环糊精衍生物__(期刊论文)

新型药物辅料2羟丙基β环糊精的色谱分离纯化

http://www.100md.com 《分析化学》 2006年第5期

环糊精衍生物,,环糊精衍生物，2羟丙基β环糊精，薄层色谱，柱色谱,摘要,关键词,1引言,2实验部分,3结果与讨论,4结论,Referenc

     摘要

    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。

     关键词 环糊精衍生物，2羟丙基β环糊精，薄层色谱，柱色谱

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

    Zhang Yimin*，Zhang Zhifei，Zhou Qin，Wang Tuo

    (Key Laboratory for Green Chemical Technology of State Education Ministry,School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072)

    Abstract 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 corresponding spectra of electrospry ionizationmass spectrometry. ......

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