气相色谱串接质谱测定食醋中多组分农药残留含量的方法研究

该研究建立了食醋中多组分农药残留的气相色谱串接质谱（GC-MS/MS）检测法，并成功运用于市售食醋中农药残留的定量 检测。食醋先用氨水中和至中性，再用甲苯/环己烷的混合溶液提取，经石墨化炭黑（GCB）和N-丙基乙二胺（PSA）净化，有机相膜过滤后 进样。样品经DB-5MS柱分离后采用多反应监测（MRM）模式进行检测，外标法定量。目标化合物在一定质量浓度范围内（7.81～125 μg/L） 线性关系良好，相关系数R2均＞0.99。方法的定量限（LOQ）和检出限（LOD）分别为10.0μg/L、5.00μg/L，平均回收率为78.5%～112.0%，相对标准偏差（RSDs）为5.90%～11.40%。该方法简便、快速、准确，已成功应用于市售食醋中农药残留的检测。

Determination of multi-component pesticide residue content in vinegar by GC-MS/MS

The method for the determination of multi-component pesticide residue in vinegar by GC-MS/MSwas established and successfully applied to quantitative determination of pesticide residues in commercial vinegar. The multi-component pesticide residue in vinegar was extracted with the mixed solution of toluene and cyclohexane afterammonium hydroxide neutralization. The extraction was purified with graphitized carbon blacks (GCB) and primary secondary amine (PSA). After filtration with organic membrane,the sample was separated with DB-5MS column,determined in multiple reactions monitoring (MRM) and quantified by external standard method. The target compounds had a good linear relationship within a cer- tain mass concentration range (7.81-125 μg/L), and the correlation coefficients R2 were more than 0.99. The limit of quantification (LOQ) and the limit of detection (LOD) of the method were 10.0 μg/L and 5.00 μg/L, respectively. The average recoveries were 78.5%-112.0% and the relative standard deviations (RSDs) were 5.90%-11.40%.The method was simple, rapid and accurate, which had success fully applied to the determination of pesticide residues in commercial vinegar.