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污水中新精神活性物质的分析方法优化及验证
摘要点击 172  全文点击 55  投稿时间:2017-12-29  修订日期:2018-02-24
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中文关键词  新精神活性物质  污水流行病学  污水  固相萃取  超高效液相色谱-串联质谱联用仪
英文关键词  new psychoactive substances (NPS)  wastewater-based epidemiology  wastewater  solid phase extraction (SPE)  ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS)
作者单位E-mail
陈培培 北京大学城市与环境学院, 地表过程分析与模拟教育部重点实验室, 北京 100871 chenpeipei0420@126.com 
杜鹏 北京大学城市与环境学院, 地表过程分析与模拟教育部重点实验室, 北京 100871  
周子雷 北京大学城市与环境学院, 地表过程分析与模拟教育部重点实验室, 北京 100871  
徐泽琼 北京大学城市与环境学院, 地表过程分析与模拟教育部重点实验室, 北京 100871  
高婷婷 北京大学城市与环境学院, 地表过程分析与模拟教育部重点实验室, 北京 100871  
李喜青 北京大学城市与环境学院, 地表过程分析与模拟教育部重点实验室, 北京 100871 xli@urban.pku.edu.cn 
中文摘要
      随着对传统毒品打击力度的增大,各种为规避现行法律管制而合成的新精神活性物质(new psychoactive substances,NPS)层出不穷.NPS被滥用后,经人体新陈代谢所生成的代谢产物和未被代谢的原药随尿液进入生活污水,从而汇入污水处理厂,经处理后被排入自然水体.因此在国内外以往相关研究的基础上,应用固相萃取和UPLC-MS/MS技术,建立并优化了污水中11种常见NPS的前处理及检测方法.比较了污水前处理条件(如SPE柱、样品pH值、淋洗和复溶等)对目标物回收率的影响.结果表明最优前处理条件为:选用Oasis MCX柱,在pH=2的条件下加载样品,用2 mL pH=2的超纯水和2 mL甲醇淋洗SPE柱,400 μL 20%的甲醇水溶液复溶.通过对目标物的保留时间、回收率、基质效应、检出限和定量限、精密度等指标的评价,说明优化后的前处理方法和C18-UPLC-MS/MS检测方法高效可靠.应用优化后的方法对北京市11家污水处理厂的进、出水样进行了分析,验证了方法的可靠性,为进一步开展NPS的污水流行病学研究及健康风险评价提供了参考依据.
英文摘要
      New psychoactive substances (NPS) are emerging continuously, as the crackdown against traditional drugs becomes stricter. Metabolites of NPSs and the unchanged drugs enter wastewater through urine and are collected and treated by wastewater treatment plants before being discharged into the aquatic environment. Based on previous research, solid phase extraction (SPE) and ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) were used and the detection method of 11 NPSs was optimized. Influences of wastewater pretreatment procedures, including SPE columns; pH values of water samples; and processes of flushing and redissolving on NPS recoveries were compared. It was shown that the best recovery was achieved when Oasis MCX columns were used and the pH value of wastewater samples was adjusted to 2. A flushing process with 2 mL water at pH=2 followed by 2 mL methanol was needed. Redissolution of the residue after evaporation was best achieved with 400 μL of a 20% methanol water solution. It was indicated by retention times, recoveries, matrix effects, limits of detection, limits of quantification, as well as precision that C18-UPLC-MS/MS and the optimized method are efficient and valid. Influent and effluent samples from 11 municipal wastewater treatment plants in Beijing were analyzed using the optimized method for validation. The validated method can be used as an important reference for monitoring NPSs via wastewater-based epidemiology and for assessing the risk of NPS abuse in China.

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