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Isolation and Purification of Five Phloroglucinol Derivatives From Agrimonia Pilosa Ledeb by Counter-Current
Lulu Fu1, Chenghua Lu1, Shengqiang Tong1
1College of Pharmaceutical Science, Zhejiang University of Technology, 288 Liuhe Rd, Hangzhou 310014, P.R. China.
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%.
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