固相萃取-超高效液相色谱-串联质谱法测定污水中16种全氟和多氟烷基化合物  

Determination of 16 Perfluoroalkyl and Polyfluoroalkyl Substances in Wastewater by Solid Phase Extraction-Ultraperformance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：原盛广[1,3] 郎爽 王颖[2] 李振涵[1,3] 张文强 单保庆[1,3] 贾丽 Yuan Shengguang;Lang Shuang;Wang Ying;Li Zhenhan;Zhang Wenqiang;Shan Baoqing;Jia Li(Research Center for Eco-Environmental Sciences,Chinese Academy of Sciences,Beijing 100085,China;Beijing Center for Physical and Chemical Analysis,Beijing 100089,China;University of Chinese Academy of Sciences,Beijing 100049,China)

机构地区：[1]中国科学院生态环境研究中心,北京100085 [2]北京市理化分析测试中心,北京100089 [3]中国科学院大学,北京100049

出　　处：《生态毒理学报》2021年第3期239-251,共13页Asian Journal of Ecotoxicology

基　　金：国家水体污染控制与治理重大科技专项(2017ZX07107-004-001);中国科学院青年创新促进会(2018058);广东省重点领域研发计划资助项目(2019B110205002)。

摘　　要：建立了以固相萃取-超高效液相色谱-串联质谱同时测定污水中16种全氟和多氟烷基化合物(PFASs)的方法。样品经固相萃取柱富集浓缩,采用BEH-C 18色谱柱(2.1 mm×100 mm,1.7μm),以甲醇和5 mmol·L^(-1)乙酸铵溶液(pH=9)为流动相梯度淋洗,负离子多反应监测模式进行定性和定量分析,内标法定量。16种PFASs在0.1~40μg·L^(-1)范围内线性关系良好,相关系数(r^(2))>0.99,目标物加标回收率为65.1%~129.0%,相对标准偏差(RSD)为0.8%~8.0%(n=6),方法检出限为0.012~4.00 ng·L^(-1)。方法重现性好,灵敏度高。适用于污水中PFASs的定量测定。A method for the simultaneous determination of 16 perfluoroalkyl and polyfluoroalkyl substances(PFASs)in wastewater by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry was established.The sample was enriched and concentrated on a solid-phase extraction column with a BEH-C18 column(2.1 mm×100 mm,1.7μm),using methanol and 5 mmol·L^(-1) ammonium acetate solution(pH=9)as mobile phases with gradient elution,and quantified in the negative ion multiple reaction monitoring mode with internal standard method.The linear range of the 16 PFASs was 0.1~40μg·L^(-1) with the correlation coefficients(r^(2))greater than 0.99,the spiked recoveries were 65.1%~129.0%,the relative standard deviations(RSD)were 0.8%~8.0%(n=6),and the method limits of detection were 0.012~4.00 ng·L^(-1).The method has good reproducibility and high sensitivity.It is suitable for the quantitative determination of PFASs in wastewater.

关 键 词：全氟和多氟烷基化合物 固相萃取-超高效液相色谱-串联质谱 污水 

分 类 号：X171.5[环境科学与工程—环境科学]