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(r.2)均大于0.99,检出限(LOD,S/N=3)为5~20 μg/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 (NIV),deoxynivalenol (DON),3-acetyl-deoxynivalenol (3-ACDON) and 15-acetyl-deoxynivalenol (15-ACDON) in various grains and their products by liquid chromatography-tandem 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 C18 column (100 mm×2.1 mm,1.7 μm) with gradient elution using acetonitrile-water as mobile phases.The analytes were quantified by isotope internal standard method.The correlation coefficients (r.2) were all above 0.99.The limits of detection (LODs,S/N=3) ranged from 5 μg/kg to 20 μg/kg.The recoveries of the five mycotoxins spiked in blank grain and its product samples varied from 84.2% to 114.5%,with the relative standard deviations (RSDs) of 0.4%-9.9% (n=6).The method is accurate,efficient,sensitive and practical.
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