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目的建立液相色谱-串联质谱法测定延胡索药材中12种农药残留的方法。方法延胡索样品用乙腈提取,过N-丙基乙二胺(PSA)柱净化,用ZORBAX Eclipse plus C18色谱柱分离,以电喷雾电离串联质谱在正离子多反应监测(MRM)模式下进行测定,内标法定量。结果 12种农药成分在相应的测定范围内线性关系良好,相关系数在0.997 7~0.999 9内,加样回收率范围为65.5%~117.8%,RSD范围为0.4%~4.5%,各农药的检出限为0.1~2.5μg·kg?1。结论本方法简便、灵敏、重现性好,可用于延胡索药材中12种农药残留的同时检测。延胡索药材农药残留量甚微,符合安全性要求。
Objective To establish a method for the determination of 12 pesticide residues in Cynanodum cuspidata by liquid chromatography-tandem mass spectrometry. Methods The samples of Corydalis yanhusuo were extracted with acetonitrile and purified with a N - propyl ethylenediamine (PSA) column. The samples were separated on a ZORBAX Eclipse plus C18 column and analyzed by electrospray ionization tandem mass spectrometry in positive ion MRM mode. Internal standard method. Results The linear relationships of the 12 pesticide components in the corresponding range of determination ranged from 0.997 7 to 0.999 9. The recoveries ranged from 65.5% to 117.8% with RSD ranging from 0.4% to 4.5%. The pesticide tests The limit is 0.1 ~ 2.5μg · kg -1. Conclusion The method is simple, sensitive and reproducible. It can be used for the simultaneous detection of 12 pesticide residues in Corydalis yanhusuo. Corydalis pesticide residues are small, in line with safety requirements.