西酞普兰中间体在纤维素键合手性固定相上的拆分

Enantiomeric resolution of citadiol on immobilized cellulose chiral stationary phase

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 an HPLC method for the chiral separation of citadiol（CTD） enantiomers to determine the optical purity of products using different separation processes.Methods：The column used was Chiralpak IC（250 mm×4.6 mm,5 μm） at a flow rate of 1.0 mL·min-1 and 25 ℃.Effects of standard mobile phases including the bulk of hexane and nonstandard mobile phases involving tetrahydrofuran,methyl tertiary butyl ether,methylene chloride,etc.were studied on the chiral separation of CTD.Effects of temperature and the system applicability test were investigated using the optimal mobile phases.Results：The optimal standard mobile phase consisted of hexane-n-propanol-TEA（80∶ 20∶ 0.1,v/v） with the resolution value of 9.04,while the optimal nonstandard one was hexane-CH2Cl2-ethanol-DEA（50∶ 50∶ 2∶ 0.1,v/v） with the resolution value of 10.22.S-（-）-CTD eluted prior to R-（＋）-CTD.Conclusion：Using the optimal mobile phases CTD enantiomers can be separated in short time,with high resolution values and good system applicability.These methods can be used to determine the optical purity of CTD with high efficiency and good repetition.