气相色谱-质谱联用法测定浙贝母中20种农药残留

目的: 建立一种同时测定浙贝母中20种有机氯、拟除虫菊酯类农药残留量的分析方法。 方法: 样品用乙腈超声提取,经过Florisil固相萃取柱净化样品,用GC-MS选择离子模式进行测定,采用内标法进行定量,以3个添加水平测定样品的回收率和RSD。 结果: 回收率在67.7%~131.8%之间,RSD均低于15%。各农药检测限均小于0.01 mg·kg^-1。 结论: 采用该方法测定浙贝母中20种有机氯及拟除虫菊酯类农药残留量,简单,快速,准确,灵敏,且重复性好,可用于浙贝母中多种农药残留的同时测定。

Objective: To develop an analysis method based on gas chromatography-mass spectrometry(GC-MS)to determine 20 kinds of pesticide residue for Fritillarae Thunberghii Bulbus. Methods: Sample was exracted with acetonitrile by the ultrasonic extraction,and the extract was further purified through a Florisil solid-phase extraction column chromatography.The prepared sample was then analyzed by GC-MS with selective ion monitoring(SIM)mode.Quantitative by internal standard method.There were three supplemental Levels for determing recoreries and RSD. Results: The recoreries were 67.7%-131.8%.and all RSDs were less than 15.0%;The limits of detection(LOD)ranged below 0.01 mg·kg^-1 under the signal noise ratio 3:1. Conclusion: The method is simple,rapid,sensitive,and of good repeatability.It is suitable for the multiresidues analysis of pesticides in Fritillarae Thunberghii Bulbus.

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