固相萃取高效液相色谱/串联质谱优化测定水中EE2

Determination of EE2 in Water by Solid Phase Extraction/HPLC/MS/MS

不少研究表明,17α-乙炔基雌二醇(EE2)是雌情活力最强的类固醇雌激素。通过响应曲面法(RSM)优化EE2的高效液相色谱/串联质谱联用(HPLC/MS/MS)检测中的多离子检测反应(MRM)条件,获得EE2的最优碎片电压为182.0V,最优碰撞能为54.0V。配合固相萃取(SPE)预处理技术,采用HPLC/MS/MS内标检测法检测了重庆主城区嘉陵江表面水与污水水样中的EE2浓度,方法检测限为0.1ng/L;线性范围为0.51～99.37ng/mL;精密度试验中RSD为0.276%;重复性试验中RSD为8.788%;加标回收试验结果良好;单个混合样品分析周期为28.0min。

The research shows that 17α-ethinyloestradiol （EE2） has the highest oestrogenic potential. The multiple reaction monitoring （MRM） conditions in determination method of HPLC-MS-MS for EE2 were optimized by the response surface method （RSM）. The optimal fragment voltage of EE2 is 182.0 V, and the collision energy is 54.0 V. After a sample pretreatment using two-step solid phase ex- traction （SPE） , this method was applied for the determination of EE2 in Jialing River surface water and sewage samples from Chongqing City. The detection limit is 0.1 ng/L, and the linear range is 0.51 to 99.37 ng/mL. The RSD in precision test is 0. 276%, and the RSD in repetitive experiments is 8. 788%. The average recovery is satisfactory, and the analysis cycle time of each sample for HPLC-MS-MS is 28.0 min.