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  • Screening multimycotoxins in food-grade gums by stable isotope dilution and liquid chromatography/tandem mass spectrometry.

Screening multimycotoxins in food-grade gums by stable isotope dilution and liquid chromatography/tandem mass spectrometry.

Journal of AOAC International (2014-07-24)
Kai Zhang, Jon W Wong, Zhengwei Jia, Marta Vaclavikova, Mary W Trucksess, Timothy H Begley
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.

MATERIALS
Product Number
Brand
Product Description

Supelco
Ammonium formate, eluent additive for LC-MS, LiChropur, ≥99.0%
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Ammonium formate, BioUltra, ≥99.0% (calc. based on dry substance, NT)
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Ammonium formate, ≥99.995% trace metals basis
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Methanol, NMR reference standard
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Methanol, HPLC Plus, ≥99.9%
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Methanol, ACS spectrophotometric grade, ≥99.9%
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Methanol, suitable for HPLC, gradient grade, suitable as ACS-grade LC reagent, ≥99.9%
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Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
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Residual Solvent - Acetonitrile, Pharmaceutical Secondary Standard; Certified Reference Material
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Methanol, analytical standard
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Aflatoxin G2-13C17 solution, ~0.5 μg/mL in acetonitrile, analytical standard
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Methanol, ACS reagent, ≥99.8%
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Methanol, Absolute - Acetone free
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Methanol, ACS reagent, ≥99.8%
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Methanol, Laboratory Reagent, ≥99.6%
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Ammonium formate, reagent grade, 97%
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Methanol, ACS reagent, ≥99.8%
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Methanol, BioReagent, ≥99.93%
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Methanol, suitable for HPLC, ≥99.9%
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Ammonium formate solution, BioUltra, 10 M in H2O
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Acetonitrile, electronic grade, 99.999% trace metals basis
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Deoxynivalenol
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Acetonitrile, ACS reagent, ≥99.5%
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Formic acid, reagent grade, ≥95%
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Formic acid, ≥95%, FCC, FG
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Acetonitrile, anhydrous, 99.8%
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Acetonitrile, suitable for HPLC, gradient grade, ≥99.9%
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Acetonitrile, HPLC Plus, ≥99.9%
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Acetonitrile, suitable for HPLC, gradient grade, ≥99.9%
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Aflatoxin B1-13C17 solution, ~0.5 μg/mL in acetonitrile, analytical standard