超高效液相色谱-串联质谱法测定城市污水中5种胺酮类新精神活性物质  

Determination of five ketamine analogues in municipal wastewater by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：安琪 徐布一 罗莉娅 白登文 陶虹利 王欢博 AN Qi;XU Buyi;LUO Liya;BAI Dengwen;TAO Hongli;WANG Huanbo(School of Environment and Resource,Southwest University of Science and Technology,Mianyang 621010,China;National Anti-Drug Laboratory Sichuan Regional Center,Chengdu 610299,China)

机构地区：[1]西南科技大学环境与资源学院,绵阳621010 [2]国家毒品实验室四川分中心,成都610299

出　　处：《分析试验室》2024年第10期1417-1422,共6页Chinese Journal of Analysis Laboratory

基　　金：四川省科技计划项目重点研发项目(2023YFS0418,2020YFS0056);毒品监测管控与禁毒关键技术公安部重点实验室开放课题(2022-KLDMC-07)资助。

摘　　要：建立了基于固相萃取(SPE)-超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定污水中5种胺酮类新精神活性物质氟胺酮(2-FDCK)、2-(甲氨基)-2-(2-甲苯基)-环己-1-酮(2-MDCK)、2-(乙氨基)-2-(2-氟苯基)-环己-1-酮(2-FDCNEK)、2-(2-溴苯基)-2-(甲氨基)-环己-1-酮(2-BrDCK)、2-(乙氨基)-2-苯基-环己-1-酮(2-oxo-PCE)的分析方法。污水样品过滤后,通过Oasis MCX固相萃取柱进行净化和富集;采用Poroshell 120 EC-C18色谱柱分离,0.1%甲酸水和乙腈为流动相梯度洗脱;电喷雾离子源正离子(ESI+)、动态多反应监测(dMRM)模式,同位素内标法定量。结果表明,5种胺酮类分析物在0.02~20.0 ng/mL范围内线性良好,线性相关系数(R^(2))均大于0.999;检出限(LOD)和定量限(LOQ)分别低于0.08 ng/L和0.27 ng/L。在5.0 ng/L和50.0 ng/L浓度加标水平下,5种胺酮类分析物的相对标准偏差(RSD)低于6.2%,平均回收率为103%~120%。将该方法用于某城市6个污水处理厂采集的实际污水样品分析,检测出2-FDCK和2-FDCNEK,表明该方法适用于污水中胺酮类新精神活性物质的监测。An analytical method was developed for the simultaneous determination of five ketamine analogues including 2-fluoro deschloroketamine(2-FDCK),2-(methylamino)-2-(2-methyphenyl)-cyclohexanone(2-MDCK),2-fluorodeschloro-N-ethyl-ketamine(2-FDCNEK),2-bromo deschloroketamine(2-BrDCK),and 2-oxo-PCE in municipal wastewater based on solid phase extraction(SPE)-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The wastewater samples were filtered,then the analytes were cleaned-up and enriched by an Oasis MCX solid phase extraction column.The five ketamine analogues were separated on a Poroshell 120 EC-C18 column with a gradient elution of 0.1%formic acid in water and acetonitrile as the mobile phases.The mass spectra were collected in the positive ion(ESI+)and dynamic multiple reaction monitoring(dMRM)mode.Isotope internal standard method was selected for the quantification of the analytes.Results showed that the linearity was good in the range of 0.02-20.0 ng/mL for each ketamine analogue,and the correlation coefficients(R^(2))were higher than 0.999.The limits of detection(LODs)and limits of quantification(LOQs)were lower than 0.08 ng/L and 0.27 ng/L,respectively.At spiked concentrations of 5.0 ng/L and 50.0 ng/L,the relative standard deviations(RSDs)were lower than 6.2%and the average recoveries were in the range of 103%-120%,showing satisfactory precision and accuracy.The method was applied to actual wastewater samples collected from six wastewater treatment plants,and 2-FDCK and 2-FDCNEK were detected,indicating that the proposed method is suitable for the determination of ketamine analogues in wastewater.

关 键 词：新精神活性物质 固相萃取 液相色谱-串联质谱 污水 

分 类 号：O657.31[理学—分析化学] X832[理学—化学]