反相高效液相色谱法制备洋川芎内酯Ⅰ  

Preparation of Senkyunolide Ⅰ by Reversed-Phase High Performance Liquid Chromatography

作　　者：张晓哲[1] 徐青[1] 肖红斌[1] 梁鑫淼[1] 

机构地区：[1]中国科学院大连化学物理研究所,辽宁大连116011

出　　处：《色谱》2004年第1期41-43,共3页Chinese Journal of Chromatography

摘　　要：建立了一种快速、高效制备洋川芎内酯Ⅰ的工艺路线。以醋酸铵为改性剂,利用台阶梯度洗脱和MCI树脂柱脱盐的方式,通过反相高效液相色谱法制备,从川芎的95%(体积分数)乙醇提取物中快速分离到目标产物洋川芎内酯Ⅰ和副产物阿魏酸。经检测,二者的纯度均达到98%以上。该方法操作简便,能够排除由样品中阿魏酸所引起的峰交叉干扰,上样量大,适合于洋川芎内酯Ⅰ的大量制备。A method for the isolation of senkyunolide Ⅰ from Chuanxiong with reversed-phase preparative high performance liquid chromatography (HPLC) is described. After 95% ethanol extract was obtained with solvent extraction and normal-phase silica column separation, a fraction containing senkyunolide Ⅰ was acquired and subjected to preparative HPLC for the isolation of target component. In the experiment a solvent system consisting of methanol-0.05 mol/L NH_4Ac aqueous solution was found effective to eliminate the interference of ferulic acid that was the major compound in the sample. Senkyunolide Ⅰ and ferulic acid were separated completely by using a stepwise gradient solvent system of 10% methanol in 10 min, and 60% methanol in 10-40 min. The subfractions were collected and subjected to an open MCI gel CHP-20P column for desalination respectively. Senkyunolide Ⅰ was obtained and the structure was identified by mass spectrometry (MS) and nuclear magnetic resonance (NMR). This method is effective and reliable for the preparation of senkyunolide Ⅰ from Chuanxiong.

关 键 词：洋川芎内酯Ⅰ 制备工艺 反相高效液相色谱法 阿魏酸 川芎 分离 纯化 

分 类 号：R284.2[医药卫生—中药学]