两种离子液体-分散液液微萃取方法富集水中4种胺类化合物的比较  

Comparison of Two Ionic Liquid Dispersive Liquid-Liquid Microextraction Approaches for Determination of Acrylamide,Caprolactam,Benzidine and Aniline in Water

作　　者：徐能斌[1] 冯加永[1] 朱丽波[1] 钱飞中[1] 徐立红 陈钟佺[1] 汪晟乐[1] 

机构地区：[1]宁波市环境监测中心,宁波315012 [2]绍兴市环境监测中心,绍兴312000

出　　处：《分析化学》2016年第1期117-123,共7页Chinese Journal of Analytical Chemistry

基　　金：国家高技术研究发展计划(No.2011AA060603);环保部科研公益性行业专项(No.201209016);宁波市自然科学基金(No.2011A610087)资助~~

摘　　要：建立了温度控制/超声辅助-离子液体-分散液液微萃取-超高效液相色谱-串联质谱检测水中4种胺类化合物的方法,并对两种前处理方法的优化参数进行了详细比较,最终证明超声辅助方法具有更高的回收率。水样在调节pH之后加入[C8MIM][PF6]和乙腈,通过水浴控温/超声辅助的方法促进萃取,冷却后离心分离,即可进入超高效液相色谱串联质谱检测。超声辅助方法中,4种胺类物质线性良好,相关系数范围在0.9969-0.9991,检出限范围为5.0-50 ng/L。在3个浓度水平6次平行加标实验中,4种胺类物质平均回收率为81.5%-106.9%。日内相对标准偏差和日间相对标准偏差分别为7.6%-15.7%和14.7%-22.9%。本方法操作简便,灵敏度高,适用于大批量样品的快速分析。A comparative study of the performance of ultrasound-assisted（UA）,and temperature-controlled（TC） ionic liquid（IL） dispersive liquid-liquid microextraction（IL-DLLME） was presented.Various parameters that affected extraction efficiency were evaluated.UA-IL-DLLME was found to provide the better extraction efficiency.After adjustment of pH,the water sample was mixed with[C8MIM][PF6]and acetonitrile,then was extracted under ultrasound-assisted/temperature-controlled conditions.The mixture was then centrifuged,separated,and analyzed by UPLC-MS/MS.Under the optimal conditions,the calibration curves were linear well with correlation coefficient ranged from 0.9969-0.9991,and the limits of detection of acrylamide,caprolactam,aniline and benzidine were in the range of 5.0-50 ng/L.At the spiked levels of three concentrations,the average recoveries were between 81.5%and 106.9%.The relative standard deviations of run-to-run and day-to-day were 7.6%-15.7%and 14.7%-22.9%,respectively.The developed method is simple and sensitive,and was suitable for rapid analysis of large quantities of samples.

关 键 词：丙烯酰胺 己内酰胺 联苯胺 苯胺 超高效液相色谱-质谱法 分散液液微萃取 离子液体 超声辅助 

分 类 号：O657.63[理学—分析化学] X832[理学—化学]