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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
Dimethyl ether, puriss., ≥99.9% (GC)
Sigma-Aldrich
Hexane, anhydrous, 95%
Sigma-Aldrich
Ethyl acetate, ReagentPlus®, ≥99.8%
Sigma-Aldrich
Ethyl acetate, anhydrous, 99.8%
Sigma-Aldrich
Dimethyl ether, puriss., ≥99.9% (GC)
Supelco
Dichloromethane, Selectophore, ≥99.5%
Supelco
Dichloromethane, ≥99.9%
Sigma-Aldrich
Ethyl acetate, ≥99%, FCC, FG
Sigma-Aldrich
Dimethyl ether, ≥99%
Sigma-Aldrich
Ethyl acetate, natural, ≥99%, FCC, FG
Sigma-Aldrich
Dichloromethane, anhydrous, ≥99.8%, contains 40-150 ppm amylene as stabilizer
Sigma-Aldrich
5α-Androstan-17β-ol-3-one, purum, ≥99.0% (TLC)
Supelco
Hexane, analytical standard
Supelco
5α-Androstan-17β-ol-3-one, VETRANAL®, analytical standard
Sigma-Aldrich
Methanol-12C, 99.95 atom % 12C
Supelco
Aflatoxin G1
Millipore
Bifido Selective Supplement B, suitable for microbiology
Sigma-Aldrich
Methanol solution, NMR reference standard, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
Supelco
Neosolaniol
Supelco
Dichloromethane, analytical standard
Sigma-Aldrich
Aflatoxin G2
Sigma-Aldrich
Aflatoxin G1, from Aspergillus flavus
Sigma-Aldrich
Zearalenone, fungal mycotoxin
Sigma-Aldrich
Deoxynivalenol
Sigma-Aldrich
Fumonisin B1 from Fusarium moniliforme, ≥98% (HPLC)
Supelco
Diacetoxyscirpenol solution, ~100 μg/mL in acetonitrile, analytical standard
Sigma-Aldrich
5α-Androstan-17β-ol-3-one, ≥97.5%
Sigma-Aldrich
Dimethyl ether, ≥99.9%
Supelco
Ethyl acetate, analytical standard
Sigma-Aldrich
Dichloromethane, puriss. p.a., ACS reagent, reag. ISO, ≥99.9% (GC)