【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。更多还原

【Abstract】 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 NH₄Ac 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.更多还原