Zhang Xiaozhe, Xu Qing, Xiao Hongbin, Liang Xinmiao
Dalian Institute of Chemical Physics, The Chinese Academy of Sciences, Dalian 116011, China.
Se Pu. 2004 Jan;22(1):41-3.
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.
描述了一种采用反相制备高效液相色谱（HPLC）从川芎中分离川芎内酯I的方法。通过溶剂萃取和正相硅胶柱分离得到95%乙醇提取物后，获得含有川芎内酯I的馏分，并将其进行制备型HPLC以分离目标成分。实验中发现由甲醇 - 0.05 mol/L醋酸铵水溶液组成的溶剂系统可有效消除样品中主要化合物阿魏酸的干扰。使用10%甲醇在10分钟内、60%甲醇在10 - 40分钟内的梯度洗脱溶剂系统可将川芎内酯I和阿魏酸完全分离。收集各亚馏分并分别通过开放的MCI凝胶CHP - 20P柱进行脱盐处理。获得了川芎内酯I，并通过质谱（MS）和核磁共振（NMR）对其结构进行了鉴定。该方法对于从川芎中制备川芎内酯I有效且可靠。
