新型药物辅料2-羟丙基-β-环糊精的色谱分离纯化

Chromatographic Separation and Purification of Novel Drug Excipient 2-Hydroxypropyl-β-Cyclodextrin

利用薄层色谱方法对碱浓度为1.5%、β-环糊精∶环氧丙烷(摩尔比)=1∶21的条件下生成的2-羟丙基-β-环糊精进行了定性分析,并通过对展开剂的选择和优化,得到了3种能有效分离不同取代度2-羟丙基-β-环糊精的展开剂体系,分别为正丙醇-水-浓氨水(6∶3∶1,V/V),异丙醇-水-浓氨水(6∶4∶0.5,V/V)和乙醇-水-浓氨水(6∶3∶0.8,V/V)。通过以乙醇体系为洗脱剂的硅胶柱色谱对其进行分离纯化,得到了两种不同取代的2-羟丙基-β-环糊精。经过ESI-MS谱图分析,确定分离后产品分别为单取代和双取代2-羟丙基-β-环糊精。

2-Hydroxypropyl-β-cyclodextrins （2-HP-β-CDs） were synthesized in 1.5% （m/V） NaOH solution with a molar ratio of β-cyclodextrin to propylene oxide 1：21. The products were analyzed by thin layer chromatography （TLC） through three optimized developing solvent systems： 1-propanol-H2O-concetrated aq. ammonia （6：3：1, V/V） ; 2-propanol-H2O-concetrated aq. ammonia （6：4：0.5, V/V） .and ethanol-H2O-concetrated aq. ammonia （6： 3：0.8, V/V）. Two purified compounds with different substitution degrees were obtained by using above-mentioned ethanol system as the eluent through a silica gel column separation treatment, and the substitution degrees of these separated compounds could be proved by their con：esponding spectra of electrospry ionization-mass spectrometry.