干柱层析法制备性分离冰片中龙脑和异龙脑

PREPARATIVE SEPARATION OF BORNEOL AND ISOBORNEOL IN BINGPIAN BY DRYCOLUMN CHROMATOGRAPHY

用干柱层析法,以硅胶为吸附剂,石油醚-醋酸乙酯-氯仿(20:2:6)为展开剂,在50×4cmi.d.柱上,下行展开,按龙脑和异龙脑在薄层板上的Rf值,初步判断柱上谱带的相应位置,分段切割,采用“打孔进样法”于薄层板上直接进样检试,分别收集龙脑和异龙脑谱带段吸附剂,用无水乙醇洗脱,减压回收溶剂,残液于冰箱中放置,即可得龙脑和异龙脑纯品。

Borneol(Ⅰ) and isoborneol (Ⅱ) insynthetic Bingpian are separated by meansof dry-column chromatography (DCC).The sample mixed with a small amount ofadsorbent is transferred to the top of thecolum (50×4cm i.d.) packed with silicagel (200 mesh) and developed with petro-leum ether-ethyl acetate-chloroform (20: 2:6) until the solvent has spread from thetop to the bottom of column. The zones ofⅠand Ⅱ can be located by the correspond-ing Rf of TLC. They are then eluted sep-arately with absolute alcohol. After theconcentration of the eluent by vacuum dis-tillation, the crystals of Ⅰ andⅡ are iso-lated from the residual solution on stand-ing. The purities of Ⅰ and Ⅱ are testeadwith known specimens by TLC.