固相萃取-高效液相色谱-串联质谱法测定生活饮用水中11种全氟化合物的方法探究及应用  

Exploration and Application of 11 Determination Perfluorinated Compounds in Domestic Drinking Water Using Solid-Phase Extraction Ultra-High Performance Liquid Chroma-tography Tandem Mass Spectrometry

作　　者：张琪雨 吴艳龙 张祥汉 曾志鹏 胡颖斌 ZHANG Qiyu;WU Yanlong;ZHANG Xianghan;ZENG Zhipeng;HU Yingbin(Zhuhai W ater Supply and Drainage Pollution Control Center,Zhuhai 519000,China)

机构地区：[1]珠海市供水与排水治污中心,广东珠海519000

出　　处：《净水技术》2024年第S02期246-251,307,共7页Water Purification Technology

基　　金：广东省自然科学基金项目(2021A1515010365)。

摘　　要：文章开发固相萃取-高效液相色谱-串联质谱法(SPE-HPLC-MS)对生活饮用水中11种全氟化合物(PFCs)进行同时测定的分析方法。样品经WAX固相萃取小柱萃取后,浓缩直接进液相色谱-质谱联用仪进行分析,以ZORBAX SB-Aq色谱柱(2.1 mm×100 mm,3.5μm)进行分离,5 mmol/L乙酸铵溶液和甲醇为流动相梯度洗脱,使用电喷雾AJS离子源负离子(ESI-)模式进行扫描,多反应监测模式(MRM)检测。结果显示:11种PFCs在线性值为5.0~200.0 ng/L呈现良好的线性关系(r=0.998 4~0.999 8),方法检出限为0.32~1.20 ng/L。11种全氟化合物对生活饮用水实际样品低、中、高3个加标水平下的加标回收率分别为80.8%~104.0%、84.1%~102.0%、86.9%~123.0%,相对标准偏差(RSD)为0.8%~11.0%。该检测方法灵敏度高、操作简便,实现了普通HPLC-MS同时测定11种PFCs且能满足《生活饮用水卫生标准》(GB 5749—2022)限值要求,适用于检测生活饮用水中的PFCs。Solid-phase extraction high-performance liquid chromatography tandem mass spectrometry(SPE-HPLC-MS)for determining 11 perfluorinated compounds(PFCs)in domestic drinking water was established in this paper.After the sample was extracted by WAX solid phase extraction column,it was concentrated and directly sent to the liquid chromatography-mass spectrometer for analysis.It was separated by ZORBAX SB Aq chromatographic column(2.1 mmx100 mm,3.5μm).The mobile phase was 5 mmol/L ammonium acetate solution-methanol for gradient elution.The electrospray AJS ion source negative ion(ESI-)mode scanning and multi reaction monitoring mode(MRM)were used for detection.The results showed that the linear relationships of 11 PFCs were good,within the linear range from 5.0 ng/L to 200 ng/L(r=0.9984~0.9998),with a detection limit from 0.32 ng/L to 1.20 ng/L.The recovery rates of 11 PFCs at three spiking levels of low,medium,and high for actual samples of drinking water were from 80.8%to 104.0%,from 84.1%to 102.0%,and from 86.9%to 123.0%,respectively,with a relative standard deviation(RSD)from 0.8%to 11.0%.This detection method has the advantages of simple operation and high sensitivity,it achieves the simultaneous determination of 11 PFCs by a conventional HPLC-MS mothod and meets the limit values of Standards for Drinking Water Quality(GB 5749-2022).It is suitable for the detection of PFCs in drinking water.

关 键 词：生活饮用水 固相萃取 液质联用 全氟化合物(PFCs) 方法探究 

分 类 号：R123[医药卫生—环境卫生学]