凝胶渗透 GC-QQQ 法测定白酒中六六六与滴滴涕农药残留

摘要

After the evaporation of alcohol from liquor ,the organic phase is extracted by methylene chloride and acetone ,then purified and condensed by gel permeation chromatography method .The target analyte is detected by selective ion detection mode ,qualitatively confirmed by abundance ratio of ions ,and quantified by internal standard method .BHC and DDT have a good linear relationship (correlation coeffi-cients are greater than 0 .99) in mass concentration of 0.01-0.2 mg/L ,the detection limit is 0.20 -1.0μg/L .At three spiked levels of BHC and DDT in liquor ,the average recovery rates are from 80.2% to 108.2% and the repeatability relative standard deviations (RSDs) are between 2 .0% and 4 .6% .The method is accurate and reliable ,it can be used for the qualitative and quantitative analysis of BHC and DDT residues in liquor .%采用三重串联四级杆气质联用仪，建立了白酒中六六六和滴滴涕残留的快速检测方法。白酒去酒精后，采用二氯甲烷＋丙酮提取，有机相用凝胶渗透进行净化、浓缩；经H P-5M S毛细管柱分离后进行质谱分析，采用选择性离子检测模式，以子离子丰度比定性，内标法定量。六六六与滴滴涕在0.01～0.2mg／L质量浓度范围内线性关系良好（相关系数均大于0.99），方法检出限为0.20～1．0μg／L。白酒中六六六与滴滴涕的3个添加水平的回收率在80.2％～108．2％，重复性的相对标准偏差（RSD ）在2．0％～4．6％之间。该方法准确可靠，适用于白酒中六六六与滴滴涕残留的定性定量分析。