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引用本文:   陈勇杰, 张蓓蓓, 陈国松, 赵永刚, 王济奎. 超高效液相色谱-串联质谱法测定污水和污泥基质中的20种全氟及多氟化合物. 分析化学, 2019, 47(4): 533-540. doi:  10.19756/j.issn.0253-3820.181766 [复制]

Citation:   CHEN Yong-Jie , ZHANG Bei-Bei , CHEN Guo-Song , ZHAO Yong-Gang , WANG Ji-Kui . Analysis of 20 Kinds of Perfluoroalkyl and Polyfluoroalkyl Substances in Wastewater and Sludge Samples with Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry. Chinese Journal of Analytical Chemistry, 2019, 47(4): 533-540. doi: 10.19756/j.issn.0253-3820.181766 [复制]

超高效液相色谱-串联质谱法测定污水和污泥基质中的20种全氟及多氟化合物

收稿日期: 2018-12-09

基金项目: 本文系江苏省环境监测基金项目(No.1210)资助

Analysis of 20 Kinds of Perfluoroalkyl and Polyfluoroalkyl Substances in Wastewater and Sludge Samples with Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

Received Date:  2018-12-09

建立了适用于测定污水和污泥两种基质中全氟-多氟化合物(PFASs)的样品前处理方法和仪器检测方法,用于测定污水和污泥两种介质中20种PFASs:9种全氟羧酸(PFCAs)、3种全氟磺酸(PFSAs)、2种N-烷基全氟辛基磺酰胺乙醇(FOSEs)、2种N-烷基全氟辛基磺酰胺(FOSAs)和4种氟调醇(FTOHs)。对于污水样品,采用WAX固相萃取小柱对样品进行净化及富集,WAX小柱活化上样后,分别用4 mL甲醇和3 mL甲醇(含0.5%(V/V) NH4OH)依次洗脱非离子型全氟化合物(FOSEs、FOSAs和FTOHs)和离子型全氟化合物(PFCAs和PFSAs),相应的洗脱液定容后,用液相色谱-质谱进行检测。对于污泥样品,采用加速溶剂萃取法,以乙腈为萃取剂对所有目标物进行萃取,萃取液经氮吹浓缩,过石墨化碳柱净化后检测。结果表明,水样和污泥样品中20种PFASs的平均加标回收率分别为62%~130%和71%~126%,相对标准偏差为0.9%~12.7%和0.4%~15.2%,方法定量限分别为0.24~4.32 ng/L和0.04~0.12 ng/g。本方法前处理简单,灵敏度高,重现性好,适用于工业污水及污泥基质中多种PFASs的同时检测。

关键词:   全氟化合物, N-烷基全氟辛基磺酰胺乙醇, N-烷基全氟辛基磺酰胺, 氟调醇, 污水, 污泥
Key words:   Per- and polyfluoroalkyl substances, Perfluoroalkane sulfonamidoethanols, Perfluoro-1-octanesulfonamides, Fluorotelomer alcohols, Wastewater, Sludge
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超高效液相色谱-串联质谱法测定污水和污泥基质中的20种全氟及多氟化合物

陈勇杰, 张蓓蓓, 陈国松, 赵永刚, 王济奎

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