通过逐步增加流动相流速，利用高速逆流色谱法从药用植物蛇床子中制备分离和纯化佛手柑内酯和欧前胡素。
Preparative isolation and purification of bergapten and imperatorin from the medicinal plant Cnidium monnieri using high-speed counter-current chromatography by stepwise increasing the flow-rate of the mobile phase.
作者信息
Lia Hua-Bin, Chen Feng
机构信息
Department of Botany, The University ofHong Kong, Pokfulam Road, Hong Kong, China.
出版信息
J Chromatogr A. 2004 Dec 17;1061(1):51-4. doi: 10.1016/j.chroma.2004.10.091.
A high-speed counter-current chromatography (HSCCC) method was developed for the preparative separation and purification of bergapten and imperatorin from the Chinese medicinal plant Cnidium monnieri (L.) Cusson. The crude extract was obtained by extraction with ethanol from the dried fruits of Cnidium monnieri (L.) Cusson under sonication. Preparative HSCCC with a two-phase solvent system composed of n-hexane-ethyl acetate-ethanol-water (5:5:5:5, v/v/v/v) was successfully performed by increasing the flow-rate of the mobile phase stepwise from 1.0 to 2.0 ml min(-1) after 180 min. The components purified and collected were analyzed by high-performance liquid chromatography. The method yielded 45.8 mg of bergapten at 96.5% purity and 118.3 mg of imperatorin at 98.2% purity from 500 mg of the crude extract in a single run. The recoveries of bergapten and imperatorin were 92.1 and 93.7%, respectively.
建立了一种高速逆流色谱（HSCCC）方法，用于从中药蛇床子中制备分离和纯化佛手柑内酯和欧前胡素。通过在超声处理下用乙醇从蛇床子干燥果实中提取得到粗提物。采用正己烷 - 乙酸乙酯 - 乙醇 - 水（5:5:5:5，v/v/v/v）组成的两相溶剂系统，在180分钟后将流动相流速从1.0逐步提高到2.0 ml min⁻¹，成功进行了制备型HSCCC。对纯化收集的组分进行高效液相色谱分析。该方法单次运行从500 mg粗提物中得到纯度为96.5%的佛手柑内酯45.8 mg和纯度为98.2%的欧前胡素118.3 mg。佛手柑内酯和欧前胡素的回收率分别为92.1%和93.7%。
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