反相液相色谱法制备纯化柠檬苦素类似物配糖体

Research on the Separation of Limonoid Glucosides by Reversed-Phase Preparative High Performance Liquid Chromatography

利用反相制备液相色谱结合吸附树脂柱色谱和离子交换色谱方法 ,从甜橙种子的提取物中纯化制备了一种柠檬苦素类似物配糖体 ,经 NMR测定为奥巴叩酮配糖体。

Obacunone\|17\|β\|D\|glucopyranoside (OG) was isolated from the seeds of Citrus Sinensis Osbeck by using solvent extraction, classical polymer adsorption column separation and weak base anion ion\|exchange separation, OG was finally purified by C_18 reversed-phase preparative high performance liquid chromatography and was identified by thin-layer chromatography. The purity of OG was analyzed by analytical reversed-phase HPLC. At last the structure of OG was determined by1H and13C nuclear magnetic resonance spectrometry (NMR). In this work, the conditions of the reversed\|phase preparative HPLC technique to purify limonoid glucosides was optimized. The reversed\|phase preparative HPLC on a C_18 column with a mobile phase of acidic acetonitrile\|water (about 0.2% TFA, V/V) at pH 3 enabled the baseline separation of limonoid glucosides in the extract. The results show that OG is the predominant limonoid glucoside in the seeds of Citrus Sinensis Osbeck and nomilin glucoside is the second one. The results also show that the classical polymer adsorption column separation and weak base anion ion\|exchange separation are effective for purifying limonoid glucosides.