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作 者:原帅 于治国[2] 王海峰[3] 向平 施妍 杨欢 刘梦曦 骆如欣 沈保华 YUAN Shuai;YU Zhi-guo;WANG Hai-feng;XIANG Ping;SHI Yan;YANG Huan;LIU Meng-xi;LUO Ru-xin;SHEN Bao-hua(Shanghai Key Laboratory of Forensic Medicine,Shanghai Forensic Service Platform,Institute of Forensic Science,Ministry of Justice,PRC,Shanghai 200063,China;School of Pharmacy,Shenyang Pharmaceutical University,Shenyang 110016,China;College of Environmental Science and Engineering,Tongji University,Shanghai 200092,China)
机构地区:[1]司法鉴定科学研究院上海市法医学重点实验室上海市司法鉴定专业技术服务平台司法部司法鉴定重点实验室,上海200063 [2]沈阳药科大学药学院,辽宁沈阳110016 [3]同济大学环境科学与工程学院,上海200092
出 处:《质谱学报》2021年第6期1080-1090,共11页Journal of Chinese Mass Spectrometry Society
基 金:国家自然科学基金(81871531);上海市法医学重点实验室资助项目(17DZ2273200);上海市司法鉴定专业技术服务平台资助项目(19DZ2292700);中央级科研院所基本科研业务费资助项目(GY2018Z-2)。
摘 要:本研究采用固相萃取对城市生活污水样品进行前处理,超高效液相色谱-串联高分辨质谱法筛选及确证污水中阿片类、苯丙胺类和苯二氮卓类等36种滥用物质,并将其应用于实际污水样品。结果表明,该方法的专属性强,36种滥用物质的检出限范围为5~20 ng/L。在12个污水样品中共检出吗啡、可待因、哌替啶、曲马多4种阿片类滥用物质,甲基苯丙胺1种苯丙胺类滥用物质以及地西泮、去甲西泮、艾司唑仑、阿普唑仑4种苯二氮卓类滥用物质。城市生活污水中存在多种滥用物质,区域流行性不同,利用本方法可进行快速、准确地筛选与确认。Assessing collective drug consumption based on the species and concentrations of illicit drugs and their metabolites in wastewater is an objective,real-time,accurate,convenient and effective monitoring technology.In order to establish a rapid screening and confirmation method for the abuse of opioids,amphetamines and benzodiazepines in wastewater,solid phase extraction was used to pretreat the wastewater sample,and ultra-high liquid chromatography-tandem high-resolution mass spectrometry was used to screen and confirm 36 kinds of analytes.Moreover,the method was applied to real wastewater samples collected from different wastewater treatment plants.Different HPLC columns and mobile phases were tested for optimization of the method.The peak shapes,retention time,separation and sensitivity of the chromatographic procedure were evaluated.Finally,an Accucore Hypersil Gold column(100 mm×2.1 mm×1.9μm),and the mobile phases of ultrapure water with 2 mmol/L ammonium formate-0.1%formic acid(A)and acetonitrile-methanol(1∶1,V∶V)with 2 mmol/L ammonium formate and 0.1%formic acid were applied because of good peak shapes and separation.TraceFinder software was selected for rapid screening,and retention time,molecular mass,fragment ions and isotope distribution were collected as the screening basis.A substance could be judged as positive if it all met these 4 screening conditions.Therefore,the results obtained were more authentic and reliable.The LODs ranged from 5 to 20 ng/L.The extraction recoveries were higher than 70%for all compounds in wastewater,and the matrix effect ranged from-24.4%to 21.2%.In the real wastewater samples,4 opioids of morphine,codeine,pethidine,tramadol,1 amphetamine of methamphetamine and 4 benzodiazepines of diazepam,nordazepam,estazolam,alprazolam were detected,and the error of all compounds were less than 5×10^(-6).There are many kinds of abused substances in wastewater,and the regional prevalence is also different.The method established in this article can be used for rapid and accurate scr
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