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目的:建立西酞普兰对映异构体的HPLC手性分析方法,用于草酸艾司西酞普兰光学纯度的分析测定。方法:采用不易变性的卵类粘蛋白键合硅胶(ES-OVM)为手性固定相,以乙腈-0.05 mol.L-1磷酸盐缓冲液(pH 7.0)(15︰85)为流动相,流速为1.0 mL.min-1,柱温30℃,检测波长240 nm,对西酞普兰对映异构体进行分离测定。结果:西酞普兰对映异构体在卵粘蛋白柱上实现了良好的分离,分离度为1.90。将该方法应用于手性拆分得到的草酸艾司西酞普兰的光学纯度测定,结果光学纯度大于97.9%。结论:该方法分离度与重现性好,可用于西酞普兰的光学纯度的分析测定及对拆分过程进行监测,结果可靠。
OBJECTIVE: To establish a HPLC chiral method for the determination of citalopram enantiomers for the optical determination of escitalopram oxalate. Methods: The immiscible egg-like mucin-bonded silica gel (ES-OVM) was used as the chiral stationary phase. The mobile phase consisted of acetonitrile-0.05 mol·L-1 phosphate buffer pH 7.0 (15︰85) The flow rate was 1.0 mL.min-1, the column temperature was 30 ℃ and the detection wavelength was 240 nm. The enantiomers of citalopram were separated and determined. RESULTS: The citalopram enantiomers were well separated on the ovum ovalbumin column with a resolution of 1.90. The method was applied to the optical purity determination of escitalopram oxalate obtained by chiral resolution. The optical purity was greater than 97.9%. Conclusion: The method has good resolution and reproducibility, which can be used for the determination of citalopram optical purity and monitoring the resolution process, and the results are reliable.