凝胶渗透色谱–气相色谱质谱法测定黑鱼品中敌敌畏

Determination of Dichlorvos in Snakehead by Gas Chromatography-Mass Spectrography Using Gel Penetrating Chromatogram

摘要: 目的：对黑鱼中敌敌畏的检测方法进行优化。本文采用优化的样品前处理方法，通过凝胶色谱仪净化，利用气相色谱–电子轰击离子源–质谱法(GC-EI-MS)进行检测。敌敌畏在0.01~1 mg/L范围内具有良好的线性关系，相关系数为0.9999。敌敌畏农药残留的检出限为0.01 mg/kg。3个添加水平的回收率范围为73%~90%，相对标准偏差不大于10%。

Abstract: Aim: To optimize the determination method of dichlorvos in snakehead. This paper was based on the optimization of sample pretreatment method, and then the supernatant was analyzed by gas chro- matography-mass spectrography using gel penetrating chromatogram. Calibration curves of dichlorvos were linear between 0.01 and 1 mg/L, with correlation coefficients of more than 0.9999. The limit of method detection is 0.01 mg/kg. Recoveries of the dichlorvos were in the range of 73%~90% with relative standard deviations of no more than 10% in a spiked concentration.