Journal
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
Volume 408, Issue 1, Pages 307-317Publisher
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-015-9110-7
Keywords
Trichothecenes; Enniatins; Stable isotope dilution assay; LC-MS/MS; Solid-phase extraction; Barley
Funding
- Forschungskreis der Ernahrungsindustrie e.V. (FEI, Bonn)
- AiF
- German Federal Ministry of Economic Affairs and Energy (AiF) [17221 N]
- Wissenschaftsforderung der Deutschen Brauwirtschaft e.V.
- Faculty Graduate Center Weihenstephan of TUM Graduate School at Technische Universitat Munchen, Germany
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A multi-mycotoxin stable isotope dilution LC-MS/MS method was developed for 14 Fusarium toxins including modified mycotoxins in cereals (deoxynivalenol, 3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol, HT2-toxin, T2-toxin, enniatin B, enniatin B1, enniatin A1, enniatin A, beauvericin, fusarenone X, nivalenol, deoxynivalenol-3-glucoside, and zearalenone). The chromatographic separation of the toxins with particular focus on deoxynivalenol and deoxynivalenol-3-glucoside was achieved using a C-18-hydrosphere column. An expedient sample preparation method was developed that uses solid-phase extraction for the purification of trichothecenes combined with zearalenone, enniatins, and beauvericin and provides excellent validation data. Linearity, intra-day precision, inter-day precision, and recoveries were >= 0.9982, 1-6 %, 5-12 %, and 79-117 %, respectively. Method accuracy was verified by analyzing certified reference materials for deoxynivalenol, HT2-toxin, and T2-toxin with deviations below 7 %. The results of this method found barley malt samples from 2012, 2013, and 2014 frequently contaminated with high concentrations of enniatin B, deoxynivalenol, and its modified mycotoxin deoxynivalenol-3-glucoside. Samples from 2012 were especially contaminated. Fusarenone X was not detected in any of the analyzed samples.
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