Determination of deoxynivalenol and metabolites in maize samples by LC-MS/MS

In Vietnam, the regulation QCVN 8-1:2011/BYT has been issued to control mycotoxin content in food products. However, there are currently no regulations or studies on their derivatives and metabolites. Deoxynivalenol-3-glucoside (D3G) and two acetylated derivatives of deoxynivalenol (DON), namely 15-acetyldeoxynivalenol (15-AcDON) and 3- acetyldeoxynivalenol (3-AcDON), have been frequently detected in naturally contaminated grains such as wheat, barley, and corn. This study developed and applied a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to determine deoxynivalenol (DON) and its metabolites, including deoxynivalenol-3-glucoside (D3G), 3- acetyldeoxynivalenol (3-AcDON), and 15-acetyldeoxynivalenol (15-AcDON) in maize. The instrumental conditions comprised a C18 HSS SB (150 mm × 2.1 mm × 1.7 µm) column for separation and an MS/MS detector in positive and negative electrospray ionization (ESI) source, employing multi-reactive ion monitoring mode, with an injection volume of 2 µL. The method has been fully validated and meets the performance requirements of AOAC, demonstrating high specificity. The linearity range was established from 100 µg/kg to 1000 µg/kg, with a method detection limit (MDL) of 30 µg/kg. The repeatability and recovery rates were determined to be between 1.45% to 4.31% and 90% to 110%, respectively. The validated method was applied to analyze 50 maize samples. Deoxynivalenol (DON) was detected in 10 samples (20%), while deoxynivalenol-3-glucoside (D3G), 3- acetyldeoxynivalenol (3-AcDON), and 15-acetyldeoxynivalenol (15-AcDON) were not detected in any of the samples.