β-环糊精固载硅胶薄层色谱法拆分盐酸克伦特罗对映体

Resolution of Clenbuterol Hydrochloride Enantiomers by Thin-Layer Chromatography on Silica Gel Impregnated with β-Cyclodextrin

以羧甲基纤维素钠为交联剂,将β-环糊精固载在硅胶GF254表面上,并用其制备薄层色谱板。使用该薄层板拆分了盐酸克伦特罗对映异构体。考察了薄层拆分中展开剂的影响,发现展开剂中醇的种类和比例对拆分效果有较大的影响。分别考察了10种醇与乙腈混合溶剂作展开剂对拆分的影响,结果显示,只有正丁醇-乙腈、仲丁醇-乙腈、叔丁醇-乙腈混合溶剂作展开剂可拆分盐酸克伦特罗对映体。薄层色谱法拆分盐酸克伦特罗对映体的条件为:以1·00gβ-环糊精固载在15·00g硅胶GF254表面上,并用其制备薄层板,以乙腈-仲丁醇(体积比为20∶80)混合溶剂作展开剂,于室温下展开。在此条件下,盐酸克伦特罗对映体单体在薄层色谱板上的比移值Rf分别为0·34和0·72,分离度Rs为4·09,实现了基线分离,而且样品在薄层色谱板上的斑点大小一致,拆分效果最好。

The resolution of clenbuterol hydrochloride enantiomers was achieved by thin-layer chromatography on silica gel GF254 plates impregnated with β-cyclodextrin. The effect of stereoselective auxiliary （acetonitrile and alcohol ） was investigated. Resolution of clenbuterol hydrochloride enantiomers could be attained by using alcohols of butanol, 2-butanol or tert-butanol together with acetonitrile as developing solvent. The optimal conditions of resolution were determined as follows： a plate prepared with 15.00 g silica gel GF254 impregnated with 1.00 g β-cyclodextrin, acetonitrile-2-butanol （20： 80, v/v） as developing solvent and developed at room temperature. Under these conditions, Rf of the two isomers of clenbuterol hydrochloride enantiomers were 0.34 and 0.72 respectively. The resolution was 4.09 with baseline separationand the spots in chromatogram were almost of the same size.