利用QuEChERS-UPLC-MS/MS法测定甘蓝、草莓中7种农药残留的实验条件优化探索

The Condition Optimization Determination of Multi-Residue of Pesticides in Cabbage and Strawberry by QuEChERS-UPLC-MS/MS

为了给农药残留检测工作提供新的技术和方法,建立了一种通过QuEChERS方法和超高效液相色谱-串联质谱法快速测定不同基质中多种农药残留的方法。样品用乙腈提取,经QuEChERS方法C18净化,以T3色谱柱(100 mm×2.1 mm×1.8μm)通过超高效液相色谱分离,电喷雾离子源正离子多反应监测(MRM)模式进行测定。通过流动相、吸附剂种类和吸附剂用量的选择,以及加标回收率实验,建立和优化了QuEChERS-UPLC-MS/MS测定农药多残留的方法。结果表明:除咪鲜胺外,其他农药在1～200μg/L范围内各待测物线性良好,高、中、低浓度回收率在93.4%～99.1%之间,变异系数小于4%,方法的检出限为0.1～1.0μg/kg。基质效应对定量结果影响可忽略不计。QuEChERS-UPLC-MS/MS方法简便、快速、准确、灵敏、节省有机溶剂,可满足甘蓝、草莓中多种农药残留同时检测的实际需要。

A method of QuEChERS-UPLC-MS/MS to determine multi-residue of pesticides in different matrix rapidly was established. Samples were extracted by acetonitrile, cleaned up by C18 with QuEChERS method, separated by T3 column （100 mm× 2.1 min× 1.8μm） via UPLC, analyzed by multiple reaction monitoring （MRM） mode via positive electrospray ionization. Through the selection of mobile phase test, adsorbent selection test, adsorbent dosage test and the recovery test, the method of QuEChERS-UPLC-MS/MS for the deter- mination of multi-residue analysis was established and optimized. The results show that the pesticides have good linearity in the ranges of 1--200μg/L except prochloraz. The absolute recoveries are between 93.4% and 99. 1%, and the precision is lower 4%. The limit of quantitative detection is 0.1-1.0 μg/kg. Matrix effect on the quantitative results can be neglected. The QuEChERS-UPLC-MS/MS method is simple, rapid, saving organic solvent, which can meet the demands of practical used determination of multi-residue pesticides in cabbage and strawberry. accurate, sensitive, for the simultaneous