超高效液相色谱-串联质谱法对比11种净化方式对当归中50种农药残留检测的影响

Evaluation on Efficiencies of 11 Purification Methods Toward 50 Pesticide Residues in Angelica sinensis by Ultra-high Performance Liquid Chromatography/Tandem Mass Spectrometry

采用超高效液相色谱-串联质谱仪(UPLC-MS/MS)同时测定当归药材中50种农药残留,对比了11种净化方式对检测结果的影响,筛选出最有效的基质净化方法。以回收率为考察指标,评估了不同基质净化方法对当归中多农残的提取净化效果,最终确定样品经乙腈提取,NaCl净化,在电喷雾正负离子扫描、依赖保留时间的动态多反应监测模式(dMRM)下,以基质匹配内标法定量。结果表明,50种农药在NaCl净化法下回收率最高,在各自的浓度范围内线性关系良好(R^2>0.99);3个添加水平(10、50、100μg/kg)下,大多数农药的回收率为70.1%~117.7%,相对标准偏差(RSD,n=6)不大于20.0%,50种农药的定量限为1.0~20.0μg/kg。该方法为当归中准确、高效、经济的检测目标物提供了可靠依据。

Fifty pesticides in Angelica sinensis,were determined by ultra-high performance liquid chromatography/tandem mass spectrometry(UPLC-MS/MS).Through comparing 11 kinds of purification methods,the best effective matrix purification method was selected.The pesticide residues were extracted from samples with acetoniteile,cleaned-up with NaCl and then analyzed using UPLC-MS/MS in dynamic multiple reaction monitoring(dMRM)mode with positive and negative electrospray ionization.The pesticide residues were quantified by matrix matched standard solution-internal standard method.All calibration curves showed good linearity(R^2>0.99)within the test ranges.The average recoveries of most pesticides at the spiked levels of 10,50,100μg/kg ranged from 70.1%~117.7%with RSDs of 1.0%~20.0%.The limits of quantification of 50 pesticides were 1.0~20.0μg/kg.The method provides a reliable basis for accurate,efficient and economical detection of targeted analytes in Angelica sinensis.