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

The article focuses on the development and validation of a simplified and robust liquid chromatography–tandem mass spectrometry (LC–MS/MS) method for the simultaneous determination of 37 regulated and emerging mycotoxins, including five Alternaria toxins (ATs) and six major ergot alkaloids (EAs) with their epimers, across diverse food matrices. Using a single-step sample extraction with formic acid–acidified acetonitrile–water and analysis on a biphenyl LC column under acidic conditions, the method achieved accurate quantification with recoveries mostly between 70–120% and relative standard deviations below 20% in baby wheat cereal, peanut, tomato puree, and blended flour. Matrix-matched calibration was employed to compensate for matrix effects inherent to different food types, enabling quantification limits suitable for regulatory compliance. This approach addresses challenges in multi-mycotoxin analysis by enabling simultaneous detection of chemically diverse mycotoxins, including ATs and EAs, which often require distinct analytical conditions.