建立了超快速液相色谱-串联质谱（ UFLC-MS／MS）同时测定当归药材中135种农药及其代谢物（包括有机磷类、氨基甲酸酯类、拟除虫菊酯类农药等）残留量的分析方法。以回收率为考察指标，评估了不同的提取溶剂、固相萃取小柱、洗脱溶剂及体积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，PSA 固相萃取柱净化处理，在电喷雾正离子扫描、依赖保留时间的多反应监测模式（ scheduled MRM ）下，以基质匹配校准曲线内标法定量。结果表明，135种农药及其代谢物在各自的浓度范围内线性关系良好（ r＞0.99）；3个添加水平（10、50、100μg／kg）下，除了烯草酮回收率偏低（62.0％~68.2％）外，其余农药的回收率为71.3％~119.7％，相对标准偏差（ RSD，n＝6）不大于19.9％，135种农药及其代谢物的定量限为1.0~10.0μg／kg。该方法样品前处理简单、快速、灵敏，可用于当归药材中多类别农药残留量的定性、定量。
A method using solid-phase extraction( SPE)followed by ultra-fast liquid chroma-tography-tandem mass spectrometry( UFLC-MS/MS)has been established for simultaneously quantitative determination of 135 pesticides and their metabolites ( organophosphorus pesti-cides,pyrethroid pesticides and carbamate pesticides,etc.)in Angelica sinensis. The pesticide residues were extracted from the samples by acetonitrile,cleaned-up with a primary secondary amine( PSA ) column and then analyzed using UFLC-MS/MS in multiple reaction monitoring ( MRM)mode with positive electrospray ionization. The pesticide residues were quantified by matrix matched standard solution-internal standard method. All of the pesticides had good linear responses with r>0. 99. The average recoveries of the pesticides at the spiked levels of 10,50,100 μg/kg ranged from 71. 3%-119. 7% with the RSDs of 1. 0%-19. 9%,except for clethodim(62.0%-68.2%). The limits of quantification of the 135 pesticides and their metabo-lites were 1.0-10.0 μg/kg. The results demonstrated that the method is simple,fast,sensitive and can be used for the analysis of the multiclass of pesticide residues in Angelica sinensis.
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