固相萃取-高效液相色谱串联质谱法测定饮用水中39种药品及个人护理品  

Determination of 39 Pharmaceuticals and Personal Care Products in Drinking Water by Solid Phase Extraction-High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：吴孟李 张琪雨 吴艳龙 曾志鹏 胡颖斌 张祥汉 WU Mengli;ZHANG Qiyu;WU Yanlong;ZENG Zhipeng;HU Yingbin;ZHANG Xianghan(Zhuhai Monitoring Station of National Urban Drainage Monitoring Network,Zhuhai 519000,China;Zhuhai Water Supply and Drainage Pollution Control Center,Zhuhai 519000,China)

机构地区：[1]国家城市排水监测网珠海监测站,广东珠海519000 [2]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8期111-123,共13页Water Purification Technology

基　　金：广东省自然科学基金项目(2021A1515010365)。

摘　　要：文章建立了应用固相萃取-高效液相色谱-串联质谱同时测定生活饮用水中39种药品及个人护理品的分析方法。样品经HLB固相萃取小柱萃取后,浓缩直接进高效液相色谱-质谱联用仪进行分析,以Agilent PFP色谱柱(2.1 mm×100 mm,2.7μm)进行分离,甲醇-0.1%甲酸水溶液为流动相梯度洗脱,采用电喷雾AJS离子源正离子(ESI)模式扫描,多反应监测模式(MRM)进行检测。结果显示:39种药品及个人护理品在0.05~100μg/L的不同线性范围均呈现良好的线性关系(r=0.9954~0.9999),方法检出限为0.029~1.300 ng/L。39种药品及个人护理品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63.0%~123.0%、70.1%~126.0%、78.7%~122.0%,相对标准偏差分别为1.4%~19.0%、0.7%~9.3%、0.6%~9.8%。该检测方法实现了普通高效液相色谱质谱仪同时测定39种药品及个人护理品且能满足国家标准的精密度和准确度,具有操作简单、灵敏度高等优点,适用于生活饮用水中药品及个人护理品的检测。An analytical method for the simultaneous determination of 39 pharmaceuticals and personal care products(PPCPs)in drinking water using solid-phase extraction,high-performance liquid chromatography,and tandem mass spectrometry was established.After being extracted by HLB solid phase extraction column,the sample was concentrated and directly sent to the high performance liquid chromatography-mass spectrometer for analysis.The Agilent PFP column(2.1 mm×100 mm,2.7μm)was used for separation.Methanol-0.1%formic acid aqueous solution was used as the mobile phase for gradient elution.The electrospray AJS ion source positive ion(ESI)mode was used for scanning,and the multi reaction monitoring mode(MRM)was used for detection.The results showed that 39 PPCPs exhibit good linear relationships within different linear ranges of 0.05~100μg/L(r=0.9954~0.9999),and the detection limit of the method was from 0.029 to 1.300 ng/L.The recovery rates of 39 PPCPs for actual samples of drinking water at low,medium,and high spiking levels were 63.0%~123.0%,70.1%~126.0%,and 78.7%~122.0%,respectively,with relative standard deviations of 1.4%~19.0%,0.7%~9.3%,and 0.6%~9.8%.This detection method achieves the simultaneous determination of 39 PPCPs using a conventional high-performance liquid chromatography mass spectrometer,and can meet the precision and accuracy requirements of national standard.It has the advantages of simple operation and high sensitivity,and is suitable for the detection of PPCPs in drinking water.

关 键 词：固相萃取 液质联用 生活饮用水 药品 个人护理品 

分 类 号：TU991[建筑科学—市政工程]