色谱

色谱 ›› 2014, Vol. 32 ›› Issue (5): 472-476.DOI: 10.3724/SP.J.1123.2014.01042

• 研究论文 • 上一篇    下一篇

固相萃取-超高效液相色谱-电喷雾串联质谱法同时测定地表水中16种全氟有机化合物

张明, 唐访良, 俞雅雲, 陈峰, 徐建芬, 叶永根   

  1. 杭州市环境监测中心站, 浙江 杭州 310007
  • 收稿日期:2014-01-24 修回日期:2014-03-27 出版日期:2014-05-08 发布日期:2014-04-26
  • 通讯作者: 唐访良
  • 基金资助:

    杭州市社会发展科研攻关项目（20130533B02）；杭州市环境保护科技项目（2013HZHB002）.

Simultaneous determination of sixteen perfluorinated organic compounds in surface water by solid phase extraction and ultra performance liquid chromatography with electrospray ionization tandem mass spectrometry

ZHANG Ming, TANG Fangliang, YU Yayun, CHEN Feng, XU Jianfen, YE Yonggen   

  1. Hangzhou Environmental Monitoring Central Station, Hangzhou 310007, China
  • Received:2014-01-24 Revised:2014-03-27 Online:2014-05-08 Published:2014-04-26

PDF

432

被引次数

17

摘要：

建立了固相萃取-超高效液相色谱-电喷雾串联三重四极杆质谱联用技术分析水中16种全氟有机化合物的高通量检测方法。样品经WAX固相萃取柱富集和净化后，采用Waters ACQUITY UPLCTM BEH C18色谱柱，含2 mmol/L乙酸铵的甲醇和含2 mmol/L乙酸铵的水作为流动相进行梯度洗脱，质谱采用电喷雾负离子电离，多反应监测模式检测。16种全氟有机化合物在0.5~100 μg/L或1.0~100 μg/L浓度范围内线性关系良好，相关系数为0.9987~0.9999，方法的检出限为0.06~0.46 ng/L；高、中、低3个添加水平的回收率为67.6%~103%，相对标准偏差为2.94%~12.0%。结果表明，该方法灵敏、准确且检测范围广，分析速度快，是一种适于实际水样中全氟有机化合物检测分析的方法。

关键词: 超高效液相色谱, 地表水, 电喷雾串联质谱, 固相萃取, 全氟有机化合物

Abstract:

A high-throughput detection method has been developed for the determination of sixteen perfluorinated organic compounds (PFCs) in surface water by solid phase extraction-ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (SPE-UPLC-ESI-MS/MS). The water samples were concentrated and purified through WAX solid phase extraction cartridges. The UPLC separation was performed on an ACQUITY UPLCTM BEH C18 column utilizing a gradient elution program of methanol (containing 2 mmol/L ammonium acetate) and water (containing 2 mmol/L ammonium acetate) as the mobile phases at a flow rate of 0.4 mL/min. The MS/MS detection was performed under negative electrospray ionization (ESI-) in multiple reaction monitoring (MRM) mode. Good linearities were observed in the range of 0.5-100 μg/L or 1.0-100 μg/L with correlation coefficients from 0.9987 to 0.9999. The limits of detection (LODs) for the sixteen perfluorinated organic compounds were in the range of 0.06-0.46 ng/L. The recoveries ranged from 67.6% to 103% with the relative standard deviations between 2.94% and 12.0%. This method was characterized by high sensitivity and precision, extensive range and high speed, and can be applied for the analysis of PFC contaminants in surface water.

Key words: electrospray ionization tandem mass spectrometry (ESI-MS/MS), perfluorinated organic compounds, solid phase extraction (SPE), surface water, ultra performance liquid chromatography (UPLC)

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