在线SPE-UPLC-MS-MS快速检测水样中3种痕量类固醇雌激素  

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[3] WAN Qiao-ling;WANG Long;YU Wei-wei(Chongqing Monitoring Station,Water Quality Monitoring Network of National Urban Water Supply,Chongqing 400060,China;Chongqing Academy of Metrology and Quality Inspection,Chongqing 401123,China;Key Laboratory of Hydraulic and Waterway Engineering of the Ministry of Education,Chongqing Jiaotong University,Chongqing 400074,China)

机构地区：[1]国家城市供水水质监测网重庆监测站,重庆400060 [2]重庆市计量质量检测研究院,重庆401123 [3]重庆交通大学水利水运工程教育部重点实验室,重庆400074

出　　处：《化学研究与应用》2018年第7期1186-1189,共4页Chemical Research and Application

基　　金：国家重点研发计划项目(2017YFC0404706)资助

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.

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 

分 类 号：O657.7[理学—分析化学]