Abstract

Five non-polar phloroglucinol derivatives, viz. pseudo-aspidin, α-kosin and agripinol A-C were isolated and purified from Agrimonia pilosa Ledeb by semi-preparative counter-current chromatography. The separation was performed by a two-step elution with non-aqueous solvent systems. In the first step, an elution mode of a two-phase solvent system consisting of n-hexane-acetonitrile-dichloromethane-methanol (6:6:0.5:0.5, v/v/v/v) was used. We obtained sample Ι containing three components (47.0 mg) and sample ΙΙ containing two components (24.8 mg) from crude extract (371.0 mg). In the second step, sample Ι was successfully separated by closed-loop recycling mode with a solvent system consisting of n-hexane-acetonitrile-dichloromethane (10:7:3, v/v/v), yielding 17.8 mg of pseudo-aspidin, 18.5 mg of α-kosin and 6.4 mg of agripinol A. The other two compounds—8.7 mg of agripinol B and 13.6 mg of agripinol C—were obtained from sample ΙΙ in the same manner. All the isolated compounds had a high purity exceeding 95%.

中文翻译：

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非水溶剂体系逆流色谱法分离和纯化龙蒿中五种间苯三酚衍生物

摘要

五种非极性间苯三酚衍生物，即。通过半制备逆流色谱法从松毛龙牙草中分离和纯化了假阿斯匹定，α-kosin和agripinol AC 。通过非水溶剂体系的两步洗脱进行分离。在第一步骤中，一个两相溶剂体系的洗脱模式包括ñ -己烷-乙腈-二氯甲烷-甲醇（6：6：0.5：0.5，V / V / V / V）中的溶液使用。我们从粗提取物中（371.0mg）获得了包含三种组分（47.0mg）的样品I和包含两种组分（24.8mg）的样品II。在第二步中，样品Ⅰ通过闭环再循环模式成功分离，其中溶剂系统由n-己烷-乙腈-二氯甲烷（10：7：3，v / v / v），得到17.8 mg假阿斯匹定，18.5 mgα-kosin和6.4 mg阿格品醇A。其他两种化合物-8.7 mg阿格品醇以相同的方式从样品II获得B和13.6mg的农心磷脂C-。所有分离出的化合物均具有超过95％的高纯度。