在线固相萃取/超高效液相色谱-串联质谱测定地表水中90种药品及个人护理用品  

Determination of 90 Pharmaceutical and Personal Care Products in Surface Water by Online Solid Phase Extraction with UPLC-MS/MS

作　　者：李珏 徐巧 李剑 王天琦 杨继伟 俞晓峰 LI Jue;XU Qiao;LI Jian;WANG Tian-qi;YANG Ji-wei;YU Xiao-feng(Hangzhou Puyu Technology Development Co.Ltd,Hangzhou 311300,China)

机构地区：[1]杭州谱育科技发展有限公司,浙江杭州311300

出　　处：《分析测试学报》2024年第5期722-730,共9页Journal of Instrumental Analysis

摘　　要：该研究建立了在线固相萃取(OSPE)/超高效液相色谱-串联质谱(UPLC-MS/MS)测定地表水中90种药品及个人护理用品(PPCPs)的分析方法。水样经过滤后直接进样注入OSPE柱中进行净化和富集,通过阀切换将目标物转移到分析柱中进一步分离分析。采用Waters HSS T3 C_(18)(100 mm×2.1 mm,1.8μm)色谱柱进行分离,以0.1%甲酸水溶液和乙腈为流动相进行洗脱。质谱采用正、负离子同时采集,多反应监测(MRM)模式检测,内标法定量。在优化的色谱-质谱条件下,90种PPCPs呈良好的线性关系,相关系数(r^(2))均大于0.99,检出限为0.06~10.00 ng/L,定量下限为0.24~40.00 ng/L;在10、20、100 ng/L加标水平下,90种化合物的回收率为81.2%~120%,大多数化合物的相对标准偏差(n=7)小于10%。该方法的分析效率、灵敏度高,运行稳定,可作为地表水中PPCPs的监测方法。This study established an online solid phase extraction(OSPE)/ultrahigh performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method for the determination of 90 pharmaceutical and personal care products(PPCPs)in surface water.After filtration,the water sample was directly injected into the OSPE column for purification and enrichment,and the target substances were transferred to the analysis column for further separation and analysis through valve switching.Using a Waters HSS T3 C_(18)(100 mm×2.1 mm,1.8μm)chromatographic column for separation,with 0.1%formic acid aqueous solution and acetonitrile as the mobile phase for elution.The analytes were detected in multiple reaction monitoring(MRM)mode through positive and negative electrospray ionization(ESI),and quantified with internal standard method.Under optimized chromatography-mass spectrometry conditions,90 PPCPs showed good linear relationships with the correlation coefficients(r^(2))more than 0.99.The detection limits reached 0.06-10.00 ng/L,and the quantitation limits reached 0.24-40.00 ng/L.The recoveries in actual samples analyzed at spiked concentrations of 10,20,and 100 ng/L were between 81.2%and 120%,with relative standard deviations(n=7)of most compounds less than 10%.This method has high analysis efficiency,sensitivity,and stable operation,and could be used as a monitoring method for analyzing PPCPs in surface water samples.

关 键 词：药品及个人护理用品 在线固相萃取 超高效液相色谱-串联质谱 地表水 

分 类 号：O657.7[理学—分析化学] X132[理学—化学]