[1]邬晶晶,桂萍,郭风巧.固相萃取-UPLC-MS/MS法测定水中17种全氟化合物[J].中国给水排水,2022,38(12):28-36.
　WUJing-jing,GUIPing,GUOFeng-qiao.SPE-UPLC-MS/MS for Determination of 17 PFCs in Water[J].China Water & Wastewater,2022,38(12):28-36.
点击复制

固相萃取-UPLC-MS/MS法测定水中17种全氟化合物

中国给水排水[ISSN:1000-4062/CN:12-1073/TU] 卷: 第38卷 期数: 2022年第12期 页码: 28-36 栏目: 出版日期: 2022-06-17
Title:
SPE-UPLC-MS/MS for Determination of 17 PFCs in Water
作者:
邬晶晶， 桂萍， 郭风巧
（中国城市规划设计研究院，北京 100044）
Author(s):
WU　Jing-jing， GUI　Ping， GUO　Feng-qiao
（China Academy of Urban Planning & Design， Beijing 100044， China）
关键词:
固相萃取;  超高效液相色谱-串联质谱;  背景干扰;  全氟化合物
Keywords:
solid phase extraction;  UPLC-MS/MS;  background interference;  PFCs
摘要:
基于固相萃取-超高效液相色谱串联质谱建立了生活饮用水及水源水中17种全氟化合物的测定方法。水样经WAX固相萃取柱富集后用超高效液相色谱串联质谱测定，采用Cortecs C18色谱柱进行分离，流动相为含2 mmol/L乙酸铵的水和甲醇/乙腈（80∶20），采用多反应监测（MRM）模式测定，电喷雾电离源（ESI），负离子扫描。通过管材及捕集柱优化，在采样、样品前处理、检测等全过程消除了背景干扰。17种全氟化合物的标准曲线线性相关系数（R2）均大于0.99，定量限范围为0.083~1.56 ng/L。加标4种不同浓度时，生活饮用水（出厂水、管网水）的加标回收率为65.0%~117.8%，相对标准偏差为0.13%~17.93%；水源水的加标回收率为67.0%~117.8%，相对标准偏差为0.60%~18.71%。与国标中规定的11种全氟化合物的超高效液相色谱串联质谱检测方法相比，该方法灵敏度高、稳定性好，提高了检测效率，可实现饮用水中17种痕量全氟化合物从源头到龙头的全流程高效准确检测。
Abstract:
A method for determination of 17 perfluorinated compounds (PFCs) in drinking water and source water was established based on solid phase extraction-ultra?performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The water sample was extracted by WAX solid phase extraction (SPE) column and determined by UPLC-MS/MS. The separation was performed on a Cortecs C18 column with mobile phases of water containing 2 mmol/L ammonium acetate and methanol/acetonitrile (80∶20), and PFCs were analyzed by using multiple reaction monitoring (MRM) mode, negative electrospray ionization and negative ion scanning. Background interference was eliminated in the whole process of sampling, sample pre-treatment and detection through optimization of the pipe material and trap column. The linear correlation coefficients (R2) of 17 PFC standard curves were all greater than 0.99, and the limits of quantification ranged from 0.083 ng/L to 1.56 ng/L. When adding standard solutions of 4 different concentrations, the recoveries of drinking water (product water and pipe water) were 65.0%-117.8% and the relative standard deviations (RSD) were 0.13%-17.93%. The recoveries of source water were 67.0%-117.8%, and the RSD were 0.60%-18.71%. Compared with 11 PFCs detection methods proposed in the national standard, this method has the advantages of high sensitivity, good stability and high detection efficiency, which can detect 17 trace PFCs in drinking water from source to tap.

相似文献/References:

[1]郎朗,董晓琪,狄静波.SPE-HPLC法测定松花江哈尔滨段水样中11种抗生素[J].中国给水排水,2018,34(20):114.
　LANG Lang,DONG Xiao qi,DI Jing bo.Determination of 11 Antibiotics in Harbin Section of Songhua River by SPE-HPLC[J].China Water & Wastewater,2018,34(12):114.
[2]黄思静,汪义杰,朱斌,等.超高效液相色谱-高分辨质谱法测定水体中青霉素残留[J].中国给水排水,2021,37(2):112.
　HUANG Si-jing,WANG Yi-jie,ZHU Bin,et al.Determination of Penicillin Residues in Water by Ultra High Performance Liquid Chromatography-High Resolution Mass Spectrometry[J].China Water & Wastewater,2021,37(12):112.
[3]陈峰,张宝锋,何平,等.固相萃取/液相色谱-电喷雾串联质谱法测定水中噻菌灵[J].中国给水排水,2021,37(22):109.
　CHEN Feng,ZHANG Bao-feng,HE Ping,et al.Determination of Thiabendazole in Water by Solid Phase Extraction/Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry[J].China Water & Wastewater,2021,37(12):109.

更新日期/Last Update: 2022-06-17