Fu Lulu, Lu Chenghua, Tong Shengqiang, Xu Min, Tang Lan, Shan Weiguang
College of Pharmaceutical Science, Zhejiang University of Technology, 288 Liuhe Rd, Hangzhou 310014, P.R. China.
J Chromatogr Sci. 2021 Feb 15;59(3):212-216. doi: 10.1093/chromsci/bmaa087.
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%.
通过半制备逆流色谱法从仙鹤草中分离并纯化出5种非极性间苯三酚衍生物，即伪蛇麻脂素、α-蛇麻脂素和仙鹤草酚A - C。分离采用非水溶剂系统两步洗脱进行。第一步，使用由正己烷 - 乙腈 - 二氯甲烷 - 甲醇（6:6:0.5:0.5，v/v/v/v）组成的两相溶剂系统的洗脱模式。从粗提物（371.0毫克）中得到含有三种成分的样品Ⅰ（47.0毫克）和含有两种成分的样品Ⅱ（24.8毫克）。第二步，样品Ⅰ通过由正己烷 - 乙腈 - 二氯甲烷（10:7:3，v/v/v）组成的溶剂系统的闭环循环模式成功分离，得到17.8毫克伪蛇麻脂素、18.5毫克α-蛇麻脂素和6.4毫克仙鹤草酚A。另外两种化合物——8.7毫克仙鹤草酚B和13.6毫克仙鹤草酚C——以相同方式从样品Ⅱ中获得。所有分离得到的化合物纯度均超过95%。
