色谱

色谱 ›› 2014, Vol. 32 ›› Issue (5): 529-534.DOI: 10.3724/SP.J.1123.2013.12043

• 技术与应用 • 上一篇    下一篇

液相色谱-串联质谱法测定污水处理厂水样中双酚A、四溴双酚A及烷基酚类化合物

丁洁1,2, 张圣虎1, 刘济宁1, 周林军1, 陈国松2, 石利利1   

  1. 1. 环境保护部南京环境科学研究所, 江苏 南京 210042;
    2. 南京工业大学理学院, 江苏 南京 210009
  • 收稿日期:2013-12-31 修回日期:2014-03-05 出版日期:2014-05-08 发布日期:2014-04-26
  • 通讯作者: 刘济宁
  • 基金资助:

    国家高技术研究发展计划（“863”计划）项目（2013AA06A308）；环保公益性行业科研专项（201309028）.

Determination of bisphenol A, tetrabromobisphenol A and alkylphenols in water samples of sewage treatment plant using liquid chromatography-tandem mass spectrometry

DING Jie1,2, ZHANG Shenghu1, LIU Jining1, ZHOU Linjun1, CHEN Guosong2, SHI Lili1   

  1. 1. Nanjing Institute of Environmental Sciences, Ministry of Environmental Protection, Nanjing 210042, China;
    2. College of Sciences Nanjing Tech University, Nanjing 210009, China
  • Received:2013-12-31 Revised:2014-03-05 Online:2014-05-08 Published:2014-04-26

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399

被引次数

39

摘要：

近年来，双酚A、四溴双酚A及烷基酚类化合物由于其对水生生物的内分泌干扰作用受到越来越广泛的关注。污水处理厂是处理这类化合物的重要途径，研究目标物在其中的浓度分布对于探明此类物质在环境中的暴露水平具有重要意义，而建立相应的分析测定方法则是开展上述研究的基础。本研究建立了同时测定污水处理厂水样中双酚A、四溴双酚A及6种烷基酚类化合物的反相液相色谱-电喷雾串联质谱分析方法。结果发现，以ZORBAX Eclipse Plus C18色谱柱（150 mm×2.1 mm，3.5 μm）为分离柱，乙腈和0.02%（v/v）氨水溶液为梯度洗脱的流动相，电喷雾质谱负离子模式下目标化合物在11 min内分离；在1~100 μg/L范围内，双酚A、四溴双酚A及6种烷基酚类化合物的峰面积与质量浓度的线性关系良好（R2≥0.998），方法定量限为2.0~20 ng/L；添加水平分别为0.2、2、20 μg/L时，目标化合物的平均回收率分别为64.3%~118.0%、65.9%~100.5%、70.3%~102.7%，相对标准偏差均小于7.1%。基于上述方法，对江苏省某工业园区污水处理厂水样中相关物质进行检测，出水中检出5种目标化合物，质量浓度范围为11.9~3015.3 ng/L。结果表明，该方法准确可靠、灵敏度高，适用于污水处理厂水样中相关烷基酚类化合物的检测。

关键词: 双酚A, 水样, 四溴双酚A, 烷基酚类, 污水处理厂, 液相色谱-串联质谱

Abstract:

Bisphenol A, tetrabromobisphenol A and alkylphenols have received much attention in recent years because of their endocrine disrupting effects to aquatic ecosystem. The fate of these compounds in sewage treatment plant which is important to deal with this kind of compounds has significance on the study of exposure levels of the target compounds in the environment, and the development of analytical method is the basis on the above study. An analytical method based on liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) with negative ionization mode has been developed for measuring bisphenol A, tetrabromobisphenol A and six alkylphenols in raw and treated sewage samples. The target compounds were separated on a ZORBAX Eclipse Plus C18 column (150 mm×2.1 mm, 3.5 μm) with mobile phases of acetonitril and 0.02% (v/v) ammonia. Analyte confirmations were performed under multiple reaction monitoring (MRM) mode and the eight compounds were separated within 11 min. The calibration curves were linear in the range of 1-100 μg/L (R2≥0.998). The quantification limits of the eight compounds were 2.0-20 ng/L. The recovery experiments were performed with samples spiked at the levels of 0.2, 2 and 20 μg/L, and the recoveries for the target compounds were in the range of 64.3%-118.0%, 65.9%-100.5% and 70.3%-102.7% (RSD<7.1%, n=3), respectively. Based on the analytical method, the raw and treated sewage samples from an industrial park of Jiangsu Province were analyzed. Five compounds were detected in the water outlet in the range of 11.9-3015.3 ng/L. It shows that the method is simple, selective, sensitive and can be used to analyze the water samples of sewage treatment plant containing alkylphenols.

Key words: alkylphenols, bisphenol A, liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), sewage treatment plant (STP), tetrabromobisphenol A, water sample

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