离子液体和氯代溶剂分散液-液微萃取／高效液相色谱法联用富集和分析环境水样中酞酸酯类污染物的对比研究  

Comparative study of ionic liquids and chlorinated solvents based dispersive liquid-liquid microextraction of phthalates pollutants in environmental water followed by high performance liquid chromatography

作　　者：马维炜[1] 王青[1] 薛林科[1] 杜新贞[1] 

机构地区：[1]西北师范大学化学化工学院,甘肃省生物电化学与环境分析重点实验室,兰州730070

出　　处：《分析试验室》2013年第7期30-35,共6页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金项目(21265019)资助

摘　　要：以4种室温离子液体和4种氯代溶剂为萃取剂,与高效液相色谱(HPLC)联用,对比研究了分散液-液微萃取(DLLME)对5种痕量酞酸酯类化合物(PAEs)的富集分离性能。以1-辛基-3-甲基咪唑六氟磷酸盐([OMim][PF6])和建议研究四氯化碳替代品为典型萃取溶剂优化了萃取条件。结果表明,在1.00～100μg/L范围内色谱峰面积与PAEs浓度成良好的线性关系(相关系数>0.995);对于10.0μg/L加标混合样品,平均加标回收率88.2%～103.3%,RSD在2.1%～6.8%之间(n=5),LOD在0.01～0.08μg/L范围内(S/N=3)。与四氯化碳相比,[OMim][PF6]作为DLLME的萃取溶剂对PAEs的富集倍数较高,水相盐效应影响较小。超声波辅助微萃取(USA)可在2 min达到平衡,建立的USA-DLLME-HPLC方法可用于黄河水样和城生活区污水样品中痕量PAEs的富集分离和测定。A comparative study of 4 ionic liquids and 4 chlorinated solvents based dispersive liquid-liquid microextraction （DLLME） was performed for the enrichment and separation of 5 phthalates （PAEs） in environmental water combined with high performance liquid chromatography （HPLC）. The experimental conditions were examined with 1-octyl-3-methylimidazolium hexafluorophosphate and tetrachloromethane as representative extraction solvents, respectively. Under the optimized conditions, the results showed that good linearity was obtained in the range of 1.00 ～ 100 μg/L with correlation coefficients of exceeding 0. 995. The average recoveries ranged from 88.2% to 103.3% for water samples spiked with 10.0 μg/L and the relative standard deviations （RSD） were 2.1% ～ 6.8 % （ n = 5 ）. The limits of detection were within 0.01 ～ 0.07 μg/L （S/N = 3 ）. [ OMim ] [ PF6 ] exhibited higher enrichment factors and lower salting effect compared with tetrachloromethane. Ultrasound afforded rapid dispersion of microdrops of the extractant and microextraction equilibrium. The developed method was suitable for the enrichment and determination of PAEs in the Yellow River and urban wastewater samples.

关 键 词：分散液-液微萃取 离子液体 酞酸酯 样品前处理 超声波 

分 类 号：O657.7[理学—分析化学]