硅胶柱色谱结合高速逆流色谱法分离制备白首乌根皮中的苯乙酮类成分

Separation and Purification of Acetophenones from Cynanchum bengei Decne Root Bark by Combination of Silica Gel and High-speed Counter-current Chromatography

目的:创建硅胶柱色谱结合高速逆流色谱法制备分离泰山白首乌根皮中苯乙酮类成分的方法。方法:白首乌根皮粗提物先经过硅胶柱色谱进行初步分离,得到含有苯乙酮类成分的A和B两个组分,分别采用石油醚-乙酸乙酯-甲醇-水(4∶6∶4.5∶5.5,V/V)和石油醚-乙酸乙酯-甲醇-水(4∶6∶3∶7,V/V)的两相溶剂体系进行制备并分离。结果:从260 mg组分A中分离制备得到对苯二酚3.9 mg(1)、4-羟基苯乙酮17.1 mg(2)、2,5-二羟基苯乙酮13.3 mg(3)和2,4-二羟基苯乙酮21.0 mg(4);从300 mg组分B中分离得到白首乌二苯酮136 mg(5)。经高效液相色谱分析,其纯度分别为97.0%、96.6%、99.2%、99.7%、99.5%。结论:该法简便、快速、高效,可用于白首乌根皮中苯乙酮类成分的快速分离制备,有较好的实用价值,为白首乌根皮的开发利用提供了参考依据。

Objective： To develop a method for separation and purification of acetophenones from Cynanchum bengei Decne root bark by combination of silica gel and high-speed counter-current chromatography （ HSCCC ）. Methods ： The crude extract of C. bengei was separated by silica gel chromatography and part A and B were obtained. Then, part A and B were separated by HSCCC with a two-phase solvent system composed of petroleum ether-ethyl acetate-methanol-water （4：6：4. 5：5.5, V/V） and （4：6：3：7, V/V）, respectively. Results： From 260 mg of part A, four compounds with p-dihydroxybenzene 3.9 mg （1）, 4-hydroxyacetophenone 17. 1 mg （2）, 2, 5-di-hydroxyacetophenone 13.3 mg （3） and 2, 4-dihydroxyaceto-phenone 21.0 mg （4） were obtained. And from 300 mg of part B, baishouwubenzoph-enone 136 mg （5） were obtained. The compounds purity determined by HPLC were 97.0% , 96. 6% , 99.2% , 99. 7% , 99.5% , respectively. Conclusion： The established method is simple and efficient. It can be used for separation of acetophenones from C. bengei. The results provide a reference basis for C. bengei root bark development and utilization.