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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
Aflatoxin G1-13C17 solution, ~0.5 μg/mL in acetonitrile, analytical standard
Sigma-Aldrich
Methanol solution, NMR reference standard, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
Sigma-Aldrich
Acetonitrile, electronic grade, 99.999% trace metals basis
Supelco
Aflatoxin B2-13C17 solution, ~0.5 μg/mL in acetonitrile, analytical standard
Sigma-Aldrich
Ammonium formate solution, BioUltra, 10 M in H2O
Supelco
Aflatoxin B1-13C17 solution, ~0.5 μg/mL in acetonitrile, analytical standard
Sigma-Aldrich
Methanol-12C, 99.95 atom % 12C
Supelco
Ammonium formate solution, 10 mM in H2O, suitable for HPLC
Sigma-Aldrich
Formic acid solution, BioUltra, 1.0 M in H2O
Sigma-Aldrich
Formic acid, ≥95%, FCC, FG
Sigma-Aldrich
Acetonitrile, anhydrous, 99.8%
Sigma-Aldrich
Deoxynivalenol
Sigma-Aldrich
Methanol solution, (Methanol:Dimethyl sulfoxide 1:1 (v/v))
Sigma-Aldrich
Methanol solution, contains 0.50 % (v/v) triethylamine
Supelco
Acetonitrile, analytical standard
Sigma-Aldrich
Formic acid, ACS reagent, ≥96%
Sigma-Aldrich
Acetonitrile, ReagentPlus®, 99%
Sigma-Aldrich
Formic acid, reagent grade, ≥95%
Sigma-Aldrich
Acetonitrile, biotech. grade, ≥99.93%
Sigma-Aldrich
Acetonitrile, ≥99.5% (GC)
Sigma-Aldrich
Formic acid, ACS reagent, ≥88%
USP
Methyl alcohol, United States Pharmacopeia (USP) Reference Standard
Supelco
Acetonitrile, Pharmaceutical Secondary Standard; Certified Reference Material
USP
Residual Solvent Class 2 - Acetonitrile, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Acetonitrile, suitable for DNA synthesis, ≥99.9% (GC)
Sigma-Aldrich
Acetonitrile, ACS reagent, ≥99.5%
Sigma-Aldrich
Acetonitrile, suitable for HPLC, gradient grade, ≥99.9%
Sigma-Aldrich
Acetonitrile, suitable for HPLC-GC, ≥99.8% (GC)
Sigma-Aldrich
Acetonitrile, for HPLC, for UV, ≥99.9% (GC)
Sigma-Aldrich
Acetonitrile, suitable for HPLC, gradient grade, ≥99.9%