QuEChERS-超高效液相色谱-串联质谱法测定葡萄中100种农药及其代谢物

目的 建立了葡萄中多菌灵等100种农药及其代谢物的超高效液相色谱-三重四级杆串联质谱（UPLC-MS/MS）检测方法。方法 样品采用1%乙酸乙腈涡旋提取，N-丙基乙二胺（PSA）粉末分散固相萃取净化，经BEH-C18超高效液相色谱柱分离后，在电喷雾正离子（ESI+）模式下，通过多反应监测（MRM）模式测定。结果 100种农药及其代谢物在1~100 ug/L浓度范围内线性关系良好，决定系数（r2）均大于0.9984；100种农药及代谢物的平均回收率在77.6%~118%之间，相对标准偏差为0.3%~29%，符合农药多残留分析的要求。结论 该方法能够对葡萄中100种农药及其代谢物进行快速、准确的测定。

Determination of 100 kinds of pesticides and their metabolites in grapes by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

Objective An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) method was developed for the determination of 100 pesticides and metabolites in grapes.Methods The tested grape sample was extracted with 1% glacial acetic acid acetonitrile and then purified with N- propyl ethylenediamine (PSA) powder, separated by BEH-C18 ultra high performance liquid chromatography column, and detected by multiple reaction monitoring (MRM) mode in electrospray positive ion (ESI+) mode. Results The results showed that the linearity was satisfied with the correlation coffcients more than 0.998;The average recoveries of 100 pesticides and their metabolites ranged from 77.6% to 118% with relative standard deviation(RSD)of 0.29% to 28.9% which were good enough for the routine analysis of the pesticide residues. Conclusion The method can be used as routine analysis method in multi-residual pesticide monitoring of grapes.