在线SPE-UPLC-MS-MS快速检测水样中3种痕量类固醇雌激素

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英文篇名：Rapid quantification of 3 trace steroid estrogens in water samples using online SPE-UPLC-MS-MS 作者：万巧玲 ; 王龙 ; 余薇薇 英文作者：WAN Qiao-ling;WANG Long;YU Wei-wei;Chongqing Monitoring Station,Water Quality Monitoring Network of National Urban Water Supply;Chongqing Academy of Metrology and Quality Inspection;Key Laboratory of Hydraulic and Waterway Engineering of the Ministry of Education,Chongqing Jiaotong University; 关键词：类固醇雌激素 ; 在线固相萃取-超高速液相色谱-串联质谱 ; 雌酮 ; 17β-雌二醇 ; 17α-乙炔基雌二醇 英文关键词：SEs;;online SPE-UPLC-MS-MS;;E1;;E2;;EE2 中文刊名：HXYJ 英文刊名：Chemical Research and Application 机构：国家城市供水水质监测网重庆监测站;重庆市计量质量检测研究院;重庆交通大学水利水运工程教育部重点实验室; 出版日期：2018-07-15 出版单位：化学研究与应用 年：2018 期：v.30 基金：国家重点研发计划项目(2017YFC0404706)资助 语种：中文; 页：HXYJ201807026 页数：4 CN：07 ISSN：51-1378/O6 分类号：148-151

摘要

雌酮(E1)、17β-雌二醇(E2)和17α-乙炔基雌二醇(EE2)是雌情活力最强的3种类固醇雌激素(SEs)。3种SEs在水样中一般含量很低,富集预处理繁琐耗时,且普通高效液相色谱-串联质谱(HPLC-MS-MS)检测过程也耗时较长。利用在线固相萃取-超高速液相色谱-串联质谱(在线SPE-UPLC-MS-MS)的在线SPE功能和超高流速,采用多反应检测模式(MRM)和内标定量方法,直接进样同时快速检测了重庆主城区某水厂水源水和出厂水中3种SEs的浓度。方法全过程检测时间由8.5h大幅缩减为仅11min。3种SEs在该方法中的定量检测限分别为0.500ng·L~(-1),0.200ng·L~(-1)和0.100ng·L~(-1),符合相关国际标准要求。
        Estrone( E1),17β-estradiol( E2) and 17α-ethinylestradiol( EE2) exhibit the highest estrogenic potential. Because of the low concentrations of the 3 compounds in water,their enrichment method for the pretreatment was difficult and time-consuming,and their usual analysis methods suing HPLC-MS-MS were also time-consuming.A simple and quick analysis method by online SPE-UPLC-MS-MS using the direct injection and internal standard was established with the multiple reaction monitoring( MRM). The established method was then applied for the quantification of the 3 organic compounds in the water samples collected from a water work and Yangtze River at the urban section of Chongqing City.The total analysis time of the new established method was shortened to only 11 min from about 8. 5 h.The detection limits of the 3 organic compounds were 0. 500 ng·L~(-1),0. 200 ng·L~(-1) and 0. 100 ng·L~(-1),which were suitable for the Standard in UK,and the experimental sensitivity,precision,accuracy,and repeatability were qualified.

引文

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