| 污水中常见违禁药物分析方法优化及验证 |
| 摘要点击 1995 全文点击 807 投稿时间：2016-06-25 修订日期：2016-08-03 |
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| 中文关键词 违禁药物 污水 固相萃取 超高效液相色谱-串联质谱 回收率 |
| 英文关键词 illicit drugs wastewater SPE UPLC-MS/MS recovery |
| 作者 | 单位 | E-mail | | 高婷婷 | 北京大学城市与环境学院, 地表过程与分析实验室, 北京 100871 | gaottjy@163.com | | 杜鹏 | 北京大学城市与环境学院, 地表过程与分析实验室, 北京 100871 | | | 徐泽琼 | 北京大学城市与环境学院, 地表过程与分析实验室, 北京 100871 | | | 杨军 | 北京市城市排水监测总站有限公司, 北京 100012 | | | 张华方 | 北京市城市排水监测总站有限公司, 北京 100012 | | | 李喜青 | 北京大学城市与环境学院, 地表过程与分析实验室, 北京 100871 | xli@urban.pku.edu.cn |
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| 中文摘要 |
| 违禁药物作为一种新型污染物得到了环境科学界的广泛关注.本文根据国内外已有研究，比较了污水样的前处理条件如SPE柱和水样pH值、冲洗、酸化及复溶过程.结果表明，对实际污水样的前处理应将样品pH值调为2，选用Oasis MCX柱，无需除杂质的冲洗和氮吹过程的酸化步骤，因两种上机测定方法HILIC-UPLC-MS/MS和C18-UPLC-MS/MS不同而分别选择200 μL乙腈和100 μL乙腈+100 μL 5 mmol·L-1乙酸铵复溶.通过比较HILIC法和C18法的保留时间及检出限、定量限、回收率和基质效应等方法评价指标，确定污水样的测定应选用C18-UPLC-MS/MS.最后，将优化后的测定方法用于分析北京市12家污水处理厂的进、出水样，验证了方法的可靠性，为违禁药物的污水流行病学研究和环境风险评价奠定了基础. |
| 英文摘要 |
| Illicit drugs have been recognized as a group of emerging pollutants.Based on previous research,procedures to pre-treat wastewater including SPE column,pH of water samples,and processes of washing,acidifying and re-dissolving were compared.It was found that the best recovery was achieved when wastewater was adjusted to pH=2 and Oasis MCX column was used.It was not necessary to flush the loaded column or to acidify the eluate prior to evaporation using nitrogen steam.After evaporation,it is recommended to redissolve the evaporated samples using 200 μL acetonitrile and 100 μL acetonitrile+100 μL 5 mmol·L-1 ammonium acetate in Milli-Q water for HILIC-UPLC-MS/MS and C18-UPLC-MS/MS,respectively.After comparing retention times,limit of detection,limit of quantification,recoveries,and matrix effects of HILIC and C18 methods,C18-UPLC-MS/MS was chosen.Influent and effluent samples from 12 wastewater treatment plants in Beijing were analyzed using the optimized method for validation.The validated methods set a firm foundation to apply the sewage-based epidemiology to monitor illicit drug abuse in China. |
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