色谱

色谱 ›› 2014, Vol. 32 ›› Issue (8): 817-821.DOI: 10.3724/SP.J.1123.2014.03045

• 研究论文 • 上一篇    下一篇

羧基化多壁碳纳米管固相萃取-液相色谱-串联质谱法测定环境水体中四溴双酚A和双酚A

寇立娟1,2, 梁荣宁1   

  1. 1. 中国科学院海岸带环境过程与生态修复重点实验室, 山东省海岸带环境过程重点实验室, 中国科学院烟台海岸带研究所, 山东 烟台 264003;
    2. 中国科学院大学, 北京 100049
  • 收稿日期:2014-03-27 修回日期:2014-05-08 出版日期:2014-08-08 发布日期:2014-08-01
  • 通讯作者: 梁荣宁，E-mail：rnliang@yic.ac.cn
  • 基金资助:

    中国科学院人才专项项目（2060299）.

Determination of tetrabromobisphenol A and bisphenol A in environmental water using carboxylated multiwalled carbon nanotubes as sorbent for solid-phase extraction combined with liquid chromatography-tandem mass spectrometry

KOU Lijuan1,2, LIANG Rongning1   

  1. 1. Key Laboratory of Coastal Environmental Processes and Ecological Remediation, Shandong Provincial Key Laboratory of Coastal Environmental Processes, Yantai Institute of Coastal Zone Research, Chinese Academy of Sciences, Yantai 264003, China;
    2. Graduate University of Chinese Academy of Sciences, Beijing 100049, China
  • Received:2014-03-27 Revised:2014-05-08 Online:2014-08-08 Published:2014-08-01

PDF

280

被引次数

19

摘要：

建立了羧基化碳纳米管固相萃取-液相色谱-串联质谱联用检测环境水体中四溴双酚A和双酚A的方法。比较了多壁碳纳米管、C60和羧基化多壁碳纳米管作为固相吸附剂对水体中四溴双酚A和双酚A的吸附效率。固相萃取浓缩后的样品经Thermo Scientific Hypersil C18色谱柱（150 mm×4.6 mm，3 μm）分离，采用串联质谱负离子模式进行检测。结果表明，四溴双酚A和双酚A在0.02~1.0 mg/L范围内具有良好的线性关系（r2≥0.99），空白样品中的检出限（S/N=3）分别为0.04 μg/L和0.2 μg/L。将所建立的方法应用于实际环境水体中四溴双酚A和双酚A的检测，添加回收率在82%~99%之间，精密度小于5.0%，该方法可用于复杂环境样品中痕量四溴双酚A和双酚A的检测。

关键词: 固相萃取, 环境水, 双酚A, 四溴双酚A, 羧基化多壁碳纳米管

Abstract:

A method for the determination of tetrabromobisphenol A and bisphenol A in environmental water using carboxyl-functionalized multiwalled carbon nanotubes as solid-phase extraction sorbent and liquid chromatography-tandem mass spectrometry was established. Comparison of three nanomaterials including multiwalled carbon nanotubes, C60 and carboxyl-functionalized multiwalled carbon nanotubes used as solid-phase extraction sorbents was made. After preconcentration by solid-phase extraction, tetrabromobisphenol A and bisphenol A were separated on a Thermo Scientific Hypersil C18 column (150 mm×4.6 mm, 3 μm) and then detected by tandem mass spectrometry in negative electrospray ionization (ESI) mode. The results showed a good linear response in the concentration range of 0.02-1.0 mg/L for tetrabromobisphenol A and bisphenol A, and the limits of detection (S/N=3) were 0.04 μg/L and 0.2 μg/L for tetrabromobisphenol A and bisphenol A, respectively. The application of the proposed approach has been carried out for the determination of tetrabromobisphenol A and bisphenol A in spiked lake water and sea water samples. The recoveries varied from 82% to 99% with the relative standard deviations below 5.0%. The proposed method can be used for the determination of tetrabromobisphenol A and bisphenol A at trace level in complex environmental samples.

Key words: bisphenol A, carboxyl-functionalized multiwalled carbon nanotubes, environmental water, solid-phase extraction (SPE), tetrabromobisphenol A

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