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盐析萃取样品前处理结合GC-MS/MS检测葡萄酒中农药及其代谢产物残留
Determination of pesticide and its metabolites in wine by salting out extraction sample pretreatment combined with GC-MS/MS
【摘要】 以葡萄酒中所含的乙醇为萃取剂,利用乙醇-水-磷酸氢二钾盐析萃取体系提取,结合GC-MS/MS法测定了葡萄酒中农药及其代谢产物残留。实验表明:在葡萄酒样品中加入适量乙醚可以减小萃取液的极性,从而提高脂溶性的农药残留的萃取率,并降低色素、单宁等极性杂质在萃取液中的含量。在萃取液中直接加入适量无水MgSO4和净化剂PSA,即可实现萃取液的快速净化。该样品前处理方法操作简便,快速。用于葡萄酒中27种农药及其代谢产物残留的测定,回收率为78%~112%,相对标准偏差为2.9%~11%,检出限为0.9~8.0μg·kg-1。
【Abstract】 The alcohol contained in wine was used as the extractant, and the pesticides and their metabolites in wine were extracted and determined by the ethanol water potassium phosphate salt extraction system.The results showed that adding appropriate amount of ether into wine sample could reduce the polarity of the extract, improve the extraction rate of fat soluble pesticide residues, and reduce the content of polar impurities such as pigment and tannin in the extract.By adding appropriate amount of anhydrous magnesium sulfate and PSA directly into the extraction liquid, the extraction liquid can be quickly purified.The method is simple and rapid, and can be used for the determination of 27 pesticides and their metabolites in wine.The recoveries are 78%~112%,the relative standard deviations are 2.9%-11%,and the detection limits are 0.9~8.0 μg·kg-1.
【Key words】 pesticide; metabolites; salting out extraction; GC-MS/MS; wine;
- 【文献出处】 化学研究与应用 ,Chemical Research and Application , 编辑部邮箱 ,2022年02期
- 【分类号】TS262.6;O657.63
- 【下载频次】194