柱色谱-高速逆流色谱法分离纯化虎杖中大黄素-8-O-β-D-吡喃葡萄糖苷  

Separation and purification of emodin-8-O-β-D-glucopyranoside from Polygoni Cuspidati Rhizoma et Radix by column and high-speed counter-current chromatography

作　　者：赵东梅[1] 王威[1] 刘坤[1] 邵延琳 刘洋[1] 刘小红[1] 高华[1] 高琪[1] 

机构地区：[1]青岛大学药学院,山东青岛266021

出　　处：《中草药》2016年第12期2118-2122,共5页Chinese Traditional and Herbal Drugs

基　　金：山东省重点研发计划(2015GSF119001)

摘　　要：目的建立从虎杖药材中高效制备分离大黄素-8-O-β-D-吡喃葡萄糖苷(EG)的方法。方法采用大孔吸刚树脂柱色谱和ODS柱色谱分离目标组分,高速逆流色谱(HSCCC)纯化目标化合物,质谱和核磁共振波谱数据鉴定结构,HPLC不加校正因子的主成分自身对照法检测纯度。结果优化确定以二氯甲烷-醋酸乙酯-甲醇-水(8:1:6:5)为HSCCC溶剂系统,上相为固定相,下相为流动相,纯化制备了符合定量测定用要求的EG对照品,HPLC法检测质量分数大于98%。结论方法适于从虎杖药材中大量制备高纯度EG,为含有该成分的天然产物及其制剂质量评价提供对照物质。Objective To develop an effective and rapid method for the preparation of emodin-8-O-β-D-glucopyranoside （EG） reference substance from Cuspidati Rhizoma et Radix （PCRR）. Methods The target fraction was isolated by macroporous resin column chromatography and ODS column chromatography, and then the target compound was purified by high-speed counter-current chromatography （HSCCC）. The structure was identified by ESI-MS and NMR spectral techniques, and its purity was determined by HPLC analysis using the main component self-comparison with no correction factor method. Results A solvent system that consisted of dichloromethane-ethyl acetate-methanol-water （8 ： 1 ： 6 ： 5） was applied to the separation based on assessment using HPLC partition coefficient method. The upper phase was used as the stationary phase, while the lower phase was used as the mobile phase. The reference substance of EG was prepared, and its purity was up to 98% in line with the standard of quantitative analysis. Conclusion The method is suitable for the preparation of EG from PCRR, which provides a basis for the quality control of natural product and their preparations.

关 键 词：虎杖 大黄素-8-O-β-D-吡喃葡萄糖苷 高速逆流色谱 分离纯化 大孔吸附树脂 HPLC 

分 类 号：R284.2[医药卫生—中药学]