制备高效液相色谱法分离补骨脂中的补骨脂苷和异补骨脂苷*

Preparation of psoralenoside and isopsoralenoside by preparative high performance liquid chromatography from psoralen

关键词:  补骨脂苷  异补骨脂苷  制备高效液相色谱

Key words:  psoralenoside  isopsoralenoside  preparative HPLC

摘要:

[目的] 建立制备高效液相色谱法(HPLC)分离纯化补骨脂中补骨脂苷和异补骨脂苷的方法。[方法] 补骨脂药材用乙酸乙酯提取后再经甲醇提取,浓缩甲醇提取液成浸膏,水混悬浸膏,过AB-8大孔树脂,收集水洗脱部分,处理后进行高效液相分离制备。采用汉邦C18制备柱(20mm×250mm,5μm);流动相:乙腈-0.05%甲酸水(15:85);体积流量:8.0mL/min;检测波长:246nm;柱温:室温。[结果] 从补骨脂中分离得到了补骨脂苷和异补骨脂苷两个化合物。[结论] 该方法简便、快速,分离得到的化合物采用HPLC归一化法定量,质量分数大于96%,可用做补骨脂苷和异补骨脂苷的制备。

Abstract:

[Objective] To establish a method for isolation and purification of psoralenoside and isopsoralenoside by preparative HPLC.[Methods] After being extracted with ethyl acetate, the seeds of Psoralea corylifolia was extracted by methanol. Then the methanol extracts were evaporated to dryness under reduced pressure. The extract was resuspended by water and separated via AB-8 type macroporous resin column chromatography, then eluted by distilled water. Fraction collected was concentrated to a certain volume. The solution was isolated and purified by preparative HPLC. The method was performed on a Hanbon preparative column C18 （20 mm×250 mm,5 μm）using the elution of acetonitrile and water containing 0.05% formic acid （15:85）at room temperature. The flow rate was 8.0 mL/min and the wavelength of measurement was 246 nm. [Resutls] Two compounds were isolated from the seeds of Psoralea corylifolia. [Conclution] The purity of the product quantitated by normality was over 96%. The developed method is simple and rapid, which could be used for preparation of psoralenoside and isopsoralenoside.