超高效液相色谱-串联质谱法测定表层水中全氟及多氟化合物

引用本文: 刘晓雷, 刘婕, 郭睿, 赵兴茹, 申金山. 超高效液相色谱-串联质谱法测定表层水中全氟及多氟化合物[J]. 分析化学, 2018, 46(9): 1400-1407. doi: 10.11895/j.issn.0253-3820.171373 shu

Citation: LIU Xiao-Lei, LIU Jie, GUO Rui, ZHAO Xing-Ru, SHEN Jin-Shan. Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry for Determination of Per-and Polyfluorinated Compounds in Surface Water[J]. Chinese Journal of Analytical Chemistry, 2018, 46(9): 1400-1407. doi: 10.11895/j.issn.0253-3820.171373 shu

超高效液相色谱-串联质谱法测定表层水中全氟及多氟化合物

1.
河北师范大学, 化学与材料科学学院, 河北, 石家庄 050024;
2.
中国环境科学研究院, 国家环境保护饮用水水源地环境保护重点实验室, 北京 100012
基金项目:
本文系国家自然科学基金项目（No.21607145）和中央级公益性科研院所基本科研业务专项（No.YJ-2009ZX07527-007-5-1）资助

摘要: 建立了固相萃取-超高效液相色谱-串联质谱（SPE-UPLC-MS/MS）同时测定水中全氟烷基羧酸（PFCAs）、全氟烷基磺酸（PFSAs）、全氟烷基膦酸（PFPAs）、全氟烷基次膦酸（PFPis）和多氟烷基膦酸二酯（diPAPs）等23种全氟及多氟化合物的分析方法。固相萃取柱WAX柱依次用6 mL甲醇（含1%（V/V）NH₄OH）、12 mL甲醇和12 mL超纯水活化，上样后，用6 mL乙腈（含0.5%（V/V）NH₄OH）、6 mL甲醇（含1%（V/V）NH₄OH）和6 mL乙腈（含1%（V/V）NH₄OH）洗脱。样品萃取液分为3份，一份用于分析PFCAs和PFSAs，溶液组成为等体积萃取液与超纯水；一份用于分析PFPAs，溶液组成为等体积萃取液与25 mmol/L四丁基硫酸氢铵；另一份用于分析PFPis和diPAPs，溶液组成为甲醇。结果表明，水中23种全氟及多氟化合物平均加标回收率为55%~125%，相对标准偏差为0.3%~15.0%，方法检出限和定量限分别为0.003~0.215 ng/L和0.010~0.714 ng/L。本方法简便、灵敏度高、重现性好，适用于同时检测水中多类全氟及多氟化合物。

关键词:

English

Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry for Determination of Per-and Polyfluorinated Compounds in Surface Water

1.
College of Chemistry and Material Science, Hebei Normal University, Shijiazhang 050024, China;
2.
State Environmental Protection Key Laboratory of Drinking Water Source Protection, Chinese Research Academy of Environmental Sciences, Beijing 100012, China
Received Date: 26 October 2017
Revised Date: 16 July 2018
Fund Project:
This work was supported by the National Natural Science Foundation of China (No. 21607145) and the Basal Research Special of Central Public Interest Scientific Institution (No. YJ-2009ZX07527-007-5-1).

Abstract: A method for simultaneous determination of perfluoroalkyl carboxylic acids (PFCAs), perfluoroalkyl sulfonic acids (PFSAs), perfluoroalkyl phosphonic acids (PFPAs), perfluoroalkyl phosphinic acids (PFPis) and polyfluoroalkyl phosphoric acid diesters (diPAPs) from water by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS) was established. During solid phase extraction process, 6 mL of ammonia-methanol (1.0%, V/V), 12 mL of methanol, 12 mL of ultrapure water were used to activate the WAX cartridges. After sample loading, the cartridges were eluted with 6 mL of ammonia-acetonitrile (0.5%, V/V), 6 mL of ammonia-methanol (1.0%, V/V) and 6 mL ammonia-acetonitrile (1.0%, V/V). Before instrumental analysis, the sample extract was divided into three parts. For the PFCAs and PFSAs, equal parts of ultrapure water were added to the extract. For the PFPAs, equal parts of 25 mmol/L of tetra-butyl ammonium sulfate were added to the extract. For the PFPis and diPAPs, the solution was methanol. The results showed that the recoveries of target compounds were between 55%-125% with relative standard deviation varying from 0.30% to 15%. Method detection limit and quantitative limit were 0.003-0.215 ng/L and 0.01-0.714 ng/L, respectively. This method was simple with high sensitivity and good reproducibility, and suitable for simultaneous determination of five kinds of per-and polyfluorinated substances in water.

Key words:

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沈阳化工大学材料科学与工程学院沈阳 110142

超高效液相色谱-串联质谱法测定表层水中全氟及多氟化合物

English

Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry for Determination of Per-and Polyfluorinated Compounds in Surface Water

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

超高效液相色谱-串联质谱法测定表层水中全氟及多氟化合物

English

Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry for Determination of Per-and Polyfluorinated Compounds in Surface Water

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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