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

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.