分散液液微萃取-气相色谱法测定水样中甲拌磷农药  

Determination of Phorate in Water Using Dispersive Liquid-Liquid Microextraction Coupled with Gas Chromatography

作　　者：谢洪学[1,2] 何丽君[1] 吴秀玲[2] 范璐[1] 卢奎[1] 王美美 孟大维[2] 

机构地区：[1]河南工业大学化学化工学院,郑州450052 [2]中国地质大学材料科学与化学工程学院,武汉430074 [3]丝宝日化研发部,武汉430056

出　　处：《分析化学》2008年第11期1543-1546,共4页Chinese Journal of Analytical Chemistry

基　　金：河南省重大科技攻关项目(No.0422031200);河南省自然科学基金(No.0511022400);河南省高等学校青年骨干教师资助计划项目资助

摘　　要：建立了基于分散液液微萃取（DLLME）的新型样品前处理方法,并采用气相色谱/氢火焰离子化检测器对水样中痕量的甲拌磷农药进行了测定。考察了影响分散液液微萃取的因素包括萃取溶剂、分散剂、样品体积、萃取温度和离心速度等。在最佳实验条件下,对甲拌磷的富集倍数达到300倍;检出限为0.001μL/L;方法的线性范围为0.01-10μL/L,R^2为0.9986;相对标准偏差为6.65%;回收率为104%。将分散液液微萃取法与单滴液相微萃取和离子液体-液相微萃取方法进行了对比,结果表明,分散液液微萃取技术具有操作简单、快捷（前处理时间小于5 min）、富集效果好、回收率高等优点。同时预言,将离子液体与分散液液微萃取结合,将会产生更加满意的结果。A novel method for the determination of phorate in water sample has been developed using dispersive liquid liquid microextraetion （DLLME） coupled with gas chromatography by flame ionization detection （FID）. The influence of extraction parameters including extraction solvent, disperser, solvent and volume, temperature, centrifugal speed and time was investigated. Under the optimum conditions the enrichment factor was 300 and the limit of detection was 0. 001 μL/L. The linear range was 0.01 - 10 μL/L, the R^2 was 0. 9986 and the recovery was 104% for phorate. The relative standard deviations （RSDs） were 6.7%. Analytical results obtained by DLLME were compared with those generated by single-drop microextraction （SDME） and liquid phase mireoextraction （LPME） in water sample. The advantage of the DLLME technique is simple and fast （less than 5 min） with high recovery and enrichment factor.

关 键 词：分散液液微萃取 单滴微萃取 液相微萃取 甲拌磷 气相色谱 

分 类 号：X839.2[环境科学与工程—环境工程]