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  • A multi-analyte LC-MS/MS method for the analysis of 23 mycotoxins in different sorghum varieties: the forgotten sample matrix.

A multi-analyte LC-MS/MS method for the analysis of 23 mycotoxins in different sorghum varieties: the forgotten sample matrix.

Food chemistry (2015-02-11)
Emmanuel Njumbe Ediage, Christof Van Poucke, Sarah De Saeger
ABSTRACT

An LC-MS/MS method was developed and validated for the detection and quantification of 23 mycotoxins in different varieties of sorghum. The method performance characteristics were as follows: suitable linearity ranges for all 23 mycotoxins with p-value >0.05; limits of detection (1.2-50 μg/kg), limits of quantification (2.5-100 μg/kg), repeatability (RSDr, 7-22%), intermediate precision (RSDR, 14-44%) and apparent recovery (0.2-11%, expressed as bias). The method was applied to analyze 10 samples obtained from retail shops in Belgium (n=8) and Germany (n=2). Nine of the 10 samples (90%) were positive for the following mycotoxins: aflatoxin B1 (50 μg/kg), alternariol monomethyl ether (<LOQ - 79 μg/kg), alternariol (303-357 μg/kg), diacetoxyscirpenol (<LOQ - 91 μg/kg), fumonisin B1 (<LOQ - 95 μg/kg), fumonisin B2 (<LOQ), fumonisin B3 (<LOQ), T2 (<LOQ) and zearalenone (<LOQ).

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Acetic acid, natural, ≥99.5%, FG
Sigma-Aldrich
Acetic acid, ≥99.5%, FCC, FG
Supelco
Acetic acid, analytical standard
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Methanol, analytical standard
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Methanol, anhydrous, 99.8%
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15-O-Acetyl-4-deoxynivalenol from Fusarium graminearum
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3-Acetyldeoxynivalenol, from Fusarium roseum
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Aflatoxin B1 from Aspergillus flavus, from Aspergillus flavus
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Aflatoxin B2
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Sterigmatocystin
Sigma-Aldrich
Sterigmatocystin, powder, ≥98% (TLC)
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Zearalanone
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Acetic acid, for luminescence, BioUltra, ≥99.5% (GC)
Supelco
15-Acetyldeoxynivalenol solution, ~100 μg/mL in acetonitrile, analytical standard
Aflatoxin B2 solution, 3.80 μg/g in acetonitrile, ERM®, certified reference material
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Acetic acid-12C2, 99.9 atom % 12C
Supelco
Fumonisin B1 solution, ~50 μg/mL in acetonitrile: water, analytical standard
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Aflatoxin B2 solution, 0.5 μg/mL in acetonitrile, analytical standard
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3-Acetyldeoxynivalenol solution, ~100 μg/mL in acetonitrile, analytical standard
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Methanol, NMR reference standard
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3-Acetyldeoxynivalenol
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Fumonisin B1, reference material, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
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Aflatoxin B2 solution, certified reference material, 3 μg/mL in benzene:acetonitrile (98:2), ampule of 1 mL
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Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
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Methanol, ACS reagent, ≥99.8%
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Acetic acid, glacial, ACS reagent, ≥99.7%
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Methanol, Absolute - Acetone free
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Methanol, ACS spectrophotometric grade, ≥99.9%
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Acetic acid, glacial, puriss., meets analytical specification of Ph. Eur., BP, USP, FCC, 99.8-100.5%
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Acetic acid, glacial, ≥99.99% trace metals basis