Purification method of rohitukine from the stem bark of Dysoxylum binectariferum

红果樫木树皮中罗希吐碱的纯化方法(英文)

To develop a simple and rapid purification method of rohitukine from the stem bark of Dysoxylum binectariferum. A L9 （34） orthogonal test was designed to optimize the extraction condition. Rohitukine in the plant extract was purified by using solvent-solvent partition and cation exchange resion （CER）. Five different types of packing materials, including XAD-2 resin, polyamide, Sephadex LH-20, ODS and CER, were compared and CER showed the best capacity for rohitukine separation. The purification procedure was optimized as follows： the plant material powder was extracted with 70% ethanol （v/m = 60） by ultrasonic agitation for 60 min, then the 70% ethanol extract was dissolved in aqueous solution （pH 1, adjusted with 0.5 mol/L HCl） and extracted with equal volume of n-butanol. The aqueous layer was retained and the pH was adjusted to 10 with 25% aqueous ammonia and a solventsolvent partition was performed with equal volume of n-butanol. The obtained n-butanol extract was dissolved in aqueous solution （pH 1, adjusted with 0.5 mol/L HCl）, and purified by a CER column eluting with H2O and 70% ethanol （pH 10, adjusted with 25% aqueous ammonia）, successively. Rohitukine existed in 70% ethanol eluate, with a purity up to 53.3%. The method developed in this study provides a simple and rapid approach for the preparation of rohitukine from the stem bark ofD. binectariferum.

建立红果樫木树皮中罗希吐碱的提取工艺。利用L9（3^4）正交实验确定罗希吐碱的提取条件，比较5种填料（XAD-2树脂，聚酰胺，葡聚糖凝胶LH-20，ODS和阳离子交换树脂）以及液液萃取技术对红果樫木提取物中罗希吐碱的分离效果。提取条件确定为：药材用70％乙醇（v／m=60）超声提取60分钟；提取物溶解于酸水溶液（0，5mol／L HCl调pH1），经等体积正丁醇萃取除去杂质；25％氨水调剩余水溶液pH10，再经等体积正丁醇萃取；正丁醇萃取物溶解于酸水溶液（0．5mol／L HCl调pH1），经阳离子交换树脂色谱分离，水和70％乙醇（pH10，25％氨水调节）为洗脱剂。罗希吐碱存在于70％乙醇洗脱物中，含量可达到53．3％。该工艺为从红果樫木树皮中制备罗希吐碱提取物提供一种简单有效的方法。