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。
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.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2006年第5期713-716,共4页
Chinese Journal of Analytical Chemistry
基金
天津市自然科学基金(No.030024)资助
关键词
环糊精衍生物
2-羟丙基-Β-环糊精
薄层色谱
柱色谱
β-Cyclodextrin derivatives, 2-hydroxypropyl-β-cyclodextrin, thin-layer chromatography, column chromatography