Simultaneous Determination of Alternaria Toxins, Ergot Alkaloid Epimers, and Other Major Mycotoxins in Various Food Matrixes by LC–MS/MS

Abstract

Abstract Background Various food commodities are vulnerable to different types of fungal pathogens and could be contaminated with differential classes of mycotoxins as a result. It is ideal to implement a generic method for the simultaneous determination of multi-mycotoxins in different food matrixes or agricultural products. Objective In this study, a simplified sample preparation procedure and a reliable LC–MS/MS analytical method were developed for the comprehensive measurement of 37 regulated and emerging mycotoxins including five Alternaria toxins (ATs) and six major ergot alkaloids (EAs) and their corresponding epimers. Four different food commodities (baby wheat cereal, peanut, tomato puree, and blended flour) were chosen for method validation to demonstrate the applicability of this analytical method across a wide range of food types. Methods Sample extraction was performed using a formic acid-acidified acetonitrile–water (4 + 1, v/v) solution followed by extract dry-down and reconstitution in a water–methanol (1 + 1, v/v) solution for analysis on a biphenyl LC column. Chromatographic analysis was performed using regular acidic LC conditions for baseline separation of ergot alkaloid epimers and completed with a short 11 min cycle time. Results Accurate quantification was achieved using matrix-matched calibration standards in the range of 0.4 to 400 µg/kg. The recoveries of all mycotoxins (except citrinin) in fortified samples were from 70 to 120%, and the RSD was less than 20%. Conclusion The established workflow was simple and fast for multi-mycotoxin determination in a wide variety of food commodities with LOQs needed to meet the regulatory levels. Highlights The developed method provided the unique benefit of simultaneous analysis of Alternaria toxins (ATs) and ergot alkaloids (EAs) together with other major regulated mycotoxins.