高速逆流色谱在分离纯化木蝴蝶活性成分中的线性放大  

Linear scale-up of the separation of active components from Oroxylum indicum using high-speed counter-current chromatography

作　　者：袁媛[1] 骆厚鼎[2] 陈俐娟[2] 

机构地区：[1]四川大学化学工程学院,四川成都610065 [2]四川大学生物治疗国家重点实验室,四川成都610041

出　　处：《色谱》2008年第4期489-493,共5页Chinese Journal of Chromatography

摘　　要：利用高速逆流色谱分离纯化中草药木蝴蝶乙酸乙酯粗提物中的黄酮类活性成分,并将分离规模从分析型线性放大到制备型,以获得大量的活性成分,为进一步的药物筛选提供物质基础。实验在分析型高速逆流色谱上对分离参数进行了系统优化,并将优化条件放大到制备型高速逆流色谱上对911.6mg木蝴蝶乙酸乙酯粗提物进行分离,得到5种化合物,经高效液相色谱、电喷雾电离质谱和核磁共振氢谱、碳谱分析鉴定,分别为白杨素(160.9mg,纯度为97.3%)、黄芩素(130.4mg,纯度为97.6%)、黄芩素-7-O-葡萄糖苷(314.0mg,纯度为98.3%)、黄芩素-7-O-双葡萄糖苷(179.1mg,纯度为99.2%)和一种新的白杨素双葡萄糖苷(21.7mg,纯度为98.8%)。该放大过程不仅将处理量提高了53倍,还保持了在分析型设备上的分离度和分离时间。该工作为天然产物的研究提供了一个高效的分离纯化方法。High-speed counter-current chromatography was used to separate and purify flavonoids from the ethyl acetate extract of Oroxylum indicum. After the optimization of separation conditions on analytical instrument, including the two-phase solvent system, rotation speed, flow rate, sample volume and sample concentration, a linear scale-up procedure was performed at preparative grade. Chrysin （ 160.9 rag, 97.3% in purity）, baicalein （ 130.4 mg, 97.6% in purity）, baicalein-7-O-glucoside （314.0 mg, 98.3% in purity）, baicalein-7-O-diglucoside （ 179. 1mg, 99.2% in purity）, and a new chrysin-diglucoside （21.7 mg, 98.8% in purity） were obtained from 911.6 mg ethyl acetate extract of Oroxylum indicum by only one step. These five compounds were identified using high performance liquid chromatography, mass spectrometry and nuclear magnetic resonance. With the improvement of the throughput for 53 times after such a scale-up, the resolution and the separation time were kept as the same as those of the analytical grade separation. Therefore, the linear scale-up provided an efficient method for the separation of natural products.

关 键 词：高速逆流色谱 线性放大 黄酮 木蝴蝶 中草药 

分 类 号：O658[理学—分析化学]