Journal
MOLECULES
Volume 21, Issue 7, Pages -Publisher
MDPI AG
DOI: 10.3390/molecules21070838
Keywords
modified mycotoxin; deoxynivalenol-3-glucoside; stable isotope dilution assay; LC-MS; MS; beer; labeled standard; synthesis
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.
- Wissenschaftliche Station fur Brauerei in Munchen e.V.
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Modified mycotoxins have been gaining importance in recent years and present a certain challenge in LC-MS/MS analysis. Due to the previous lack of a labeled isotopologue of the modified mycotoxin deoxynivalenol-3-glucoside, in our study we synthesized the first C-13-labeled internal standard. Therefore, we used the Konigs-Knorr method to synthesize deoxynivalenol-3--d-[C-13(6)]-glucoside originated from unlabeled deoxynivalenol and [C-13(6)]-labeled glucose. Using the synthesized isotopically-labeled standard deoxynivalenol-3--d-[C-13(6)]-glucoside and the purchased labeled standard [C-13(15)]-deoxynivalenol, a stable isotope dilution LC-MS/MS method was firstly developed for deoxynivalenol-3-glucoside and deoxynivalenol in beer. The preparation and purification of beer samples was based on a solid phase extraction. The validation data of the newly developed method gave satisfying results. Intra- and interday precision studies revealed relative standard deviations below 0.5% and 7%, respectively. The recoveries ranged for both analytes between 97% and 112%. The stable isotope dilution assay was applied to various beer samples from four different countries. In summary, deoxynivalenol-3-glucoside and deoxynivalenol mostly appeared together in varying molar ratios but were quantified in rather low contents in the investigated beers.
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