采用固相萃取技术（ SPE）结合气相色谱-三重四极杆质谱（ GC-MS／MS）建立了白芍中99种农药同时检测的分析方法。试样用乙酸乙酯提取，采用氨基固相萃取柱净化后，在 GC-MS／MS 多反应监测（ MRM）模式下进行检测，基质匹配标准曲线内标法定量。结果表明，99种农药在0.001~0.25 mg／L 范围内线性关系良好，相关系数（ r2）大于0.99，方法定量限为0.001~0.050 mg／kg。加标水平为0.05、0.10和0.20 mg／kg时，99种农药的平均回收率为66.7％~128.0％，相对标准偏差（ RSD，n=6）小于18.3％。对市售的13批样品进行测定，其中4批样品中检出微量的毒死蜱和 p，p′-滴滴伊。实验证明，建立的 SPE净化和 GC-QqQ-MS相结合的检测方法具有准确可靠、灵敏度高等优点，适用于白芍中多农药残留的同时筛查测定。
A method was established for the simultaneous determination of 99 pesticide resi-dues with combination of solid-phase extraction technique ( SPE ) and gas chromatography-triple quadrupole tandem mass spectrometry( GC-QqQ-MS ). The sample was extracted with ethyl acetate,and cleaned-up by an amino SPE column. The extract was determined by GC-MS/MS in multi-reaction monitoring ( MRM ) mode, and matrix-matched internal standard method was applied to quantify the pesticides. The results of all the 99 pesticides showed good linearity in the range of 0. 001-0. 25 mg/L,with correlation coefficients(r2)> 0. 99. The limits of quantification( LOQs ) were between 0. 001-0. 050 mg/kg. The recoveries were between 66. 7% and 128. 0% with RSD values typically lower than 18. 3% at three spiked levels of 0. 05, 0. 10 and 0. 20 mg/kg. This method has been applied to determine thirteen batches of commer-cially available samples,chlorpyriphos-ethyl and p,p′-DDE were detected in four batches of Paeoniae Radix Alba. The method is highly accurate,reliable and sensitive for monitoring the 99 pesticide residues in Paeoniae Radix Alba.
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