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

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(R²>0.99);3个添加水平(10、50、100 μg/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1.0~20.0 μg/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。

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

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(R²>0.99) within the test ranges. The average recoveries of most pesticides at the spiked levels of 10, 50, 100 μg/kg ranged from 70.1%~117.7% with RSDs of 1.0%~20.0%. The limits of quantification of 50 pesticides were 1.0~20.0 μg/kg. The method provides a reliable basis for accurate, efficient and economical detection of targeted analytes in Angelica sinensis.