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目的:建立从贯叶连翘中快速分离制备高纯度金丝桃素的方法。方法:市售贯叶连翘提取物经聚酰胺树脂预处理后直接进行高速逆流色谱分离纯化,以正己烷-乙酸乙酯-甲醇-水(3∶5∶3∶5)为溶剂系统,所得产物化学结构由1H NMR和13C NMR鉴定,纯度经高效液相色谱外标法检测。结果:在此条件下,经一步分离从300 mg预处理粗提物中可得到13.6mg纯度为95%的金丝桃素。结论:该法简便、快速、所得产物纯度高,适合于高纯度金丝桃素的制备。
Objective: To establish a method for the rapid separation of Hypericin from Hypericum perforatum. Methods: The extract from Hypericum perforatum was pretreated with polyamide resin and purified directly by high-speed countercurrent chromatography. The product was eluted with n-hexane-ethyl acetate-methanol-water The structure was identified by 1H NMR and 13C NMR and the purity was determined by HPLC external standard method. Results: Under this condition, 13.6 mg of hypericin with a purity of 95% was obtained from 300 mg of the pretreated crude extract in one step. Conclusion: The method is simple, rapid, high purity of the resulting product, suitable for the preparation of high purity hypericin.