色谱

色谱 ›› 2014, Vol. 32 ›› Issue (9): 919-925.DOI: 10.3724/SP.J.1123.2014.05024

• 特别策划：新型污染物色谱分析专栏 • 上一篇    下一篇

固相萃取-液相色谱-串联质谱法同时测定水中14种短链和长链全氟化合物

王超1, 吕怡兵1, 陈海君2, 谭丽1, 滕恩江1   

  1. 1. 中国环境监测总站, 北京 100012;
    2. 环境保护部环境保护对外合作中心, 北京 100035
  • 收稿日期:2014-05-22 修回日期:2014-07-01 出版日期:2014-09-08 发布日期:2014-08-30
  • 通讯作者: 王超
  • 作者简介:王超，preparing@126.com.
  • 基金资助:

    国家高技术研究发展计划（“863”计划）项目（2013AA06A308）.

Simultaneous analysis of 14 short- and long-chain perfluorinated compounds in water by liquid chromatography-tandem mass spectrometry using solid phase extraction

WANG Chao1, LÜ Yibing1, CHEN Haijun2, TAN Li1, TENG Enjiang1   

  1. 1. China National Environmental Monitoring Center, Beijing 100012, China;
    2. Foreign Economic Cooperation Office, Ministry of Environmental Protection, Beijing 100035, China
  • Received:2014-05-22 Revised:2014-07-01 Online:2014-09-08 Published:2014-08-30

PDF

476

被引次数

19

摘要：

建立了固相萃取-超高压液相色谱-三重四极杆质谱同时测定水中14种短链和长链全氟化合物（PFCs）的方法。水样经WAX混合型固相萃取小柱富集和净化后，采用BEH C18色谱柱、甲醇和5 mmol/L乙酸铵水溶液作为流动相进行梯度洗脱，质谱采用多反应监测模式，内标法定量分析。14种PFCs在0.1~50 μg/L范围内线性关系良好，相关系数大于0.99，方法检出限和定量限分别为0.09~1.15 ng/L和0.29~3.85 ng/L。在2、10和20 ng/L加标水平下，8种PFCs的平均回收率为85.0%、120.2%和117.4%，平均相对标准偏差为9.2%、9.0%和6.6%，6种PFCs的回收率相对较低，主要由于其在瓶/管壁上的吸附作用导致。应用本方法分析某淡水湖水样，检出4种短链和5种长链PFCs，质量浓度为41.29~49.05 ng/L和98.43~111.02 ng/L。结果表明该方法适用于对环境水体中短链和长链PFCs的同时分析测定。

关键词: 固相萃取, 全氟化合物, 水, 液相色谱-串联质谱

Abstract:

A solid phase extraction (SPE)-ultrahigh pressure liquid chromatography (UPLC) method coupled with tandem mass spectrometry was developed for the simultaneous analysis of the 14 short- and long-chain perfluorinated compounds (PFCs) in water. Water sample was concentrated and purified through WAX mixed-mode SPE cartridges. The separation of PFCs was performed on a BEH C18 column with gradient elution using methanol-5 mmol/L ammonium acetate as mobile phases. The PFCs were quantified by internal standard method in multiple-reaction monitoring mode. The calibration curves of the 14 PFCs were linear in the range of 0.1-50 μg/L with the correlation coefficients > 0.99. The limits of detection (S/N=3) and quantitation (S/N=10) of the method were 0.09-1.15 ng/L and 0.29-3.85 ng/L, respectively. The average recoveries of eight PFCs at three spiked levels of 2, 10 and 20 ng/L were 85.0%, 120.2% and 117.4%, with the relative standard deviations of 9.2%, 9.0% and 6.6%, respectively. The recoveries of the rest six PFCs were low due to unavoidable strong adsorption on the bottle/tube walls during sample pretreatment. The method was applied in the determination of PFCs in real samples of a lake in South China. Four short-chain and five long-chain PFCs were detected with mass concentrations of 41.29-49.05 ng/L and 98.43-111.02 ng/L, respectively. The results show that the method is suitable for the simultaneous analysis of short- and long-chain perfluorinated compounds in environmental water.

Key words: liquid chromatography-tandem mass spectrometry (LC-MS/MS), perfluorinated compounds, solid phase extraction, water

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