HPLC测定不同采收期川芎药材中5种药效成分的含量  

Quantitative determination of 5 active ingredients in different harvest periods of Ligusticum chuanxiong by HPLC

作　　者：刘金亮[1] 范巧佳[2] 郑顺林[1] 谭杰[1] 周娟[1] 袁继超[1] 杨世民[1] 孔凡磊[1] 

机构地区：[1]四川农业大学农学院农业部西南作物生理生态与耕作重点实验室,四川成都611130 [2]四川农业大学动物医学院,四川雅安625014

出　　处：《中国中药杂志》2014年第9期1650-1655,共6页China Journal of Chinese Materia Medica

摘　　要：该文建立了HPLC同时测定川芎药材中阿魏酸、洋川芎内酯I、洋川芎内酯H、洋川芎内酯A和藁本内酯含量的方法。用40％乙醇提取样品中的药效成分，采用Symmetry C18（4．6mm×250mm，5阻m）色谱柱，0—5min，乙腈－甲醇－1％冰醋酸（20：40：40），5～30min，乙腈-甲醇-1％冰乙酸（60～100：0：40—0）为流动相，流速1mL·min^-1，检测波长0～4．3min，321nm，4．31—30min，275nm，柱温35℃，进样体积10山，应用安捷伦1100系列液相色谱仪进行测定。5种药效成分的分离效果良好，在相应的浓度范围内与峰面积有良好的线性关系，相关系数均大于0．99，加样回收率（n=6）均在94．44％～103．1％。该方法应用于研究都江堰产区（海拔600nl左右）不同采收期对川芎阿魏酸和4种内酯类物质含量的影响，试验在4月15日（栽后245d）至5月30日（290d）内设置了10个采收期，发现5种药效成分的含量与采收期（栽后天数）均呈二次或三次函数关系，随着采收期的推迟而先增后减，阿魏酸、洋川芎内酯I、洋川芎内酯H、洋川芎内酯A和藁本内酯的含量在栽后260～265d（4月30日至5月5日）最高。A simple and quick method is described for the determination of ferulic acid, senkyunolide I, senkyunolide H, senkyunolide A and ligustilide in rhizomes of Ligusticum chuanxiong. The 5 active ingredients in the sample was extracted using 40% ethanol and analyzed by reversed-phase high performance hquid chromatography （HPLC）. Chromatography separation was performed using Agilent 1100 series HPLC system with a Symmetry Cls column and gradient elution with a mixture of three solvents：solvent A, acetonitrile, solvent B, methanol and solvent C, 1% aqueous acetic acid, 0 min to 5 min A： B： C 20：40：40, 5 min to 30 min A： B： C 60 to 100： 0：40 to 0. The effluent was monitored using a VWD detector set at 321 nm （0-4. 3 min） and 275 nm （4. 31-30 min）. The flow rate was set at 1 mL·min^-1 and the injection valume was 10 μL. The column temperature was maintained at 35 ℃. The calibration curve was linear （r ≥0. 99） over the tested ranges. The average recovery was 94. 44%-103.1% （n = 6）. The method has been successfully applied to the analysis in different harvest periods of L. chuanxiong samples. In this paper, single-factor randomized block design to study the 5 components content of L. chuanxiong on ten collecting stages. For the L. chuanxiong collected from April 15th to May 30rd, the content of 5 ingredients increased primarily, and then decreased. Determine the appropriate harvest time has important significance to the promotion of the quality of L. chuanxiong.

关 键 词：川芎 HPLC 采收期 含量 

分 类 号：R284.1[医药卫生—中药学] O657.72[医药卫生—中医学]