固相萃取-高效液相色谱-串联质谱联用法快速测定中药材猴耳环中47种农药残留

建立了固相萃取-高效液相色谱-串联质谱同时检测中药材猴耳环中47种农药残留的方法。样品经乙腈高速匀浆提取，亲水亲油平衡材料 (简称HLB) 固相萃取柱净化，采用电喷雾正离子扫描 (ESI+)、依赖保留时间的多反应监测模式 (scheduled MRM) 测定，基质匹配标准溶液外标法定量。结果表明:47种农药在各自线性范围内其质量浓度与峰面积间呈良好线性关系 (r > 0.9920)，定量限在0.001~0.015 mg/kg之间，平均回收率在54%~117%之间，RSD在2.0%~15%之间，其中40种农药的平均回收率在70%~120%之间，满足痕量分析要求。该法操作简便快捷，稳定性好，灵敏度高，适用于猴耳环中农药多残留的监控与筛查。

Rapid determination of 47 pesticide residues in Folium Archidendri by SPE- high performance liquid chromatography-tandem mass spectrometry

In this work, a method was developed for the determination of 47 pesticide residues in Folium Archidendri using HLB solid phase extraction by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Electrospray ionization source was applied by positive ionization (ESI+) in scheduled multiple reaction monitoring modes. The samples were extracted with acetonitrile by high speed homogenizer, purified by HLB SPE, and analyzed quantitatively by matrix-matched external standard curve method. The calibration curves of 47 targets showed good linearity with correlation coefficients of above 0.9920. The average recoveries were in the range of 54%-117%, with RSDs of 2.0%-15%. LOQs of all the tested pesticides were 0.001-0.015 mg/kg. Among them, the recoveries of 40 pesticides were in the range of 70%-120%, which met the requirements of multi-pesticides trace analysis. This analytical method was simple, quick, stable and sensitive, which could be used for a monitoring and screening analysis of multi-pesticide residues in Folium Archidendri.