明日叶中4-羟基德里辛和黄色当归醇的提取纯化及鉴定

Extraction,Prification and Identification of 4-Hdroxyderricin and Xanthoangelol,from Angelica keiskei

明日叶是一种药食两用的绿色蔬菜,极具开发价值。本文以明日叶为原料,首先通过单因素以及正交试验,优化了明日叶中4-羟基德里辛(4-HD)和黄色当归醇(XAG)的提取工艺参数。其次采用乙酸乙酯萃取、硅胶柱层析以及半制备液相相结合的方法对粗提液中的4-HD和XAG进行分离纯化,并对纯化物的结构及纯度进行分析。结果表明:最佳提取条件为:提取2次、提取溶剂80%乙醇、提取温度55℃、提取时间90 min、料液比1∶10。此时,4-HD得率为1.82 mg/g,XAG得率为2.12 mg/g。HPLC-MS及NMR分析结果表明:纯化得到的两种物质正是4-HD和XAG,纯度分别为99.08%和98.92%。

Angelica keiskei is a kind of high nutritional vegetable used as both food and medicine.In this study,single factor experiment and orthogonality test were developed to optimize the extraction process of 4-hydroxyderricin(4-HD)and xanthoangelol(XAG),from Angelica keiskei.The optimized extraction conditions were as follows:times of extraction,2 times;extract solvent,80%ethanol;extraction temperature,55℃;extraction time,90 min;ratio of solid to liquid,1∶10.Under these optimized conditions,the extraction yield of 4-HD and XAG were 1.82 mg/g and 2.12 mg/g,respectively.Further,isolation and purification of 4-HD and XAG by silica gel column and semi-preparative C18 column was also described,and then the structures and purities were identified by HPLC-MS and NMR.Results showed that 4-HD at 99.08%purity and XAG at 98.92%purity were obtained.