采用超高效液相色谱-静电场轨道阱高分辨质谱,建立了茶叶中21种农药残留量的检测方法。茶叶样品经甲醇和水(V甲醇∶V水=1∶1)提取后,采用乙二胺-N-丙基硅烷和强阳离子交换剂作为混合吸附剂进行萃取净化。以C18色谱柱进行色谱分离,采用Full Scan扫描模式进行定性、定量分析。结果显示,21种农药在0.5~200βμg·L-1范围内均呈良好的线性关系,相关系数(r2)大于0.99。在10、50、100βμg·kg-1 3个加标水平下,平均回收率为70%~125%之间,相对标准偏差(RSD)小于15%,定量限为10βμg·kg-1。本方法操作简单快速,灵敏度高,适用于茶叶中21种农药残留检测。
A ultra performance liquid chromatography orbitrap high resolution mass spectrometry method for the determination of 21 pesticides in tea was developed. The tea samples were extracted by methanol-water (Vmethanol∶Vwater=1∶1), and cleaned up by a mixture of adsorbents containing primary secondary amine and strong cation exchanger. The chromatography analysis was performed on a C18 column. The target analytes were analyzed by high resolution mass spectrometry under Full Scan mode. The results showed that the linearities of 21 pesticides ranged from 0.5βμg·L-1 to 200βμg·L-1 with correlation coefficients higher than 0.99. At the spiked levels of 10, 50 and 100βμg·kg-1, the average recoveries were from 70% to 125%, with the relative standard deviations (RSDs) below 15%. The limits of quantitation were 10βμg·kg-1. The method is simple, rapid, sensitive and appropriate for the determination of 21 pesticide residues in tea.
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