Abstract
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 13C-labeled internal standard. Therefore, we used the Königs-Knorr method to synthesize deoxynivalenol-3-β-d-[13C6]-glucoside originated from unlabeled deoxynivalenol and [13C6]-labeled glucose. Using the synthesized isotopically-labeled standard deoxynivalenol-3-β-d-[13C6]-glucoside and the purchased labeled standard [13C15]-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.
Highlights
Fusarium species are ubiquitously present and can infect a wide range of crops
We developed a stable isotope dilution assay (SIDA) for D3G and DON by using the newly-synthesized internal standard deoxynivalenol-3-β-D-[13C6]-glucoside and the commercially available standard [13C15]-DON, Molecules 2016, 21, 838 respectively
We developed a stable isotope dilution assay (SIDA) for D3G and DON by using the newly-synthesized internal standard deoxynivalenol-3-β-D-[13 C6 ]-glucoside and the commercially available standard
Summary
Fusarium species are ubiquitously present and can infect a wide range of crops. A well-known crop disease caused by different Fusarium species, like F. graminearum, F. culmorum, or F. avenaceum [1], can lead to yield loss and reduce grain quality. Fungal infestation of cereals, such as maize, wheat, and barley, is often associated with mycotoxin contamination and, especially affects the safety of human and animal diets. Fusarium toxins can be categorized in several major groups: fumonisins, enniatins, zearalenones, and trichothecenes [2]. The latter group can be divided in type A, B, C, and D trichothecenes, among which type A and B toxins are most abundant and relevant in food and feed [2]. Deoxynivalenol (DON) and its modified form deoxynivalenol-3-glucoside (D3G)
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