气相色谱-质谱联用法测定浙贝母中20种农药残留

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李鑫健;方翠芬;马临科;祝明

【期刊名称】《药物分析杂志》【年(卷),期】2012(032)003

【摘要】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 CC - MS with selective ion monitoring (SIM)mode. Quantitative by internal standard method. There were three supplemental Levels for determing recore-ries 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,

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