RRLC/MS/MS测定菊花中农药残留量

目的 建立中药材中113种农药残留量的测定方法,并用该方法测定了菊花中的农药残留量.方法 菊花样品经高速均质器提取、石墨化碳-氨基固相萃取柱(SPE)净化后,用高效液相色谱串联质谱仪(RRLC/MS/MS)进行定性、定量分析.结果 经方法学验证,113种农药重复性和精密度良好,回收率在72.3％ ～ 115.2％之间,相对标准偏差小于15％,检测限大多低于0.001mg/kg,符合农药多残留测定要求.与农药质谱数据对照,发现菊花中农药残留有13种之多.结论 本方法前处理简便、灵敏度高、重复性好,可用于菊花样品中农药残留的筛查和定量测定.

Determination of pesticides in Chrysanthemi Flos by RRLC/MS/MS

AIM To establish a method for the simultaneous determination of multi-pesticide residues in Chrysanthemi Flos.METHODS One hundred and thirteen pesticides were extracted by high-speed homogenization for 3 minuties,and then purified through Carb/NH2 solid phase extraction(SPE) cartridges.The residues were simultaneously identified and quantified by LC/MS/MS.RESULTS The analytical performance was demonstrated by the recoveries of three concentration levels for each pesticide.In general,the recoveries ranged from 72.3%-115.2%,with relative standard deviations(RSDs) better than 15%.The limit of detection(LOD) for most of the targeted pesticides was below 0.001 mg/kg.As compared with pesticides’MS data,thirteen kinds of pesticides were found in Chrysanthemi Flos.CONCLUSION This method is simple and sensitive with good reproducibility,which could be appilied to the screening and determination of pesticide residues in Chrysanthemi Flos.