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目的:建立西酞普兰中间体(CTD)手性对映体的高效液相色谱分析方法,用于测定不同分离过程所得产品的光学纯度。方法:采用Chiralpak IC(250 mm×4.6 mm,5μm)键合型手性柱,流速1.0 mL.min-1,柱温25℃,系统考察了以正己烷为主体的标准流动相和四氢呋喃、甲基叔丁基醚、二氯甲烷等非标准流动相体系中CTD对映体的分离效果;在优选的2种流动相中进一步考察了柱温对分离的影响以及系统适用性。结果:优选的标准流动相正己烷-正丙醇-三乙胺(80∶20∶0.1,v/v)中CTD对映体的分离度为9.04;非标准流动相正己烷-二氯甲烷-乙醇-二乙胺(50∶50∶2∶0.1,v/v)中CTD对映体的分离度为10.22,S-(-)-CTD先于R-(+)-CTD出峰。结论:CTD对映体在优选的流动相中分析时间短、分离度高、系统适用性好,所建立的分析方法高效、快速,重现性好,可用于西酞普兰中间体的光学纯度测定。
OBJECTIVE: To establish a method for the high performance liquid chromatography of chiral enantiomers of citalopram intermediates (CTDs) for the determination of optical purity of products obtained from different isolation processes. METHODS: Chiralpak IC (250 mm × 4.6 mm, 5 μm) bonded chiral column was used. The flow rate was 1.0 mL · min-1 and the column temperature was 25 ℃. The mobile phase consisted of n-hexane and tetrahydrofuran Tert-butyl ether, dichloromethane and other non-standard mobile phase CTD enantiomers separation effect; in the two preferred mobile phase further investigated the influence of column temperature on the separation and system suitability. Results: The resolution of the CTD enantiomer in the preferred standard mobile phase n-hexane-n-propanol-triethylamine (80: 20: 0.1, v / v) was 9.04; the mobile phase n-hexane- The resolution of CTD enantiomer in ethanol - diethylamine (50:50:2:0.1, v / v) was 10.22, and the S - (-) - CTD was earlier than that of R - (+) - CTD. Conclusion: The enantiomers of CTD have shorter analysis time, higher resolution and better system applicability in the preferred mobile phase. The established analytical method is efficient, rapid and reproducible and can be used for the determination of optical purity of citalopram intermediates .