应用反相高效制备液相同时分离川芎中阿魏酸、洋川芎内酯I和H  

Preparation of ferulic acid,senkyunolide I and senkyunolide H from Ligusticum chuanxiong by preparative HPLC

作　　者：熊耀坤[1,2] 梁爽[1] 洪燕龙[1] 杨秀娟[1] 沈岚[1] 杜焰[1] 冯怡[1] 

机构地区：[1]上海中医药大学中药现代制剂技术教育部工程研究中心,上海201203 [2]江西中医学院,江西南昌330004

出　　处：《中国中药杂志》2013年第12期1947-1950,共4页China Journal of Chinese Materia Medica

基　　金：国家教育部科学技术研究重点项目(211060);国家教育部高等学校博士学科点专项科研基金(20123107120009);上海市科委上海市自然科学基金项目(11ZR1434500);上海市教委重点学科项目(J50302);上海市教委创新项目(重点)(11zz112,12ZZ124)

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,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 HPLC was used to prepare ferulic acid, senkyunolide I and senkyunolide H from Ligusticurn chuanx- iong. The separation was conducted on a Shim-Pack Prep-ODS （20.0mm×250mm,5μm） column with the mobile phase of metha- nol-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 deteeted by HPLC analysis. Spectral data analyses including UV, ESI-MS and NMR were used to identify their struc- tures. This method is simple, fast, which is suitable for preparation of standard reference of ferulie acid, senkyunolide Ⅰ and senkyuno- lide H from L. chuanxiong and can meet the requirement of new drug research and development.

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 

分 类 号：R284[医药卫生—中药学]