加速溶剂萃取-GPC液相色谱柱后衍生化测定动物源性食品中多种氨基甲酸酯类农药残留量

Determination of Carbamate Pesticides in Animal-Derived Foods with Accelerated Solvent Extraction and Gel Permeation Chromatography by High Performance Liquid Chromatography Post-Column Derivation

目的建立动物源食品中12种氨基甲酸酯类农药的快速分析方法。方法以乙腈作为提取溶剂,对试样采用加速溶剂萃取,自动凝胶渗透色谱仪净化预处理,N-丙基乙二胺(PSA)填料再净化,液相色谱柱后衍生化分离,荧光检测器测定,激发波长为330nm,发射波长为465nm,外标法定量。结果12种氨基甲酸酯类农药在样品中的最低检出浓度(S/N=3)在0.24μg/kg(异丙威)～1.02μg/kg(涕灭威亚砜)之间,当试样中氨基甲酸酯类农药添加浓度分别为0.05、0.1和0.2mg/kg时,方法回收率在62.1%±8.8%～104.0%±5.6%之间,RSD均小于20%。结论方法的最低检测限和加标回收率均符合农药残留分析的要求。

Objective To determine the multi-residues of 12 kinds of carbamate pesticides in animal-derived foods.Method The samples were extracted with acetonitrile by accelerated solvent extraction（ASE）and cleaned up by auto gel permeation chromatography（GPC）and primary secondary amine（PSA）packing material.The collected solution was analyzed by high performance liquid chromatography-fluorescence detector（HPLC-FLD）with post-column derivation and quantified by external standard method.The wavelengths of excitation and emission were set at 330 nm and 465 nm,respectively.Results The limits of detection（S/N=3）of 12 kinds of carbamate pesticides ranged from 0.24 μg/kg（isoprocarb）to 1.02 μg/kg（aldicarb sulfoxide）.The recoveries ranged from 62.1%±8.8% to 104.0%±5.6% by fortified with 0.05 mg/kg,0.1 mg/kg and 0.2 mg/kg of 12 kinds of carbamate pesticides into the blank treated samples.The RSD was less than 20%.Conclusion The limits of detection and the recoveries of 12 kinds of carbamate pesticides both meet the analysis requirements of pesticide residues.