【摘要】 目的建立同时检测面粉中DON、15A-DON、3A-DON、ZEN、NIV5种镰刀菌毒素的超高效液相色谱-串联质谱(UPLC-MS/MS)方法。方法用乙腈-水(84∶16)溶液提取样品,经净化柱净化后,氮气吹干,20%甲醇液定容,用UPLC-MS/MS进行测定。UPLC-MS/MS检测镰刀菌毒素的条件为梯度洗脱,流动相为0.3%氨水和乙腈;质谱采集模式为电喷雾正离子多反应监测模式。结果 5种镰刀菌毒素在5~1 000μg/L线性范围内呈线性关系良好(相关系数r值均>0.99);检出限:DON、3A-DON、15A-DON均为0.4μg/kg,ZEN为0.3μg/kg,NIV为0.2μg/kg。不同加标水平的5种镰刀菌毒素回收率为70%~105%,相对标准偏差(RSD)为5.2%~8.9%。结论 UPLC-MS/MS法具有操作简单、灵敏度高、重现性好等特点,可同时检测面粉中5种镰刀菌毒素。更多还原

【Abstract】 Objectives To develop a simutaneous determination of 5fusarium toxins(DON,15A-DON,3-DON,ZEN,NIV5)in wheat flour by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The samples were extracted by 84%(v/v)acetonitrile-water mixure,followed by purification by purification column and dried by nitrogen.Using 20%(v/v)methanol-water mixture to dissolve to samples to a certain volume,which was analyzed by UPLCMS/MS with gradient elution.Acetonitrile and 0.3%(v/v)ammonia-water were used as the mobile phases.The mass spectrometric acquisitions were carried out by multiple reaction monitoring(MRM)in electro spray positive ionization mode.ResultsThe 5fusarium toxins showed good linear relationships in concentration ranges of 5-1 000μg/L with the correlation coefficients more than 0.99.The limits of detection(LOD)for DON,3A-DON,15A-DON were all 0.4μg/kg,LOD of ZEN and NIV were0.3μg/kg and 0.2μg/kg,respectively.The recovery rates of 5fusarium toxins at the different spiking levels ranged from 70%-105%,with relative standard deviations(RSD)of 5.2%-8.9% 。Conclusion The established UPLC-MS/MS method is easy to operate,with high sensitivity and reproducibility.It satisfies requirement for simultaneous determination of 5fusarium toxins in wheat flour.更多还原