地学前缘 ›› 2019, Vol. 26 ›› Issue (4): 307-314.DOI: 10.13745/j.esf.sf.2019.5.32

• 非主题来稿选登 • 上一篇    

超高效液相色谱串联质谱法快速测定地下水和含水层介质中16种全氟烷基酸

刘明睿，汪伶俐，陈亮   

  1. 1. 天津大学 建筑工程学院; 水利工程仿真与安全国家重点实验室, 天津 300354
    2. 中矿(天津) 盐矿检测有限公司, 天津 300450
    3. 天津大学 环境工程与科学学院, 天津 300354
  • 收稿日期:2019-02-02 修回日期:2019-03-01 出版日期:2019-07-25 发布日期:2019-07-25
  • 通信作者: 陈亮(1985—)，男，博士，长期从事水环境污染与治理的教学与科研工作。
  • 作者简介:刘明睿(1995—)，男，硕士研究生，研究方向为水文、水资源与水生态。
  • 基金资助:
    国家自然科学基金项目“设施农业区地下水系统中赤霉酸降解及其与三氮转化约束机制研究”(41772245)

Quick analysis of sixteen PFAAs in groundwater and aquifer by ultra-performance liquid chromatographytriple quadrupole mass spectrometry

LIU Mingrui,WANG Lingli,CHEN Liang   

  1. 1. School of Civil Engineering, Tianjin University; State Key Laboratory of Hydraulic Engineering Simulation and Safe, Tianjin 300354, China
    2. Sinomine (Tianjin) Rock and Mineral Analysis Co., Ltd., Tianjin 300450, China
    3. School of Environmental Science and Engineering, Tianjin University, Tianjin 300354, China
  • Received:2019-02-02 Revised:2019-03-01 Online:2019-07-25 Published:2019-07-25
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摘要： 全氟烷基酸(PFAAs)是一种新型的持久有机污染物，在各种环境介质中被频繁检出。目前，PFAAs的检测方法主要包括液相色谱串联质谱法(HPLC-MS/MS)、超高效液相色谱串联质谱法(UPLC-MS/MS)、气相色谱法和光谱类方法。但是，上述方法多存在样品前处理过程复杂、周期长、成本高的问题，不适用于PFAAs的快速检测。为此，本文建立了一种快速测量地下水和含水层介质中16种PFAAs的UPLC-MS/MS方法。水样过0.22 μm滤膜后直接测定浓度，土样经过超声离心后，取上清液过滤测量浓度。本方法分别为16种PFAAs建立了低浓度(5~50 μg/L)和高浓度(100~500 μg/L)两条校准曲线，相关系数R2＞0.99。地下水中16种PFAAs快速检测方法检出限为0.06~1.07 μg/L，回收率为75%~120%，精密度(RSD)为2.61%~9.19%(除高浓度时全氟丁烷磺酸和全氟已烷磺酸分别为11.34%和14.70%外)。含水层介质中14种PFAAs(全氟十三酸和全氟十四酸除外)方法检出限为2.69~12.33 ng/g，回收率为65%~103%，精密度(RSD)为1.96%~7.22%。

 

关键词: 全氟烷基羧酸, 全氟烷基磺酸, 水, 土壤, 液相色谱质谱

Abstract: Perfluorinated alkyl acids (PFAAs) are a group of emerging persistent organic pollutant that have received increasing attention due to their global occurrence, accumulation and toxicity. At present, PFAA detection mainly uses high-performance liquid chromatographytandem mass spectrometry (HPLC-MS/MS), ultra-performance liquid chromatographytandem mass spectrometry (UPLC-MS/MS), gas chromatography (GC) and spectroscopy. However, these detection methods often involve complicated sample pretreatment, longer work cycle and higher cost, therefore, they are not suitable for quick PFAA detection. In this study, we developed a method for quick analysis of 16 PFAAs in groundwater and aquifer based on UPLC-MS/MS. In the experiment, the groundwater sample was filtered through 0.22 μm membrane and injected directly into the detection instrument; the aquifer sample was prepared by liquid solvent extraction. A good linear calibration using 16 PFAAs standards was achieved (R2>0.99) in the low and high concentration ranges of 550 and 100500 μg/L, respectively. The method’s detection limits (MDLs) of 16 PFAAs in groundwater were 0.061.07 μg/L, and the recovery rates were 75%120% with relative standard deviations (RSD) at 2.61%9.19%. In aquifer media, MDLs of 14 PFAAs were 2.6912.33 ng/L, and the recovery rates were 65%103% with RSDs at 1.96%7.22%.

Key words: perfluoroalkyl carboxylic acid (PFCA), perfluoroalkyl sulfonic acid (PFSA), water, soil, liquid chromatographytandem mass spectrometry

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