川芎中欧当归内酯A的提取纯化与结构表征

Preparation and determination of levistolide A from Ligusticum chuanxiong Hort.

以川芎中的内酯成分得率为指标,选取提取温度、提取时间、液固比、药材颗粒度以及水解p H 5个因素,在单因素考察基础上采用正交实验对提取工艺进行优化,继而分离得到单体化合物,最后用液相色谱质谱(LC MS)联用技术及核磁共振仪(NMR)对产物进行结构表征。结果表明,最佳提取工艺条件为:提取温度30℃,提取时间50 min,液固比15 m L/g,药材颗粒度>150~180μm,水解p H=13.0,川芎内酯得率可达5.91%。在最佳工艺条件下制得的化合物进一步分离得到欧当归内酯A。

Factors affecting the extraction rate of lactone compounds from Ligusticum chuanxiong Hort.,such as extractive temperature and duration,the liquid to solid ratio,granularity and pH value of solvent,were investigated.The lactone compound obtained by isolation process was determined by liquid chromatography-mass spectrometry(LC-MS)and nuclear magnetic resonance(NMR).The optimization of extraction conditions were predicted from results of orthogonal experiments,and the optimized conditions for the lactone compound with the yield of 5.91%were as follows:extractive temperature of 30℃,duration of 50 min,liquid to solid ratio of 15 mL/g,particle size of>150-180μm and pH of 13.0.The compounds prepared under the optimized conditions were further isolated,its structural formula was proved to be levistolide A.