响应曲面法在类固醇雌激素HPLC-MS-MS定量分析中的应用

Application of response surface method in the quantification for steroid estrogens using HPLC-MS-MS

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。通过响应曲面法(RSM)优化了3种雌激素在高效液相色谱串联质谱联用(HPLC-MS-MS)检测方法中的多离子监测反应(MRM)条件,获得E1、E2和EE2的最优碎片电压分别为205.0、196.0和182.0V,最优碰撞能分别为43.0、51.0和54.0V。配合固相萃取(SPE)预处理技术,采用HPLC-MS-MS内标检测方法检测了重庆主城区嘉陵江水样中E1、E2和EE2的浓度。3者在该方法中的定量检测限分别为0.5、0.4和0.1ng/L。

Estrone （ E1 ）, 17β-estradiol （E2） and 17α-ethinylestradiol （EE2） exhibit the highest estrogenic potential. A HPLC-MS-MS analysis method using internal standard is established with the multiple reaction monitoring （MRM） model. Further more, the fragment voltages and collision energies in the MRM model are optimized by response surface method （RSM）. The optimal fragment voltages of El, E2 and EE2 are 205.0, 196.0 and 182.0 V respectively and the collision energies are 43.0, 51.0 and 54.0 V. The established method followed the two-step solid phase extraction （SPE） is then applied for the quantification of El, E2 and EE2 in the water samples collected from a activated sludge process sewage treatment work and Jialing River at the urban section of Chongqing City. The detection limits of El, E2 and EE2 are 0.5, 0.4 and 0.1 ng/L.