固相萃取/气相色谱法测定禽蛋中19种农药残留

Determination of 19 Pesticides Residues in Eggs by Gas Chromatography with Solid Phase Extraction

建立了QuEChERS及固相萃取净化技术结合气相色谱法测定禽蛋中19种农药(联苯菊酯、甲氰菊酯、氯菊酯、氯氰菊酯、氰戊菊酯、溴氰菊酯、敌敌畏、甲胺磷、乙酰甲胺磷、二嗪磷、乐果、甲基嘧啶磷、毒死蜱、杀螟硫磷、丙溴磷、氟虫腈、氟甲腈、氟虫腈硫醚及氟虫腈砜)残留的分析方法。蛋液样品经乙腈及QuEChERS提取盐包提取后,采用石墨化碳黑(GCB)吸附剂和十八烷基硅烷键合硅胶(C18)SPE小柱净化,以Agilent DB-1701(30 m×0.32 mm,0.25μm)毛细管色谱柱分离,在气相色谱火焰光度检测器(Flame photometric detector,FPD)及电子捕获检测器(Electron capture detector,ECD)上检测,外标法定量。结果显示,19种农药在各自线性浓度范围内线性关系良好,相关系数(r2)均不小于0.9993;在低、中、高3个加标水平下的回收率为78.6%~105%,相对标准偏差(n=6)为1.6%~9.3%,检出限(LOD,S/N=3)为0.138~8.33μg/kg,定量下限(LOQ,S/N=10)为0.461~27.8μg/kg。该方法操作简便、分离效果好、可靠稳定,可满足禽蛋中多种农药残留的检测要求。

A gas chromatographic(GC)method based on QuEChERS extraction salt package and solid phase extraction was established for the determination of 19 pesticides residues,i.e.bifenthrin,fenpropathrin,permethrin,cypermethrin,fenvalerate,deltamethrin,dichlorvos,methamidophos,acephate,diazinon,dimethoate,pirimiphos-methyl,chlorpyrifos,fenitrothion,profenofos,fipronil,fipronil-desulfinyl,fipronil sulfide and fipronil sulfone in eggs.The sample was extractd with acetonitrile and QuEChERS extraction salt package,and then purified with GCB adsorbent and C18 SPE.The analytes were separated on an Agilent DB-1701(30 m×0.32 mm,0.25μm)polarity capillary column,then detected by GC with FPD detector and ECD detector,and quantified by external standard method.Results showed that there were good linear relationships for 19 pesticides in their respective concentration ranges,with correlation coefficients(r2)not less than 0.9993.The recoveries at three spiked levels of low,meddle and high ranged from 78.6%to 105%,with relative standard deviations(n=6)of 1.6%-9.3%.The limits of detection(LOD,S/N=3)and limits of quantitation(LOQ,S/N=10)were in the ranges of 0.138-8.33μg/kg and 0.461-27.8μg/kg,respectively.With the advantages of simplicity,good separation,reliability and stability,the established method could meet the requirements for determination of pesticides multi residues in eggs.