followed by LC/MS/MS analysis. Mycotoxins were quantitated with the fortified [13C]-IS in each sample. The average recoveries of aflatoxins B1, B2, G1, and G2 (1, 5, and 25 microg/kg); deoxynivalenol and fumonisins B1, B2, and B3 (25, 100, and 500 microg/kg); and ochratoxin A, T-2 toxin, and zearalenone (10, 50, and 250 microg/kg) ranged from 84 to 117% with RSDs less than 20%. Method-dependent LOQs were from 0.1 (aflatoxin B1) to 25 microg/kg (fumonisin B3). Among 20 market samples, aflatoxin B1 (< LOQ) was detected in a Guar gum and a Tragacanth gum, and zearalenone (6 +/- 0.6 microg/kg) was detected in a Xanthan gum. The detected mycotoxins were further confirmed by comparing their enhanced product ion spectra to those of reference standards. The single laboratory validated stable isotope dilution and LC/MSIMS method provides sufficient selectivity, sensitivity, accuracy, and reproducibility with a simple sample preparation to screen the 11 mycotoxins in gums.

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What this paper is about

Stable isotope dilution with LC/MSIMS was used to determine the following 11 mycotoxins in food grade gums: aflatoxins B1, B2, G1, and G2; deoxynivalenol; fumonisins B1, B2, and B3; ochratoxin A; T-2 toxin; and zearalenone. Samples were fortified with 11 [13C]-uniformly labeled internal standard ([13C]-IS) mycotoxins that corresponded to the 11 target mycotoxins and extracted by acetonitrile-water (4 + 1, v/v), followed by LC/MS/MS analysis. Mycotoxins were quantitated with the fortified [13C]-IS in each sample. The average recoveries of aflatoxins B1, B2, G1, and G2 (1, 5, and 25 microg/kg); deoxynivalenol and fumonisins B1, B2, and B3 (25, 100, and 500 microg/kg); and ochratoxin A, T-2 toxin, and zearalenone (10, 50, and 250 microg/kg) ranged from 84 to 117% with RSDs less than 20%. Method-dependent LOQs were from 0.1 (aflatoxin B1) to 25 microg/kg (fumonisin B3). Among 20 market samples, aflatoxin B1 (< LOQ) was detected in a Guar gum and a Tragacanth gum, and zearalenone (6 +/- 0.6 microg/kg) was detected in a Xanthan gum. The detected mycotoxins were further confirmed by comparing their enhanced product ion spectra to those of reference standards. The single laboratory validated stable isotope dilution and LC/MSIMS method provides sufficient selectivity, sensitivity, accuracy, and reproducibility with a simple sample preparation to screen the 11 mycotoxins in gums.

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Available abstract

Stable isotope dilution with LC/MSIMS was used to determine the following 11 mycotoxins in food grade gums: aflatoxins B1, B2, G1, and G2; deoxynivalenol; fumonisins B1, B2, and B3; ochratoxin A; T-2 toxin; and zearalenone. Samples were fortified with 11 [13C]-uniformly labeled internal standard ([13C]-IS) mycotoxins that corresponded to the 11 target mycotoxins and extracted by acetonitrile-water (4 + 1, v/v), followed by LC/MS/MS analysis. Mycotoxins were quantitated with the fortified [13C]-IS in each sample. The average recoveries of aflatoxins B1, B2, G1, and G2 (1, 5, and 25 microg/kg); deoxynivalenol and fumonisins B1, B2, and B3 (25, 100, and 500 microg/kg); and ochratoxin A, T-2 toxin, and zearalenone (10, 50, and 250 microg/kg) ranged from 84 to 117% with RSDs less than 20%. Method-dependent LOQs were from 0.1 (aflatoxin B1) to 25 microg/kg (fumonisin B3). Among 20 market samples, aflatoxin B1 (< LOQ) was detected in a Guar gum and a Tragacanth gum, and zearalenone (6 +/- 0.6 microg/kg) was detected in a Xanthan gum. The detected mycotoxins were further confirmed by comparing their enhanced product ion spectra to those of reference standards. The single laboratory validated stable isotope dilution and LC/MSIMS method provides sufficient selectivity, sensitivity, accuracy, and reproducibility with a simple sample preparation to screen the 11 mycotoxins in gums.

Key concepts: Isotope dilution, Chromatography, Chemistry, Liquid chromatography–mass spectrometry, Mass spectrometry, Tandem mass spectrometry

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