Single laboratory validation for a method of analysis for Fusarium toxins including deoxynivalenol-3-glucoside in wheat and barley

Abstract
Recent reports have demonstrated that the deoxynivalenol (DON) mycotoxin produced by Fusarium sp. is metabolized to deoxynivalenol-3-glucoside (DON-3G) by glycosidation enzymes in infected plants, and subsequently DON-3G accumulates in the plant body. Although DON-3G is less toxic than DON, it is converted back to DON upon release in the intestinal tract of an animal. This reformed DON exhibits the same toxicity as DON initially produced by Fusarium. Thus, testing should be extended to DON-3G and other important mycotoxins. This study aimed to evaluate an analytical method based on liquid chromatography with tandem mass spectrometry (LC-MS/MS) for the detection and quantification of DON, acetyl forms of DON (3-Ac-DON, 15-Ac-DON), a glycoside form of DON (DON-3G), and another Fusarium mycotoxins such as nivalenol (NIV), 4-Ac-NIV, T-2 toxin (T-2), HT-2 toxin (HT-2), zearalenone (ZEA), and diacetoxyscirpenol (DAS) in wheat and barley. The method was validated using wheat and barley samples spiked with each mycotoxin at levels of 0.01 and 0.1 mg/kg. The average recovery of mycotoxins in wheat and barley ranged from 77.4% to 110.3% with a relative standard deviation of 2.2% to 15.7%. These findings demonstrated that this LC-MS/MS method is reliable for the analysis of Fusarium mycotoxins, including the acetyl and glycoside forms of DON, in wheat and barley. All parameters corresponding to the trueness, repeatability, and reproducibility as intermediate precision satisfied the criteria values.