建立了超高效液相色谱-质谱/质谱联用法(ultra-performance liquid chromatography-mass spectrometry/mass spectrometry,UPLC-MS/MS)同时分析葡萄酒中41种农药和7种真菌毒素残留的方法。样品经QuEChERS净化,UPLC-MS/MS测定,外标法定量。结果表明,48种待测物质在各自线性范围内呈现良好的线性关系,相关系数均大于0.999,检出限为0.01～5 μg/kg,定量限为0.05～17 μg/kg;在25、50、80 μg/kg加标水平下平均回收率为79.6%～122.5%,相对标准偏差(relative standard deviation,RSD,n=6)为0.21%～6.39%。该方法前处理简单、稳定性好,可以广泛应用于葡萄酒中农药和真菌毒素残留的快速筛查和定量检测。
A ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was established for the simultaneous analysis of 41 pesticides and seven mycotoxins in wine. The samples were purified with QuEChERS, and detected by UPLC-MS/MS. Some compounds were quantified by external standard method. All 48 substances showed good linearity in their linear range, the correlation coefficients were greater than 0.999, The limits of detection ranged from 0.01 μg/kg to 5 μg/kg, and the limits of quantification ranged from 0.05 μg/kg to 17 μg/kg. The average recoveries at three spiked levels of 25, 50 and 80 μg/kg were 79.6%-122.5%, with relative standard deviations(RSD) of 0.21%-6.39% (n=6). Thus, the optimized method has simple, high efficiency, good stability, and it can be widely used in the rapid screening and quantitative detection of multiple drug residues in wine.
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