固相萃取-液相色谱-串联四极杆质谱法测定地表水中22种全氟和多氟烷基类化合物

唐诗; 孙涛; 孙攀; 陈杰

doi:10.13205/j.hjgc.202604002

固相萃取-液相色谱-串联四极杆质谱法测定地表水中22种全氟和多氟烷基类化合物

doi: 10.13205/j.hjgc.202604002

唐诗¹,
孙涛^2, ,,
孙攀¹,
陈杰¹

1. 河南省郑州生态环境监测中心, 郑州 450007;
2. 北京师范大学环境学院, 北京 100875

基金项目:

国家自然科学基金山东联合基金重点项目“黄河三角洲盐沼湿地退化与生态保护机制研究”（U1806217）

详细信息

作者简介:
唐诗(1989—),女,工程师,主要研究方向为环境监测。tangshi89@163.com

通讯作者:
孙涛(1975—),男,教授,主要研究方向为生态需水。Suntao@bnu.edu.cn

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出版历程
- 收稿日期: 2025-12-10
- 网络出版日期: 2026-06-06
- 刊出日期: 2026-04-01

Determination of 22 per- and polyfluoroalkyl substances in surface water by solid-phase extraction with ultra-high performance liquid chromatography-tandem mass spectrometry

TANG Shi¹,
SUN Tao^{2
, ,},
SUN Pan¹,
CHEN Jie¹

1. Zhengzhou Ecological Environment Monitoring Center of Henan Province, Zhengzhou 450007, China;
2. School of Environment, Beijing Normal University, Beijing 100875, China

摘要

摘要: 建立了一种基于超高效液相色谱-串联四极杆质谱（UHPLC-MS/MS）联用技术，用于测定地表水中22种全/多氟烷基类化合物（PFAS）的分析方法。该方法增设了颗粒物甲醇提取环节：将水样过滤后，对截留的颗粒物用甲醇提取，再将颗粒物甲醇提取液与水样滤液合并，实现对“溶解态-颗粒态”两相中PFAS的高效捕获。样品经弱阴离子交换（WAX）固相萃取（SPE）柱富集和净化后，洗脱液经氮吹浓缩，用甲醇/水（体积比为8∶2）复溶、过滤，随后进样至UHPLC-MS/MS系统进行分离和检测，并采用同位素内标法定量分析。结果表明，该方法在1~250 μg/L的浓度范围内线性关系良好（R²>0.995）；水样中各目标化合物的方法检出限为0.2~0.6 ng/L，方法定量限为0.8~2.4 ng/L；在空白水基质和地表水基质中，目标化合物的回收率分别为85.3%~139%和76.4%~127%，且相对标准偏差（RSD，n=6）均<15%。与未提取颗粒态PFAS的传统方法相比，该方法对地表水基质中目标化合物的回收率具有显著优势。结果表明，所开发的方法灵敏、准确、可靠，其通过增设甲醇提取步骤可有效消除颗粒吸附导致的负偏差，显著提高PFAS的回收率，适用于环境地表水基质中22种常见PFAS的定量筛查。
- 超高效液相色谱串联四极杆质谱 /
- 全/多氟烷基类化合物 /
- 固相萃取 /
- 颗粒态全/多氟烷基类化合物
Abstract: A method for the determination of 22 per- and polyfluoroalkyl substances （PFAS） by ultra-high performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） was developed. The optimized method involves extracting particulate matter from filtered water samples with methanol， followed by combining the particulate methanol extract with the filtrate， thereby enabling efficient capture of PFAS from both dissolved and particulate phases. The samples were concentrated and purified using weak anion exchange （WAX） solid-phase extraction （SPE） columns. After nitrogen blowing， the residue was reconstituted in methanol/water （V/V=8∶2） and filtered prior to analysis by mass spectrometry， with quantification performed via the isotope internal standard method. The linear correlation coefficients （R²） of the standard curves for the 22 PFAS were all greater than 0.995， with linear ranges of 1 to 100 µg/L， detection limits of 0.2 to 0.6 ng/L， and quantification limits of 0.8 to 24 ng/L. The recovery rates of the 22 PFAS in blank water and surface water ranged from 85.3% to 139% and 76.4% to 127%， respectively， with relative standard deviations （RSD） of less than 15% （n=6）. Compared with the methods that do not involve the extraction of particulate PFAS， this method exhibited distinct advantages in the recovery rates of the 22 PFAS in surface water. These results demonstrate that the developed method is sensitive， accurate， and reliable. The incorporation of a methanol extraction step can effectively eliminate the negative bias induced by particulate adsorption， thus significantly enhancing the recovery of PFAS. This method is suitable for the quantitative determination of 22 common PFAS in surface water.

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