色谱

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液相萃取-高效液相色谱-串联质谱联用测定污泥中的全氟化合物

章涛1, 孙红文1*, ALDER Alfredo C.2, GERECKE Andreas C.3, MLLER Claudia3   

  1. 1. 南开大学环境污染过程与基准教育部重点实验室, 天津 300071; 2. 瑞士联邦水科学与技术研究所, 杜本多夫 8600, 瑞士; 3. 瑞士联邦材料科学与技术研究所, 杜本多夫 8600, 瑞士
  • 收稿日期:2010-01-14 修回日期:2010-02-14 出版日期:2010-05-28 发布日期:1980-09-25
  • 通讯作者: 孙红文

Analysis of perfluorinated compounds in sludge by liquid extraction and high performance liquid chromatography-tandem mass spectrometry

ZHANG Tao1, SUN Hongwen1*, ALDER Alfredo C.2, GERECKE Andreas C.3, MLLER Claudia3   

  1. 1. Key Laboratory of Pollution Processes and Environmental Criteria of Ministry of Education, Nankai University, Tianjin 300071, China; 2. Swiss Federal Institute for Environmental Science and Technology (EAWAG), Dübendorf 8600, Switzerland; 3. Swiss Federal Institute for Materials Science and Technology (EMPA), Dübendorf 8600, Switzerland
  • Received:2010-01-14 Revised:2010-02-14 Online:2010-05-28 Published:1980-09-25
  • Contact: SUN Hongwen

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677

被引次数

41

摘要： 全氟化合物是一种新型持久性有机污染物,污水处理厂是其一个主要污染来源。目前还没有建立起一种统一的污泥样品中全氟化合物的分析方法。本文报道了一种基于液相萃取和高效液相色谱-串联质谱联用技术测定污泥中的7种全氟烷基羧酸及其2种不饱和氟调酸前体物、2种全氟烷基磺酸及其5种磺酰胺衍生物前体物的方法。实验对萃取剂(甲醇)的pH值、超声萃取温度与时间、洗脱剂体积进行了优化,确定了中性溶剂、40 ℃下超声萃取10 min, Envi carbon柱净化的前处理方法,并成功地应用于实际污泥样品中全氟化合物的测定。方法的回收率为74%～141%(不饱和氟调酸除外),线性范围为0.1～20 μg/L (羧酸系列)及0.25～50 μg/L(磺酸系列)内线性关系良好(r2＞0.99),定量限为0.6～30 μg/kg(干重)。内标物质的使用可有效消除环境基质引起的仪器离子抑制现象,使定量更加准确。

关键词: 高效液相色谱-串联质谱, 活性污泥 , 全氟化合物, 液相萃取

Abstract: Perfluorinated compounds are emerging persistent organic pollutants. Wastewater treatment plants are reported to be one of their primary sources. However, a standard analytical method for sludge samples has not been set up. A novel and rapid analytical method based on the liquid extraction, followed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was set up for 7 perfluorocarboxylic acids (PFCAs) and their precursors, 6:2 and 8:2 unsaturated flourotelomer carboxylic acids (FTUCAs), and 2 perfluoroalkyl sulfonates (PFASs) and their precursors, 5 derivates of sulfonamide in sludge. The parameters of methanol extraction, including pH, sonication temperature and time, and eluent volume were optimized. The extraction method was optimized as neutral extraction under sonication at 40 ℃ for 10 min, and it was successfully used for the analysis of perfluorinated compounds in the sludge samples. The linear calibration curves were obtained in the ranges of 0.1~20 μg/L for PFCAs and 6:2/8:2 FTUCA and 0.25~50 μg/L for PFASs and their precusors with linear correlation coefficients larger than 0.99. The recoveries of the target compounds ranged from 74% to 141% (except for FTUCAs) and the limits of quantification ranged from 0.6 to 30 μg/kg (dry weight). The use of internal standards can well correct the ion suppression (or enhancement) induced by co-eluting components present in the sample extracts, and improve the quantitative accuracy.

Key words: activated sludge , high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), perfluorinated compounds, liquid extraction