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利用制备型反相高效液相色谱(pre-HPLC),从川芎中分离制备阿魏酸、洋川芎内酯I和洋川芎内酯H,并进行结构鉴定。制备色谱条件:Shim-Pack Prep-ODS色谱柱(20.0 mm×250 mm,5μm),流动相为甲醇-0.2%冰醋酸溶液(50∶50),体积流量5 mL.min-1,进样体积1 mL,检测波长278 nm。经分析HPLC测定纯度,用UV,MS,NMR等对其进行结构鉴定。鉴定结果确定为阿魏酸、洋川芎内酯I和洋川芎内酯H。质量分数大于98%。该方法简便、快速,制备阿魏酸、洋川芎内酯I和洋川芎内酯H质量分数很高,既适于用作对照品,也可满足新药研发的需要。
Preparative reversed-phase high performance liquid chromatography (pre-HPLC), isolated from the Ligustici chuanxiong Ferulic acid, Yang Chuanxiong lactone I and Chuanxiong L, and structural identification. Preparation of chromatographic conditions: Shim-Pack Prep-ODS column (20.0 mm × 250 mm, 5μm), the mobile phase methanol -0.2% glacial acetic acid solution (50:50), the volume flow rate of 5 mL.min-1, 1 mL, detection wavelength 278 nm. The purity was determined by analytical HPLC and identified by UV, MS, NMR and the like. Identification of the results identified as ferulic acid, Yang Chuanxiong lactone I and Chuanxiong lactone H. The mass fraction is more than 98%. The method is simple and rapid, and the preparation of the ferulic acid, the yangchongxiong lactone I and the yangchongxiong lactone H has a high mass fraction, which is suitable both for the reference substance and for the research and development of new drugs.