QuEChERS结合气相色谱-三重四极杆串联质谱法快速测定地参中63种农药残留

采用QuEChERS前处理技术结合气相色谱-三重四极杆串联质谱法（GC-MS/MS）对不同产地的10批地参中的63种农药残留进行测定。样品用1%醋酸-乙腈溶液和QuEChERS萃取盐包提取，经1.2 g硫酸镁、400 mg N-丙基乙二胺（PSA）及200 mg石墨化炭黑（GCB）净化，在选择反应监测模式（SRM）下检测，基质匹配内标法定量。结果显示，63种农药在5～500 ng/mL质量浓度范围内线性关系良好，相关系数（R2）均＞0.996 4；在0.05 mg/kg、0.25 mg/kg和0.75 mg/kg 3个添加水平下，各农药化合物加标回收率为71.5%～120.4%，方法的相对标准偏差（RSD）为0.12%～9.70%；仪器精密度试验结果RSD为1.93%～5.06%；检出限（LOD）为0.5～3.6 μg/kg，定量限（LOQ）为1.7～12.0 μg/kg。不同产地地参均不同程度检出5种农药残留，包括氯菊酯、丙环唑、氯唑磷、苯霜灵和肟菌酯。

Determination of 63 kinds of pesticide residues in Lycopus lucidus by QuEChERS-GC-MS/MS

63 kinds of pesticide residues in 10 batches of Lycopus lucidus from different habitats were determined by QuEChERS pretreatment combined with GC-MS/MS.The samples were extracted with 1%acetic acid-acetonitrile solution and QuEChERS,purified by 1.2 g MgSO4,400 mg N-propyleth-ylenediamine(PSA)and 200 mg graphitized carbon black(GCB),detected under selected reaction monitoring(SRM)mode,and quantitated with the matrix-matched internal standard method.The results showed that 63 pesticides had good linearity in the range from 5-500 ng/ml,and the correlation coefficients(R2)were greater than 0.9964.The standard recovery rates of each pesticide compound were mainly between 71.5%and 120.4%at the three spiked concentration levels(0.05 mg/kg,0.25 mg/kg,0.75 mg/kg),and the relative standard deviation(RSD)of the method was between 0.12%and 9.70%.The RSD of instrument precision was between 1.93%and 5.06%,the limit of detection(LOD)was 0.5-3.6μg/kg,and the limit of quantification(LOQ)was 1.7-12.0μg/kg.5 kinds of pesticide residues in L.lucidus from different habitats were detected,including permethrin,propiconazole,isazofos,benalaxyl,and trifloxystrobin.