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首页> 外文期刊>Journal of chromatography, B. Analytical technologies in the biomedical and life sciences >Combinative application of pH-zone-refining and conventional high-speed counter-current chromatography for preparative separation of alkaloids from Stephania kwangsiensis
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Combinative application of pH-zone-refining and conventional high-speed counter-current chromatography for preparative separation of alkaloids from Stephania kwangsiensis

机译：pH区精制与常规高速逆流色谱联用在广谱石楠生物碱的制备分离中的应用

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摘要

A method which involves the combination of pH-zone-refining counter-current chromatography (pH-zone-refining CCC) and conventional high-speed counter-current chromatography (HSCCC) was established for the preparative separation of alkaloids from the crude extracts of Stephania kwangsiensis. pH-zone-refining CCC was first performed with the solvent system composed of n-hexane-ethyl acetate-methanol-water (3:7:1:9, v/v), where triethylamine (10mM) was added to the upper organic stationary phase as a retainer and hydrochloric acid (5mM) to the aqueous mobile phase as an eluter. From 2.0g of crude extract, 370mg of sinoacutine and 600mg of a mixture of three other alkaloids were obtained. Then, the mixture was further separated by conventional HSCCC with the solvent system composed of n-hexane-ethyl acetate-methanol-water (7:3:6:4, v/v), yielding 42mg of (-)-crebanine, 50mg of (-)-stephanine and 30mg of l-romerine from 150mg mixture of three other alkaloids, respectively. The purities of the four compounds were all over 98% as determined by HPLC, and the chemical structures of the four compounds were confirmed by positive ESI-MS and ~1H NMR data. Results of the present study successfully indicated that this method was efficient for the preparative separation of alkaloids from natural plants.
机译：建立了将pH区域精制逆流色谱法（pH区域精制CCC）与常规高速逆流色谱法（HSCCC）结合使用的方法，用于从Stephania粗提物中分离出生物碱广西首先使用由正己烷-乙酸乙酯-甲醇-水（3：7：1：9，v / v）组成的溶剂系统进行pH区域精制CCC，其中将三乙胺（10mM）添加到上层有机层中。固定相作为保留剂，盐酸（5mM）作为流动相作为洗脱剂。从2.0克粗提物中获得370毫克西诺卡汀和600毫克三种其他生物碱的混合物。然后，将混合物通过常规HSCCC用正己烷-乙酸乙酯-甲醇-水（7：3：6：4，v / v）组成的溶剂体系进一步分离，得到42mg（-）-甲胺丁酮，50mg分别从150毫克的其他三种生物碱混合物中提取（-）-斯蒂芬宁和30毫克的l-罗马氨酸。通过HPLC测定，这四种化合物的纯度均超过98％，并且通过正ESI-MS和〜1H NMR数据证实了这四种化合物的化学结构。本研究结果成功表明该方法可有效地从天然植物中分离生物碱。

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