【摘要】 目的:建立拆分新药尤利沙星对映异构体的HPLC手性流动相添加剂法。方法:通过探讨流动相pH、手性添加剂种类及浓度对手性拆分的影响,确定流动相为甲醇-异亮氨酸手性溶液(取L-异亮氨酸1.04g和硫酸铜1.0g溶于1000mL水中)(17∶83),在C18(250mm×4.6mm,5μm)柱上拆分尤利沙星对映体,检测波长为330nm,柱温为40℃。结果:两对映体分离良好,分离度在4.0以上,左旋体及右旋体检测限均为5ng。结论:本方法分离度好,简便易行,比手性固定相经济,可用于尤利沙星光学纯度的质量控制。更多还原

【Abstract】 Objective:To establish an HPLC method to separate ulifloxacin enantiomers using chiral mobile phase additives.Methods:By optimizing factors which affect the chiral separation,the pH value of the mobile phase,the type and concentration of chiral additives,the optimum condition for chiral separation were selected.The enantiomers separation was carried out on Diamonsil C18(250 mm×4.6 mm,5 μm)column,and methanol-isoleucine solution(containing 8 mmol·L-1 L-isoleucine and 4 mmol·L-1 copper sulphate)(17∶83)as the chiral mobile phase,detecting on wavelength at 330 nm.The column temperature was set at 40 ℃.Results:The two enantiomers could be baseline separated,and the resolution was higher than 4.0.The detection limits obtained by S/N=3 were 5 ng for L-ulifloxacin and D-ulifloxacin.Conclusions:The method is simple and economic with a good resolution,and it can be used for the quality control of ulifloxacin enantiomers.更多还原