SPE-LC-MS/MS和SPE-GC-MS/MS测定绞股蓝中109种农药残留  

Determination of 109 pesticide residues in Gynostemma pentaphyllum by SPE-LC-MS/MS and SPE-GC-MS/MS

作　　者：熊颖[1] 李纯[1] 任晋 栗建明[1] 顾利红[1] XIONG Ying;LI Chun;REN Jin;LI Jian-ming;GU Li-hong(Guangzhou Institute for Drug Control,Guangzhou 510160)

机构地区：[1]广州市药品检验所,广州510160

出　　处：《中南药学》2020年第12期2044-2049,共6页Central South Pharmacy

基　　金：国家药品医疗器械审评审批制度改革子课题(中药)项目资助(No.ZG2016-2-10)。

摘　　要：目的建立绞股蓝中109种农药(含禁用农药49种)残留的液质联用和气质联用检测法。方法采用乙腈提取,经固相萃取柱HLB(液质)和PRiME HLB(气质)净化,均采用多反应监测模式,空白基质加对照品法测定。结果 109种农药在各自线性范围内与测定值线性关系良好,相关系数均大于0.99,平均回收率在53.49%~120.74%,回收率RSD在0.84%~12%,精密度RSD在1.1%~15%,方法检测限在0.001~0.060 mg·kg^-1。结论本方法能快速、有效地检测绞股蓝的农药残留,可用于绞股蓝农药监测,也可为中药材的农药残留检测提供借鉴与参考。Objective To determine 109 (including 49 forbidden pestcides) pesticide residues in Gynostemma pentaphyllum by LC-MS/MS and GC-MS/MS.Methods The samples were extracted with acetonitrile and purified by passing mode solid phase extraction (SPE) with Oasis HLB cartridge (LC-MS/MS) or PRiME HLB cartridge (GC-MS/MS).Quantitative analysis was carried out in multiple-reaction monitoring mode and with standard curve of blank matrix matching.Results The calibration curves of 109 pesticide residues showed good linearity with all correlation coefficients above 0.99.The average recoveries for all target compounds fell within 53.49%~120.74%,with relative standard deviations of 0.84%~12%.The relative standard deviations of precision expriment was at 1.1%~15%.The limit of quantitation was 0.001~0.060 mg· kg^-1.Conclusion The method is fast and effective for the screening and confirmation of 109 pesticide residues in Gynostemma pentaphyllum,which provides a basis for the control of pesticide residues in other Chinese herbal medicines.

关 键 词：固相萃取 液相色谱-串联质谱 气相色谱-串联质谱 绞股蓝 农药残留 

分 类 号：R284[医药卫生—中药学]