非水毛细管电泳测定醋酸甲羟孕酮方法的研究

Non-aqueous capillary electrophoresis method for the analysis of Medroxyprogesterone Acetate

目的:建立非水毛细管电泳技术测定醋酸甲羟孕酮含量的新方法。方法:以37cm×75μm(id)未涂层空心毛细管柱为分离通道,采用甲醇为溶剂,50mmol·L^(-1)乙酸钠溶液(pH9.4)为电泳介质,于220nm 波长柱上检测,分离电压25kV,压力进样(3447.38Pa×5s),采用峰面积内标法定量。结果:在选定的电泳条件下,醋酸甲羟孕酮的浓度在100.2～501.0μg·mL^(-1)范围内与峰面积比呈良好的线性关系(r=0.9993);低、中、高3种浓度(n=3)的平均回收率分别为101.9%,99.40%,98.70%;方法的检测限(S/N=3)为10.02μg·mL^(-1);日内和日间峰迁移时间的 RSD 分别为1.25%和2.43%,峰面积之比的RSD 分别为1.00%和1.89%。结论:该方法试剂用量少、简便、准确,可用于醋酸甲羟孕酮质量的分析。

Objective： A new non - aqueous capillary electrophoresis method for the determination of Medroxypro- gesterone Acetate. Methods： Fused - silica capillary 37 cm × 75 μm （id） was used. Medroxyprogesterone Acetate can be determination in 50 mmol· L^-1 sodium acetate （pH 9. 4） in methanol as the buffer. The effects of concentration and pH of the running buffer, running voltage was studied. The separation voltage was 25 kV, the injection pressure and injection time were 3447.38 Pa and 5 s. The UV detector was set at 220 nm. Internal calibration curve of peak area was selected. Results：There was excellent linearity between the peak area ratio and concentration of the Medroxyprogesterone Acetate in the concentration range of 100. 2 -501.0 μg· mL^-1. The correlation coefficient was 0. 9993 ,the detection limit of Medroxyprogesterone Acetate at three times the signal to noise was 10. 02 μg · mL^-1. The average recovery were 101.9% ,99.40% ,98.70% respectively at the lower, middle and higher concentration（ n = 3 ）. The relative standard deviation value for migration time of intra - assay and inter - assay were 1.25% and 2. 43% respectively. The relative standard deviation value for the ratio of peak area were 1.00% and 1.89% respectively. Conclusions： This is beneficial for routine quality control analysis of Medroxyprogesterone Acetate tablets, the results demonstrated the method is less solvent consumption, simple rapid and accurate.