逆流色谱与硅胶柱色谱相结合分离纯化高良姜中高良姜素

Separation and Purification of Galangin from Rhizomes of Alpinia officinarum Hance by Counter-Current Chromatography Combined with Silica Gel Column Chromatography

目的:建立一种从高良姜粗提物中分离制备高纯度高良姜素的方法。方法:采用逆流色谱(CCC)直接法以及逆流色谱(CCC)与硅胶柱色谱相结合两种方法从高良姜粗提物中分离制备高良姜素。结果:先用硅胶柱色谱对粗提物进行预分离,然后采用逆流色谱,以石油醚-乙酸乙酯-乙醇-水(2:0.4:0.8:0.9,V/V)为两相溶剂体系,对目标组分进行纯化,可以从高良姜粗提物中制备得到高纯度高良姜素。通过该方法可以从3.5g高良姜粗提物中分离得到纯度为99.1%的高良姜素15.6mg,纯度为95.2%的未知化合物Ⅱ5.2mg。结论:硅胶柱色谱与逆流色谱相结合为一种分离制备高纯度高良姜素有效方法。该方法可用于相关标准样品的研制及功能因子的开发。

The objective of this work was to establish a method to separate and purify galangin from rhizomes of Alpinia officinarum Hance using silica gel column chromatography combined with counter-current chromatography （CCC）. Crude galangin was separated by silica gel column chromatography and further purified by CCC using a two-phase solvent system consisting of petroleum ether, ethyl acetate, ethanol and water （2：0.4：0.8：0.9, V/F）. Using the developed method, 15.6 mg of galangin with a purity of 99.1% and 5.2 mg of an unknown compound with a purity of 95.2% were obtained from 3.5 g of crude galangin. This study demonstrates that the combination of silica gel column chromatography with counter-current chromatography can be an effective method for the separation and purification of galangin.