同位素内标-液相色谱-串联质谱法同时测定粮食及其制品中的5种真菌毒素

Simultaneous determination of five mycotoxins in various grains and their products by liquid chromatography-tandem mass spectrometry with isotope internal standard

建立了同位素内标-液相色谱-串联质谱快速测定粮食及其制品中玉米赤霉烯酮(ZON)、雪腐镰刀菌烯醇(NIV)、脱氧雪腐镰刀菌烯醇(DON)及其衍生物3-乙酰基脱氧雪腐镰刀菌烯醇(3-ACDON)和15-乙酰基脱氧雪腐镰刀菌烯醇(15-ACDON)5种真菌毒素的分析方法。以乙腈-水(84∶16,v/v)为提取液,采用多功能净化柱净化,同位素内标法定量。5种真菌毒素在各自的线性范围内线性关系良好,相关系数(r2)均大于0.99,检出限(LOD,S/N=3)为5~20μg/kg。大麦、小麦、燕麦、玉米等9种代表性粮食及其制品在3个不同添加水平下的加标回收率为84.2%~114.5%,相对标准偏差(RSD)为0.4%~9.9%(n=6)。该法操作简单,成本低,准确可靠,灵敏度高,可同时检测粮食及其制品中的5种真菌毒素。

A rapid method was established for the determination of zearalenone(ZON),nivalenol(N IV),deoxynivalenol(DON),3-acetyl-deoxynivalenol(3-ACDON)and15-acetyldeoxynivalenol(15-ACDON)in various grains and their products by liquid chromatographytandem mass spectrometry(LC-MS/MS).The samples were extracted by acetonitrile-water(84:16,v/v),and cleaned-up by multifunctional column without any further step.The separation was carried out on an Acquity UPLC?BEH C18column(100m m x2.1mm,1.7pm)with gradient elution using acetonitrile-water as mobile phases.The analytes were quantified by isotope internal standard method.The correlation coefficients(r2)were all above0.99.The limits of detection(LODs,S/N=3)ranged from5pg/kg to20pg/kg.The recoveries of the five mycotoxins spiked in blank grain and its product samples varied from84.2%to114.5%,with the relative standard deviations(RSDs)of0.4%-9.9%(n=6).The method is accurate,efficient,sensitive and practical.