SPE-UPLC-MS/MS法同时检测生活污水中四氢大麻酸等16种毒品目标物  

Simultaneous detection of 16 drugs including THC-COOH in wastewater using SPE-UPLC-MS/MS

作　　者：王蕊 郑航航 焦英 方秀英 周潇 WANG Rui;ZHENG Hanghang;JIAO Ying;FANG Xiuying;ZHOU Xiao(National Narcotics Laboratory Shaanxi Regional Center,The Narcotics Control Technical Center of Shaanxi Provincial Public Security Department,Key Laboratory of Drugs analysis&intelligent-Monitoring,Xi'an,712046,China;Yunnan Minzu University School of Chemistry and Environment,Kunming,650500,China)

机构地区：[1]国家毒品实验室陕西分中心,陕西省公安厅毒品技术中心,陕西省毒品分析与毒情智慧监测研究重点实验室,西安712046 [2]云南民族大学化学与环境学院,昆明650500

出　　处：《环境化学》2025年第3期1099-1108,共10页Environmental Chemistry

基　　金：陕西省自然科学基础研究计划项目(2024JC-YBMS-123)资助.

摘　　要：建立了一种固相萃取-超高液相-串联质谱法(SPE-UPLC-MS/MS)能同时检测生活污水中四氢大麻酸、吗啡和甲基苯丙胺等16种毒品目标物.使用WATERS Oasis HLB(60 mg,3CC)固相萃取小柱对目标物进行提取,采用多反应监测(MRM)模式,WATERS ACQUITY UPLC BEH C18(2.1 mm×100 mm×1.7μm)色谱柱,柱温40℃,以0.1%甲酸水-5 mmol·L^(−1)甲酸铵和0.1%乙腈为流动相进行洗脱分离.通过方法学验证,吗啡、O6-单乙酰吗啡、可待因和可卡因在5—250 ng·L^(−1)范围线性关系良好,其他目标化合物在1—250 ng·L^(−1)线性关系良好(R^(2)>0.998),日内精密度在0.89%—8.23%之间,日间精密度在1.47%—15.7%之间,回收率在94.4%—111%之间.SPE-UPLC-MS/MS法能够在15 min内同时完成水中16种碱性和酸性毒品目标物的检测,并成功应用于我国城市污水监测.This study presents the development of a Solid-Phase Extraction-Ultra High Liquid Chromatography-Tandem Mass Spectrometry(SPE-UPLC-MS/MS)method for the simultaneous detection of 16 target substances in domestic wastewater.These include Tetrahydrocannabinol acid(THC-COOH),morphine,methamphetamine,and others.The target substances were extracted using a solid-phase extraction column(WATERS Oasis®HLB 60 mg 3CC)and analyzed via Multiple Reaction Monitoring(MRM)mode in MS.The sample was separated on a column(WATERS ACQUITY UPLC®BEH C182.1 mm×100 mm×1.7μm),with the column temperature maintained at 40°C.A gradient elution was performed using a mobile phase consisting of 0.1%(volume fraction)formic acid-5 mmol·L^(−1) ammonium formate aqueous solution and 0.1%(volume fraction)acetonitrile solution.The method's validity was confirmed through experimental results.Notably,drugs such as morphine,O6-monoacetylmorphine,codeine,and cocaine demonstrated a strong linear relationship within the range of 5—250 ng·L^(−1).The remaining 13 targets also showed a strong linear relationship in the range of 1—250 ng·L^(−1)(R^(2)>0.998).The intra-day precision ranged from 0.89%to 8.23%,while the inter-day precision varied between 1.47%and 15.7%.The recoveries ranged from 94.4%to 111%.The SPE-UPLC-MS/MS method can simultaneously detect 16 types of acidic and alkaline drugs in wastewater within a 15-minute timeframe,demonstrating its potential for successful application in urban wastewater monitoring in China.

关 键 词：固相萃取-超高液相-串联质谱法 生活污水 毒品. 

分 类 号：X-1[环境科学与工程] O6[理学—化学]