Rapid Method for the Determination of Multiple Mycotoxins in Wines and Beers by LC-MS/MS Using a Stable Isotope Dilution Assay

A "dilute and shoot" method for the liquid chromatography-tandem mass spectrometric (LC-MS/MS) determination of multiple mycotoxins (aflatoxins B1, B2, G1, G2, ochratoxin A (OTA), fumonisins (F) B1 and B2, zearalenone, deoxynivalenol, T-2 toxin, and HT-2 toxin) in wines and beers has been developed and validated. Separation was accomplished using ultrahigh-performance liquid chromatography (UHPLC) with <10 min analysis time. Mycotoxins were detected by dynamic multiple reaction monitoring (MRM) in positive electrospray ionization mode. Due to matrix effects, C-13-uniformly labeled mycotoxins were added to the sample extracts prior to LC-MS/MS analysis. With external calibration, recoveries were 18-148% for white wines, 15-118% for red wines, and 20-125% for beers, at three spiking levels. The C-13-labeled internal standards compensated for matrix effects effectively, with overall recoveries of 94-112% for white wines, 80-137% for red wines, and 61-131% for beers, with greater recoveries for FB1 and FB2, at three spiking levels. The relative standard deviation was <20% for all analytes in the wines and beers. This method was applied to a USDA-funded nationwide survey of domestic and imported wines and beers for the determination of OTA and extended to include other mycotoxins.