Development of isotope dilution-liquid chromatography/tandem mass spectrometry for the accurate determination of zearalenone and its metabolites in corn.

A method using isotope dilution-liquid chromatography-tandem mass spectrometry (ID-LC/MS/MS) was developed for the accurate determination of zearalenone (ZEN) and its five major metabolites in corn. 13C- or 2H-labeled analogues of the target mycotoxins were used as internal standards. As the immunoaffinity columns used demonstrated selectivity to a specific chiral isomer of a racemic mixture of zearalanone-d6, a clean-up cartridge without stereoselectivity (Mycosep 226 column) was selected for the same recovery of the analyte and its internal standard with adequate elimination of matrix interferences. The method demonstrated sufficient selectivity, sensitivity, accuracy and precision over a concentration range of 20-400 µg/kg. The limit of detections and limit of quantifications were 0.14-0.33 µg/kg and 0.45-1.11 µg/kg, respectively. The accuracy values were 96.7%-103.6%, with intra and inter-day precisions of less than 3% and 4%, respectively. The expanded measurement uncertainty was less than 7% (with a 95% confidence level).