双气相色谱-双脉冲火焰光度法高通量检测动物性食品中有机磷农药残留及其代谢产物

High throuput analysis of organophosphorus pesticide residues and their metabolites in animal original foods by dual gas chromatography-dual pulse flame photometric detection

建立了动物性食品中包括代谢产物在内的54种有机磷农药残留及其代谢产物的双气相色谱-双脉冲火焰光度检测器(GC-PFPD)检测方法。动物组织样品经丙酮提取后以二氯甲烷进行液-液萃取,经凝胶渗透色谱净化后采用配有双脉冲火焰光度检测器的气相色谱仪测定。采用外标法定量,有机磷农药的响应与其浓度在线性范围内均呈良好的线性关系,相关系数在0.990 5～0.999 9之间。分别在空白鸡肉、羊肉、牛肉和猪肉样品中添加低、中和高3个加标水平的标准品进行了回收试验,回收率在50.5%～128.1%之间,相对标准偏差(n=6)在1.1%～25.5%之间,证明该方法的精密度和准确度良好。各有机磷农药的检出限在0.001～0.170 mg/kg之间,定量限在0.002～0.455 mg/kg之间。对从市场采集的动物组织样品进行了测定,检出敌敌畏、乙拌磷亚砜等有机磷农药残留。本方法灵敏度高、特异性强,且能同时检测有机磷农药多残留及其代谢产物,能够更加真实地反映动物性食品中有机磷农药的残留水平。

A method was established for the quantitative determination of 54 organophosphorus pesticide residues and their metabolites in foods of animal origin by dual gas chromatography-dual pulse flame photometric detection.Homogenized samples were extracted with acetone and methylene chloride,and cleaned-up by gel permeation chromatography（GPC）.The response of each analyte showed a good linearity with a correlation coefficient not less than 0.99.The recovery experiments were performed by a blank sample spiked at low,medium and high fortification levels.The recoveries for beef,mutton,pork,chicken were in the range of 50.5%-128.1% with the relative standard deviations（n=6） of 1.1%-25.5%,which demonstrated the good precision and accuracy of the present method.The limits of detection for the analytes were in the range of 0.001-0.170 mg/kg,and the limits of quantification were in the range of 0.002-0.455 mg/kg.Animal food samples collected from markets such as meat,liver and kidney were analyzed,and the residues of dichlorovos and disulfoton-sulfoxide were found in the some samples.The established method is sensitive and selective enough to detect organophosphorus pesticide residues in animal foods.