高等学校化学学报 ›› 2018, Vol. 39 ›› Issue (9): 1934.doi: 10.7503/cjcu20180026

• 分析化学 • 上一篇    下一篇

微波辅助离子液体分散液-液微萃取DART-Orbitrap质谱法测定环境水中的溴代阻燃剂

苏蕊1(), 汪亿晗1, 陈长宝1, 孙秀丽1, 刘淑莹1,2, 杨洪梅1()   

  1. 1.长春中医药大学吉林省人参科学研究院, 长春 130117
    2.中国科学院长春应用化学研究所, 长春 130022
  • 收稿日期:2018-01-09 出版日期:2018-09-07 发布日期:2018-06-04
  • 作者简介:

    联系人简介: 苏 蕊, 女, 博士, 副研究员, 主要从事复杂基质的质谱分析研究. E-mail: sranalchem@163.com; 杨洪梅, 女, 博士, 副研究员, 博士生导师, 主要从事质谱分析研究. E-mail: yanghm@sina.cn

  • 基金资助:
    吉林省科技厅重点科技攻关项目(批准号: 20160204027YY, 201603080YY, 201603003YY, 20170307028YY)资助.

Determination of Brominated Flame Retardants in Environmental Water by Microwave-assisted Ionic Liquid/ionic Liquid Dispersive Liquid-liquid Microextraction Coupled with DART-Orbitrap Mass Spectrometry

SU Rui1,*(), WANG Yihan1, CHEN Changbao1, SUN Xiuli1, LIU Shuying1,2, YANG Hongmei1,*()   

  1. 1. Jilin Ginseng Academy, Changchun University of Chinese Medicine, Changchun 130117, China
    2. Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, China
  • Received:2018-01-09 Online:2018-09-07 Published:2018-06-04
  • Contact: SU Rui,YANG Hongmei E-mail:sranalchem@163.com;yanghm@sina.cn
  • Supported by:
    ? Supported by the Project of Science and Technology Department of Jilin Province, China(Nos. 20160204027YY, 201603080YY, 20170307028YY, 201603003YY).

摘要:

采用微波辅助离子液体分散液-液微萃取(MA-IL/IL-DLLME)的方法提取了环境水样品中的溴代阻燃剂(BFRs), 以[C6MIM][PF6]为萃取剂, [C4MIM][BF4]为分散剂, 辅以微波照射, 在短时间内获得较高提取效率, 并结合DART串联高分辨静电场轨道阱质谱仪(DART-Orbitrap MS)对环境水中的BFRs进行测定, 建立了一种快速、 灵敏、 简便且准确测定环境水中BFRs的方法. 通过对BFRs萃取条件及DART离子源参数进行优化, 获得了最优实验条件. 为进一步明确BRFs在DART-MS中的气相离子反应特征, 讨论了5种BFRs的特征离子信息, 确定了目标离子, 明确了发生机理. 实验结果表明, 采用MA-IL/IL-DLLME萃取水样中的BFRs能够有效提高方法的灵敏度, 结合DART离子源的耐盐效应, 可将离子液体应用于质谱测定的同时, 解决DART离子源灵敏度低的难题. 在最优实验条件下, 对环境水样进行分析, 方法的回收率为80.7%~107%, RSD≤10.2%, 检出限为0.212~1.82 μg/L.

关键词: 微波辅助离子液体分散液-液微萃取, DART串联高分辨静电场轨道阱质谱仪, 溴代阻燃剂, 快速检测, 环境水

Abstract:

A new method termed microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction coupled with DART-Orbitrap mass spectrometry(MA-IL/IL-DLLME) was developed for the determination of selected five brominated flame retardants(BFRs) in environmental water. Instead of using hazardous organic solvents, two kinds of ionic liquids(ILs), hydrophobic IL([C6MIM][PF6]) and hydrophilic IL([C4MIM][BF4]), were used as extraction solvent and dispersion agent, respectively, in this method. In the extraction procedure, BFRs were extracted entirely into the [C6MIM][PF6] from environmental water samples with the help of [C4MIM][BF4]. After extraction, IL phase containing analytes was analyzed by direct analysis in real time-mass spectrometry(DART-MS). Several experimental parameters that might affect the extraction efficiency were investigated and optimized. Under the optimized experimental conditions, low limits of detection(LODs, 0.212—1.82 μg/L) were obtained. The present method also provides good recoveries(80.7%—107%) and acceptable precision(RSDs<10.2%). In addition, the negative ionization characteristics of 5 different BFRs were investigated using DART-Orbitrap MS. The experimental results demonstrated that the developed method contains the advantages including easy-to-use, high speed and high sensitivity for the analysis of BFRs in environmental water samples, showing potential application in the environmental science and environment pollution protection.

Key words: Microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction, DART-Orbitrap MS, Brominated flame retardant, Rapid detection, Environmental water

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