Liu Xiaoqin, Tong Ling, Meng Wenting, Sun Guoxiang
Se Pu. 2015 Aug;33(8):869-77. doi: 10.3724/sp.j.1123.2015.04005.
A method was established for the simultaneous determination of 99 pesticide residues 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 commercially 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.
建立了一种结合固相萃取技术（SPE）和气相色谱 - 三重四极杆串联质谱法（GC - QqQ - MS）同时测定99种农药残留量的方法。样品用乙酸乙酯萃取，并用氨基SPE柱净化。萃取物通过GC - MS/MS在多反应监测（MRM）模式下测定，并采用基质匹配内标法对农药进行定量。所有99种农药的结果在0.001 - 0.25 mg/L范围内显示出良好的线性，相关系数（r2）> 0.99。定量限（LOQs）在0.001 - 0.050 mg/kg之间。在0.05、0.10和0.20 mg/kg三个加标水平下，回收率在66.7%至128.0%之间，相对标准偏差（RSD）值通常低于18.3%。该方法已应用于测定13批市售样品，在4批白芍中检测到了乙基毒死蜱和p,p'-滴滴伊。该方法对于监测白芍中的99种农药残留具有高准确性、可靠性和灵敏性。
