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作 者 ：熊耀坤,梁爽,洪燕龙,杨秀娟,沈岚,杜焰,冯怡

期 刊 ：中国中药杂志 2013年 38卷 12期 页码：1947.

关键词：反相高效制备液相；川芎；阿魏酸；洋川芎内酯I；洋川芎内酯H；

Keywords:preparative HPLC, Ligusticum chuanxiong, ferulic acid, senkyunolide I, senkyunolide H,

摘 要 ：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,5 μm),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.

Abstract:Preparative HPLC was used to prepare ferulic acid, senkyunolide I and senkyunolide H from Ligusticum chuanxiong. The separation was conducted on a Shim-Pack Prep-ODS (20.0 mm×250 mm, 5 μm) column with the mobile phase of methanol-0.2% glacial acetic acid(50∶50)at the flow rate of 5 mL·min^-1.The detection wavelength was 278 nm, and the purity of each compound was detected by HPLC analysis. Spectral data analyses including UV, ESI-MS and NMR were used to identify their structures. This method is simple, fast, which is suitable for preparation of standard reference of ferulic acid, senkyunolide I and senkyunolide H from L. chuanxiong and can meet the requirement of new drug research and development.

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