在线固相萃取-超高效液相色谱/串联质谱法测定饮用水中8种精神类药物  

Determination of Psychotropic Pharmaceuticals in Drinking Water by Online Solid Phase Extraction Coupled with Ultra Performance Liquid Chromatography/Tandem Mass Spectrometry

作　　者：王珮玥[1] 梁娜娜[1] 冯鑫[1] 韩深[1] 崔风云 齐鹤鸣 WANG Pei-yue;LIANG Na-na;FENG Xin;HAN Shen;CUI Feng-yun;QI He-ming(Inspection and Quarantine Technical Center of Beijing Entry-Exit Inspection and Quarantine Bureau ,Beijing 100026)

机构地区：[1]北京出入境检验检疫局检验检疫技术中心,北京100026

出　　处：《分析科学学报》2018年第6期777-782,共6页Journal of Analytical Science

基　　金：北京市科技计划(No.Z151100002115059)

摘　　要：采用在线固相萃取-超高效液相色谱/串联质谱技术,建立了饮用水中奥卡西平、卡马西平、阿米替林、舍曲林、帕罗西汀、阿利马嗪、氯米帕明和氟西汀8种精神类药物的检测方法。样品经微孔滤膜过滤,用甲酸调节至pH=3.0,直接进入在线固相萃取-超高效液相色谱/串联质谱仪进行分析。实验确定样品以Oasis?HLB柱净化富集,采用ACQUITY HSS T3色谱柱分离,流动相为乙腈和0.5%(体积分数)甲酸水溶液,以电喷雾正离子多反应监测模式(MRM)进行定性定量分析。方法的定量限(LOQ)为0.1ng/L,平均回收率为68.9%～105.8%,相对标准偏差为3.6%～13.6%(n=6)。将建立的方法应用于北京市部分饮用水源地水样的分析,检测出2种精神类药物。An online solid phase extraction-ultra performance liquid chromatography/tandem mass spectrometry(SPE-UPLC-MS/MS) method was established to simultaneously determine eight psychotropic pharmaceuticals(Oxcarbazepine,Carbamazepine,Amitriptyline,Sertraline,Paroxetine,Alimemazine,Clomipramine and Fluoxetine)in drinking water.The samples were filtered by millipore filter membrane,adjusted to acidic and then directly injected into online SPE-UPLC-MS/MS.Oasis HLB carriage was used as an online SPE cartridge to purify and enrich the sample.The analytes were separated using an ACQUITY HSS T3 column and a binary mobile phase consisting of acetonitrile and water with 0.5% formic acid under the gradient elution.The eight psychotropic pharmacenticals were identified and quantified by positive electrospray ionization tandem mass spectrometry in multiple reaction monitoring(MRM)mode.The limits of quantification were 0.1 ng/L.The average recoveries in the matrix were ranging from 68.9%to 105.8% with the relative standard deviations(RSDs)of 3.6%-13.6%(n=6).The developed method was applied to analyze the water samples from Beijing.The results showed two psychotropic pharmacenticals were detected in samples.

关 键 词：饮用水 精神类药物 在线固相萃取 超高效液相色谱/串联质谱法 

分 类 号：O657.63[理学—分析化学]