超声辅助分散液-液微萃取/高效液相色谱联用富集分析环境水样中邻苯二甲酸酯类化合物  

Enrichment and Determination of Phthalates in Environmental Water by Ultrasound Assisted Dispersive Liquid-Liquid Microextraction Coupled with HPLC

作　　者：王青[1] 马维炜[1] 朱琦[1] 薛林科[1] 杜新贞[1,2] 

机构地区：[1]西北师范大学化学化工学院,甘肃兰州730070 [2]甘肃省生物电化学与环境分析重点实验室,甘肃兰州730070

出　　处：《分析测试学报》2013年第5期598-603,共6页Journal of Instrumental Analysis

基　　金：国家自然科学基金项目(21265019)

摘　　要：建立了超声波辅助分散液-液微萃取(DLLME)与高效液相色谱(HPLC)联用对环境水样中痕量邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二(2-乙基己基)酯(DEHP)和邻苯二甲酸二辛酯(DOP)富集分离测定的方法,优化了色谱分离条件,考察了萃取剂与分散剂的种类与用量、萃取时间和离子强度对超声辅助DLLME/HPLC的影响。在优化实验条件下,邻苯二甲酸酯色谱峰面积与其浓度在1.00～100μg.L-1范围内呈良好的线性关系,相关系数均大于0.996,平均加标回收率为91%～103%,相对标准偏差(RSDs,n=5)为2.0%～6.8%,5种邻苯二甲酸酯类化合物的检出限(S/N=3)分别为0.08、0.04、0.03、0.01、0.07μg.L-1。建立的方法用于环境水样中邻苯二甲酸酯的测定,平均加标回收率为85%～119%,RSDs(n=3)为2.3%～11.1%。该方法适用于环境水样中痕量邻苯二甲酸酯类化合物的富集分析。A novel method for the enrichment and determination of trace dimethyl phthalate（DMP）,diethyl phthalate（DEP）,di-n-butyl phthalate（DBP）,di（2-ethylhexyl） phthalate（DEHP） and di-n-octyl phthalate（DOP） in environmental water by ultrasound assisted dispersive liquid-liquid microextraction（DLLME） combined with high performance liquid chromatography（HPLC） was established.Experimental conditions of chromatographic separation and DLLME such as type and volume of extractants and disperser solvents,ultrasonic microextraction time and ionic strength were examined.Under the optimized conditions,the chromatographic peak areas were proportional to the concentrations of phthalates in the range of 1.00-100 μg/L with correlation coefficients more than 0.996.The average recoveries were in the range of 91%-103% with relative standard deviations（RSDs,n=5） of 2.0%-6.8% for the water sample at a spiked level of 20.0 μg·L-1.The limits of detection were 0.08,0.04,0.03,0.01,0.07 μg·L-1,respectively.This method was applied in the enrichment and determination of 5 phthalates in the real water samples with average recoveries of 85%-119% and RSDs（n=3） of 2.3%-11.1%.The developed procedure is suitable for the enrichment and determination of trace phthalates in different real environmental water samples.

关 键 词：分散液-液微萃取 高效液相色谱 邻苯二甲酸酯 富集 样品前处理 

分 类 号：O657.72[理学—分析化学] TQ414.1[理学—化学]