固相萃取/高效液相色谱/串联质谱法同时测定水中雌激素  

Simultaneous Detection of Estrogens in Sewage and River Water by Solid Phase Extraction/HPLC-MS/MS

作　　者：阳春[1] 邹玲[1] 胡碧波[1] 张真真[1] 王亚丹[1] 

机构地区：[1]重庆大学三峡库区生态环境教育部重点实验室,重庆400045

出　　处：《中国给水排水》2014年第4期87-91,共5页China Water & Wastewater

基　　金：国家自然科学基金资助项目(41101492;50308183);重庆市基础与前沿研究计划项目(CS7C2013jcyjA20021)

摘　　要：配合固相萃取预处理技术，采用HPLC—MS／MS内标分析方法检测了污水厂处理流程及其受纳水体污水水样中的雌激素雌酮（E1）、雌二醇（E2）、炔雌醇（EE2）和硫酸雌酮（E1—3-s）浓度，水样中四种目标物均有检出，受纳水体中E1—3-s的当量浓度分别占到E1当量浓度和计算总雌激素浓度的49．4％和19．1％（均折算为E2当量）。本检测方法色谱峰可有效分离，单个混合样的分析周期为12．0min，线性范围分别为（0．5～100．1）、（0．4—98．8）、（0．1～99．4）和（0．2～100．0）ng／mL，方法检测限分别为0．5、0．4、0．1和0．2ng／L，测定结果的精密度及加标回收率均良好。The concentrations of El, E2, EE2 and E1-3-S in samples from sewage treatment process and receiving water body were simultaneously analyzed using HPLC-MS/MS preceded by solid phase extraction pretreatment. All the four objective analytes were detected. E1-3-S accounted for 49.4% and 19.1% of E1 and total estrogens in receiving water body samples （calculated as E2 equivalent concentration）. The chromatographic peak of the detection method could be effectively separated. The time for analyzing a mixed sample is 12.0 min. The linear detection ranges were 0.5 to 100. 1 ng/mL, 0.4 to 98.8 ng/mL, 0.1 to 99.4 ng/mL and 0.2 to 100.0 ng/mL. The limits of detection were 0.5, 0.4, 0.1 and 0.2 ng/L. The satisfactory precision and recovery were obtained.

关 键 词：自由雌激素 结合雌激素 同时测定 高效液相色谱 串联质谱 

分 类 号：X832[环境科学与工程—环境工程] O657.63[理学—分析化学]