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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。
To establish a gas chromatography-tandem mass spectrometry (GC-MS-MS) method for the determination of 124 pesticides and their metabolites in Chinese herbs. Using isotope internal standard method, the sample was extracted with acetonitrile, purified by mixed solid-phase dispersive extractant, and analyzed by adding protective agent to correct the matrix effect. The chromatographic column was DB-5MS (30 m × 0.25 mm × 0.25 μm), temperature programmed and determined by GC-MS-MS. The average recoveries of 124 pesticides from 0.005 to 0.40 μg / mL were 84.8% -108.7% with RSDs of 2.1% ~ 12%. The detection limits (LODs) ) Is 0.005 to 0.013 mg / kg. The method is suitable for the simultaneous detection of pesticide residues in Chinese herbal medicine.