凝胶渗透色谱净化-气相色谱测定糙米中7种常见有机磷农药残留  

Residue Determination of Seven Common Organophosphorus Pesticides in Unpolished Rice by GC with Gel Permeation Chromatography Clean-up

作　　者：刘咏梅[1] 王志华[1] 储晓刚[2] 

机构地区：[1]北京化工大学可控化学反应科学与技术基础教育部重点实验室,北京100029 [2]中国进出口商品检验技术研究所,北京100025

出　　处：《农药》2004年第10期460-462,共3页Agrochemicals

摘　　要：提供7种常见有机磷农药在糙米中同时测定的方法。前处理使用凝胶渗透色谱(GPC)净化技术,毛细管气相色谱火焰光度检测器测定,GC/MS进行确证测定7种常见有机磷农药(包括敌百虫、敌敌畏、甲胺磷、甲基嘧啶磷、二嗪磷、对硫磷、水胺硫磷)。并且采用GPC研究了7种有机磷农药在凝胶渗透色谱柱上的流出规律及净化效果,凝胶渗透色谱采用的流动相为环己烷-二氯甲烷(1∶1),最佳流速是5ml/min,收集最佳时间是14～25min。经方法的线性试验、精密度试验、检测限试验,验证了方法的可行性。方法最小检出质量比范围是1～8礸/kg,精密度为0.2%～10%。精密度试验的变异系数满足农药多残留痕量分析的要求。Amethod forsimultaneousdetermination of residuesof7 commonly used organophosphoruspesticidesin unpolished rice is discussed. Samples were extracted with ethyl acetate, and then cleaned up by gel permeation chroma- tography (GPC). The organophosphorus pesticides included trichlorfon, dichlorvos, methamidophos, diazinon, pirimiphos-methyl, parathion, and isocarbphos, and were determined by capillary gas chromatography with flame photometric detection. Results wereconfirmed by gaschromatography/mass spectrometry. GPC with amobile phase of cyclohexane/dichloromethane(1:1), an optimum flow rateof5 ml/min, and optimum collection timeof 14 to 25 min, was used to determine order of emergence from the column of the 7 pesticides, as well as efficacy of column clean-up. Feasibility of themethod was validated by conducting linearity, level of precision, and detection limit experiments. The minimum detectable concentration ranged from 1 to 8 μg/kg with a range of precision of 0.2 to 10%. Coefficient of variation of the precision experiments met requirements for analysis of trace amounts of multiple pesticides.

关 键 词：凝胶渗透色谱 净化 糙米 有机磷农药 残留 

分 类 号：X839.2[环境科学与工程—环境工程]