A liquid chromatography-tandem mass spectrometric(LC-MS/MS) method was developed for the quantitative determination of aflatoxin B1(AFB1),aflatoxin M1(AFM1),T-2 toxin(T-2),HT-2 toxin(HT-2),deoxynivalenol(DON),ochratoxin A (OTA) and zearalenone(ZEN) in shrimp feed.Samples were extracted with 15 mL acetonitrile-water(4∶1,by volume),and degreased with 10 mL acetonitrile saturated hexane.The extract was cleaned up with a MycoSpinTM400 multitoxin LC-MS/MS clean-up column.The target compounds were separated on an Hypersil Gold(150 mm×2.1 mm,5 μm)chromatographic column by gradient elution with methanol-water containing 0.03%ammonia as mobile phase,and analyzed simultaneously by electron spray ionization mass spectrometry in positive or negative ion mode,and quantified by the matrix-matched external standard method.Under the optimized conditions,there were good linearities for the analytes in corresponding concentration range with their correlation coefficients(r2) more than 0.991.The limits of detection(LOD)ranged from 1.83 μg/kg to 12.63 μg/kg.Average recoveries for the target mycotoxins at high,medium and low spiked levels ranged from 87.5%to 116%with relative standard deviations of 2.4%-18%.The developed method could provide a reference for the simultaneous determination of mycotoxins in aquatic feeds.
关键词
真菌毒素液相色谱-串联质谱(LC-MS/MS)饲料
Keywords
mycotoxinliquid chromatography-tandem mass spectrometry(LC-MS/MS)feed