分散液液微萃取-气相色谱法快速测定水中23种有机磷农药  

Determination of 23 Organophosphorous Pesticide Residues in Water Using Dispersive Liquid-Liquid Microextraction Coupled with Gas Chromatography

作　　者：李晓晶[1] 陈安[2] 黄聪[1] 施洁[1] 于鸿[1] 

机构地区：[1]广州市疾病预防控制中心,广东广州510080 [2]中山大学化学与化学工程学院,广东广州510275

出　　处：《分析测试学报》2011年第3期326-329,共4页Journal of Instrumental Analysis

基　　金：广州市医学科研课题资助项目(2009-YB-126)

摘　　要：建立了分散液液微萃取（DLLME）的新型样品前处理方法，并采用气相色谱／火焰光度检测器对饮用水中的治螟磷、甲拌磷、二嗪农、乙拌磷、甲基毒死蜱、甲基对硫磷、皮蝇磷、杀螟松、马拉硫磷、毒死蜱、倍硫磷、对硫磷、溴硫磷、嘧啶磷、甲基异硫磷、稻丰散、杀扑磷、丙溴磷、乙硫磷、三唑磷、三硫磷、哒嗪硫磷、亚胺硫磷23种痕量有机磷农药残留进行测定。对萃取溶剂及其体积、分散剂及其体积、萃取时间等条件进行了优化。在最佳实验条件下，23种有机磷农药的线性范围为0．04～4．0μg／L（r≥0．998），检出限为0．002—0．016g/L，方法的加标回收率为75％～109％，相对标准偏差为1．5％～13．3％。分散液液微萃取技术具有操作简单、快捷、富集效果好、回收率高等优点。A novel method of dispersive liquid - liquid microextraction （DLLME） and gas chromatography with flame photo detection（FPD） was developed for the determination of 23 organophosphorous pesticide residues （ OPPs）, including sulfotep, phorate, diazinon, disulfoton, chlropyrifos-methyl, methyl-parathion, runnel, fenitrothion, malathion, chlorpyrifos, fenthion, parathion, bromophos, pirimiphos-ethyl, isofenphos-methyl, phenthoate, methidathion, profenofos, ethion, triazophos, trithion, pyridaphethione and phosmet in water sample. The influence of extraction parameters including the types and volumes of extraction solvent and disperser solvent as well as extraction time were investigated. Under the optimum conditions, the calibration curves for 23 OPPs were linear in the range of 0. 04 - 4. 0 μg/L with correlation coefficients not less than 0. 998. The limits of detection ranged from 0. 002 μg/L to 0. 016 μg/L. The recoveries of 23 OPPs at two spiked concentration levels of 0. 08μg/L and 2.0 μg/L were in the range of 75% - 109% with relative standard deviations （RSDs） of 1.5% - 13.3% . The DLLME technique showed good recovery and high enrichment factor. advantages of simplicity, rapidness,

关 键 词：分散液液微萃取 气相色谱 有机磷农药 饮用水 

分 类 号：O657.71[理学—分析化学] F767.2[理学—化学]