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固相萃取-液相色谱串联质谱法测定城市污水中他莫昔芬和来曲唑
引用本文:刘先军,张晶,邵兵,尹杰.固相萃取-液相色谱串联质谱法测定城市污水中他莫昔芬和来曲唑[J].分析化学,2010,38(2).
作者姓名:刘先军  张晶  邵兵  尹杰
作者单位:1. 北京市疾病预防控制中心,北京,100013;首都医科大学公共卫生与家庭医学学院,北京,100058
2. 北京市疾病预防控制中心,北京,100013
3. 北京市疾病预防控制中心,北京,100013;北京大学医学部公共卫生学院,北京,100191
基金项目:国家自然科学基金(Nos.20607004,20837003)资助项目
摘    要:他莫昔芬和来曲唑常用于治疗雌激素依赖型乳腺癌。本研究建立了城市污水中他莫昔芬和来曲唑的超高效液相色谱-串联质谱(UPLC-MS/MS)联用检测方法。水样通过Oasis HLB固相萃取柱富集后串联氨基柱,先用6 mL甲醇洗脱,再用3 mL甲醇洗脱氨基柱,合并洗脱液后浓缩。使用ACQUITY UPLCTM BEH C18反相柱,流动相为0.1%甲酸-乙腈,在梯度条件下分离;目标分析物使用超高效液相色谱-电喷雾串联质谱进行测定。本方法对他莫昔芬和来曲唑的线性范围分别是1.0~100μg/L和0.1~100μg/L,相关系数R2>0.997,检出限分别为1.0和0.1 ng/L,进水和出水的3个不同水平的加标平均回收率为68.8%~103.0%,相对标准偏差小于15%。本方法可用于城市污水中相关物质的分析。

关 键 词:超高效液相-串联质谱法  他莫昔芬  来曲唑  环境污水  固相萃取  

Determination of Tamoxifen and Letrozole in Sewage by Solid Phase Extraction and Ultra Performance Liquid Chromatography/ Tandem Mass Spectrometry
LIU Xian-Jun,ZHANG Jing,SHAO Bing,YIN Jie.Determination of Tamoxifen and Letrozole in Sewage by Solid Phase Extraction and Ultra Performance Liquid Chromatography/ Tandem Mass Spectrometry[J].Chinese Journal of Analytical Chemistry,2010,38(2).
Authors:LIU Xian-Jun  ZHANG Jing  SHAO Bing  YIN Jie
Institution:Central Laboratory;Beijing Center for Disease Control & Prevention;Beijing 100013;School of Public Health and Family Medicine;Capital Medical University;Beijing 100058;School of Public Health;Peking University;Beijing 100191
Abstract:Tamoxifen and letrozole are two of the most effective pharmaceuticals mainly used in hormonal dependent breast cancer therapy.A trace analytical method using ultra performance liquid chromatography/tandem mass spectrometry(UPLC-MS/MS) was developed to simultaneously detect these two drugs in both influent and effluent of municipal sewage treatment plant.Sewage samples were passed through an Oasis HLB cartridge,then an amino solid phase extraction cartridge was connected with Oasis HLB cartridge.Target compo...
Keywords:Ultra-performance liquid chromatography/tandem mass spectrometry  Tamoxifen  Letrozole  Sewage  Solid phase extraction  
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