固相萃取-LC-MS法检测水中痕量雌激素  

DETEMINATION OF TRACE ESTROGENS IN SURFACE WATER USING SPE-LC-MS

作　　者：常红[1] 胡建英[1] 邵兵[1] 徐烨[2] 高建峰 董民强 

机构地区：[1]北京大学城市与环境学系,北京100871 [2]东北大学理学院 [3]浙江省城市供水水质监测中心

出　　处：《环境化学》2003年第4期400-403,共4页Environmental Chemistry

基　　金：国家杰出青年科学基金项目 ( 4 992 5 1 0 3 ) ;环保"863" ( 2 0 0 1AA6460 1 0 5 )

摘　　要：研究了乙腈 /水、乙腈 /甲醇 /水、甲醇 /水三种不同流动相的条件下 ,LC MS分析雌酮 ,雌二醇 ,雌三醇 ,炔雌醇四种对象物质的灵敏度 ,发现流动相对灵敏度影响较大 ,不同流动相的对象物质的仪器检出限分别为 :330— 75 0ng·l- 1 ,1 0 0— 30 0ng·l- 1 ,5 0— 1 0 0ng·l- 1 .用固相萃取 LC MS检测杭州地区河水 ,在 8个采样点中 ,有 7个检测出了炔雌醇 ,其浓度范围在 1 1 7— 3 35ng·l- 1 之间 ,一个采样点检测出雌二醇 ,其浓度为 0 32ng·l- 1 .In this study,ESI LC MS method was used to analyze 4 estrogens(estrone(E1),17 β estradiol(E2),estriol(E3),ethynyl estradiol(EE))in surface water,and the effects of mobile phase on the sensitivities of 4 estrogens was investigated.When CH 3CN/H 2O,CH 3CN/CH 3OH/H 2O,CH 3OH/H 2O were used as mobile phase,the limits of detection were 330-750 ng·l -1 ,100-300ng·l -1 ,50-100ng·l -1 ,respectively.On the other hand,CH 3CN/H 2O,CH 3CN/CH 3OH/H 2O can separate 4 objective compounds,while the E1,E2 and E2 can not be separated completely when CH 3OH/H 2O was used as mobile phase.Finally,the method based on the off line solid phase extraction(SPE)and ESI LC MS was applied to analyze the four estrogens in surface water which were taken from Hangzhou river basin.The EE was detected in 7 samples,and its concentration ranged from 1 17 to 3 35ng·l -1 .E1 and E3 were not detected in all sample,and E 2(0 32ng·l -1 )was found in only one sample.

关 键 词：固相萃取-LC-MS法 污染 水 痕量雌激素 检测 灵敏度 

分 类 号：O661.1[理学—分析化学]