超高效液相色谱-串联质谱法测定大气细颗粒物中全氟烷基酸及其替代物

引用本文: 张海婧, 谢琳娜, 王秦, 徐春雨, 徐东群, 朱英. 超高效液相色谱-串联质谱法测定大气细颗粒物中全氟烷基酸及其替代物[J]. 分析化学, 2022, 50(4): 623-633. doi: 10.19756/j.issn.0253-3820.201269 shu

Citation: ZHANG Hai-jing, XIE Lin-na, WANG Qin, XU Chun-yu, XU Dong-qun, ZHU Ying. Determination of Perfluoroalkyl Acids and Alternatives in Atmospheric Fine Particles by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2022, 50(4): 623-633. doi: 10.19756/j.issn.0253-3820.201269 shu

超高效液相色谱-串联质谱法测定大气细颗粒物中全氟烷基酸及其替代物

中国疾病预防控制中心环境与健康相关产品安全所, 北京 100021

通讯作者: 徐东群,E-mail:xudq@chinacdc.cn; 朱英,E-mail:zhuying@nieh.chinacdc.cn

基金项目:
2014卫生行业专项项目(No.201402022)资助

摘要: 建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定大气细颗粒物(PM_2.5)中全氟烷基酸(PFAAs)及其全氟辛烷磺酸(PFOS)替代物的方法。将采样后的石英滤膜截取1/2,剪碎后以甲醇作为提取溶剂,在40℃超声提取3次,将提取液合并,离心后将上清液经ENVI Carb固相萃取柱净化,流出液经氮气吹干后,再用0.2 mL甲醇复溶,离心取上清液,在电喷雾负离子模式下,以多反应监测模式采集数据进行定量分析。方法在线性范围内线性关系良好,相关系数均大于0.9980;检测大气PM_2.5中PFAAs及其PFOS替代物的检出限为0.01~0.52 pg/m³,定量限为0.03~1.74 pg/m³,回收率在78.6%~119.3%之间,精密度在1.7%~10.5%之间。将本方法应用于北京市2019年11月份不同污染程度天气下PM_2.5中PFAAs及其PFOS替代物的测定,结果表明,在29份样品中,检出了4种PFAAs,分别为PFOA、PFHp A、PFOS和PFHx A,检出率分别为100%、79.3%、62.1%和58.6%,含量范围分别为1.94~86.9 pg/m³、0.31~4.39 pg/m³、0.29~3.51 pg/m³和0.36~1.69 pg/m³,PFOS替代物均未检出。

关键词:

English

Determination of Perfluoroalkyl Acids and Alternatives in Atmospheric Fine Particles by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

National Institute of Environmental Health, Chinese Center for Disease Control and Prevention, Beijing 100021, China

Corresponding author: XU Dong-qun, ; ZHU Ying,

Received Date: 13 May 2020
Revised Date: 11 March 2022
Fund Project:
Supported by the Public Welfare Research Program of the National Health and Family Planning Commission of China (No. 201402022)

Abstract: A ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method was developed for determination of perfluoroalkyl acids and alternatives of perfluorooctane sulfonate(PFOS) in atmospheric fine particles(PM_2.5).Half of filter was cut into small pieces and extracted by methanol for 3 times at 40℃.The extraction solutions were combined and the supernatant was purified by ENVI-Carb SPE cartridge.The effluent was dried by nitrogen at 40℃, re-dissolved with 0.2 mL of methanol, and centrifuged, and the supernatants were quantitatively analyzed in multiple reactions monitoring mode by mass spectrometry with electro-spray ionization in negative mode.The method showed a good linearity for detection of 22 compounds, with the correlation coefficients of more than 0.9980, the limits of detection of 0.01-0.52 pg/m³, the limits of quantification of 0.03-1.74 pg/m³, the spiked recoveries of 78.6%-119.3% and the relative standard deviations of 1.7%-10.5%.The PFAAs and alternatives of PFOS in PM_2.5 collected in November 2019 in Beijing were determined by the method.Four kinds of PFAAs were detected in 29 samples, including PFOA, PFHp A, PFOS and PFHx A, and the detection rates were 100%, 79.3%, 62.1% and 58.6%, respectively.The concentrations were in the range of 1.94-86.9 pg/m³, 0.31-4.39 pg/m³, 0.29-3.51 pg/m³ and 0.36-1.69 pg/m³, respectively.

Key words:

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超高效液相色谱-串联质谱法测定大气细颗粒物中全氟烷基酸及其替代物

通讯作者: 徐东群,E-mail:xudq@chinacdc.cn; 朱英,E-mail:zhuying@nieh.chinacdc.cn

English

Determination of Perfluoroalkyl Acids and Alternatives in Atmospheric Fine Particles by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

Corresponding author: XU Dong-qun, ; ZHU Ying,

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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-串联质谱法测定大气细颗粒物中全氟烷基酸及其替代物

通讯作者: 徐东群,E-mail:xudq@chinacdc.cn; 朱英,E-mail:zhuying@nieh.chinacdc.cn

English

Determination of Perfluoroalkyl Acids and Alternatives in Atmospheric Fine Particles by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

Corresponding author: XU Dong-qun, ; ZHU Ying,

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

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

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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