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在线固相萃取液质联用法测定饮用水源中的痕量联苯胺
引用本文:张雁, 何咏, 王莹, 朱慧敏. 在线固相萃取液质联用法测定饮用水源中的痕量联苯胺[J]. 环境工程学报, 2016, 10(8): 4590-4594. doi: 10.12030/j.cjee.201503037
作者姓名:张雁  何咏  王莹  朱慧敏
作者单位:1.北京市环境保护科学研究院, 国家城市环境污染控制工程技术研究中心, 北京 100037
摘    要:建立了在线固相萃取液相色谱串联质谱法测定水中痕量联苯胺的方法。样品经自动进样器注入在线固相萃取小柱后,用富集泵流动相实现对样品的富集洗脱,然后用分析泵流动相将样品从富集柱冲洗至色谱柱后用串联质谱仪进行检测。该方法可在11 min内自动完成对样品的富集、净化、进样和检测过程。当进样量为5 mL时,联苯胺在0.010~2.0 μg·L-1范围内具有良好的线性关系,相关系数R为0.999,检出限为0.8 ng·L-1,实际水样的回收率为85%~104%。该方法具有简单、快速、重现性好、灵敏高等特点,可用于环境水体中痕量联苯胺的检测。

关 键 词:联苯胺   在线固相萃取   超高效液相色谱串联质谱法   饮用水
收稿时间:2015-03-25

On-line SPE coupled with UPLC-MS/MS for determination of trace benzidine in drinking water
ZHANG Yan, HE Yong, WANG Ying, ZHU Huimin. On-line SPE coupled with UPLC-MS/MS for determination of trace benzidine in drinking water[J]. Chinese Journal of Environmental Engineering, 2016, 10(8): 4590-4594. doi: 10.12030/j.cjee.201503037
Authors:ZHANG Yan  HE Yong  WANG Ying  ZHU Huimin
Affiliation:1.Beijing Municipal Research Institute of Environmental Protection, National Engineering Techniques Research Center of Urban Environmental Pollution Control, Beijing 100037, China
Abstract:An analytical method based on on-line solid phase extraction (SPE) coupled with liquid chromatography-tandem mass spectrometry for determination of benzidine in drinking water was developed. A sample was loaded in the on-line SPE column via the auto sampler. After enrichment and purification by the mobile phase of the trapping pump, the sample was flushed from the SPE column to the analyzing column by the mobile phase of the analyzing pump. The detection was completed by tandem mass spectrometry. The concentration, purification, sampling, and detection progress were completed automatically within 11 min. A good linear relationship within 0.010 to 2.0 μg·L-1 was obtained when the sample volume was 5 mL, with a correlation coefficient of 0.999 and detection limit of 0.8 ng·L-1. Satisfactory recovery of the blank spike sample ranged from 85% to 104%. The method proposed by this paper is simple and rapid, possesses high sensitivity and good reproducibility, and can be used to detect trace benzidine in water.
Keywords:benzidine  on-line solid phase extraction  ultra performance liquid chromatography-tandem mass spectrometry  drinking water
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