离子液体分散液-液微萃取-高效液相色谱法测定酞酸酯类化合物  

Determination of phthalates by ionic liquid dispersive liquid-liquid microextraction-high performance liquid chromatography

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

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

出　　处：《西北师范大学学报（自然科学版）》2013年第3期66-70,80,共6页Journal of Northwest Normal University(Natural Science)

基　　金：国家自然科学基金资助项目(21265019)

摘　　要：以疏水性离子液体1-辛基-3-甲基咪唑六氟磷酸盐([OMIm]PF6)为萃取剂,甲醇为分散剂,采用新型的超声波辅助(USA)分散液-液微萃取(DLLME)与高效液相色谱(HPLC)联用对黄河水样和城市生活污水水样中痕量邻苯二甲酸二乙酯(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)进行了富集分离和测定,优化了萃取条件.在1.00～500μg.L-1范围内色谱峰面积与酞酸酯(PAEs)浓度成良好的线性关系(R>0.995 0);对于10.0μg.L-1加标混合样品,平均加标回收率在88.2%～91.8%,相对标准偏差在3.12%～6.70%之间(n=5),检出限(S/N=3)在0.01～0.07μg.L-1范围内.建立的方法应用于黄河水样和城市生活污水水样中酞酸酯类化合物(PAEs)的富集与分析,实验结果具有良好的精密度和准确度.A novel procedure for the enrichment and determination of trace diethyl phthalate（DEP）,di-n-butyl phthalate（DBP）,di（2-ethyl-hexyl）phthalate（DEHP） and di-n-octyl phthalate（DOP） in environmental water by ultrasound-assisted（USA） dispersive liquid-liquid microextraction（DLLME） coupled with high performance liquid chromatography（HPLC） is established using 1-octyl-3-methylimidazolium hexafluorophosphate as an extractant solvent and methanol as a disperser solvent.Experimental conditions such as chromatographic separation and DLLME（species and volume of extractants and disperser solvents,ultrasonic microextraction time and ionic strength）are examined.Under the optimized conditions,the chromatographic peak area is proportional to their individual concentration in the range 1.00～500 μg·L-1（R0.995）.The average recoveries are 88.2%～91.8% for 10.0 μg·L-1 and the relative standard deviations（RSD） 2.01%～6.76%（n=5）.The limits of detection are within 0.01～0.07 μg·L-1.The developed method is successfully applied to the enrichment and determination of 4 phthalates in the Yellow River and urban wastewater samples.Satisfactory recovery,good precision and high sensitivity are achieved for analytical results.

关 键 词：分散液-液微萃取 离子液体 酞酸酯 超声波 

分 类 号：X132[环境科学与工程—环境科学]