气相色谱-串联质谱同位素内标法测定中草药中124种农药及其代谢物残留  

Determination of 124 pesticide residues in chinese medicinal herbs by GC-MS-MS with isotope internal standard

作　　者：王建国[1] 万丽葵[2] 魏玉霞[1] 刘晓峰[1] 郭虹[1] 杨玉竹[1] 李博[1] 

机构地区：[1]北京市通州区疾病预防控制中心,北京101100 [2]中国疾病预防控制中心,北京100050

出　　处：《分析试验室》2017年第2期220-225,共6页Chinese Journal of Analysis Laboratory

摘　　要：建立测定中草药中124种农药及其代谢物残留的气相色谱-串联质谱(GC-MS-MS)方法。采用同位素内标法,样品经乙腈提取,采用混合型固相分散萃取剂净化,加入分析保护剂校正基质效应。色谱柱为DB-5MS(30 m×0.25 mm×0.25μm),程序升温,GC-MS-MS测定。124种农药残留在0.005~0.40μg/m L内呈线性关系,在0.06~0.3 mg/kg内的平均回收率为84.8%~108.7%,RSD为2.1%~12%,方法检出限(LOD)为0.005~0.013 mg/kg。该方法适合于中草药中农药多残留的同时检测。A method was established for the determination of 124 pesticide residues in Chinese medicinal herbs by GC-MS-MS.Using isotope internal standard method,the samples were extracted by acetonitrile and cleaned up with mixed solid-phase dispersion.Analyte protectants were added to counteract the matrix effect.The chromatographic column was DB-5ms（30 m × 0.25 mm ×0.25 μm）,with temperature programming.The calibration curves for 124 pesticide residues were linear in the range of 0.005 - 0.40 μg/m L.The average recovery rated were 84.8% - 108.7% in the range of 0.06 - 0.3 mg/kg with RSDs of 2.1% - 12%.The LODs were 0.005 - 0.013 mg/kg.The developed method is simple,rapid,sensitive and high efficient for simultaneous analysis of 124 pesticide residues in Chinese medicinal herbs.

关 键 词：中草药 气相色谱串联质谱法 农药残留 同位素内标 分析保护剂 

分 类 号：S481.8[农业科学—农药学] S567[农业科学—植物保护]