Shu Yaping, Liang Yong, Liang Zhenjie, Zhao Xiaoyun, Zhu Xiaohua, Feng Wanlian, Liang Jianmei, Ito Yoichiro
Institute of Analytical Chemistry, School of Chemistry and Environment, South China Normal University, Guangzhou, China.
Department of medical technology, Shangqiu Medical College, Shangqiu, China.
J Liq Chromatogr Relat Technol. 2014;37(6):773-785. doi: 10.1080/10826076.2012.749501.
Genkwanin, a flavonoid which has anti-oxidant and anti-tumor activities, was isolated and purified from flowers of Sieb. et Zucc. in a large-scale by normal-phase flash chromatography (NPFC). Dried flower buds were extracted with methanol at room temperature and concentrated. The residues were suspended in water and first extracted with petroleum ether, and then chloroform. Genkwanin was concentrated in the chloroform and insoluble fractions. Under the target-guidance of thin layer chromatography (TLC) as well as solubility, a solvent system composed of cyclohexane-acetone (22:3, v/v) was selected. At a flow rate of 30 mL/min,the insoluble and chloroform fractions were separated to yield 1.5 g and 1.35 g of genkwanin with high purities of 98.3% and 98.6% by HPLC analysis, respectively. The chemical structure of the compound was identified by ESI-MS and NMR. Results of the present study indicated that NPFC was a large preparative-scale, speedy and simple process separation technology and it was feasible to find the appropriate proportion of solvent system by transformation from TLC condition.
芫花素是一种具有抗氧化和抗肿瘤活性的黄酮类化合物，通过正相快速柱色谱法（NPFC）从紫花洋地黄的花中大规模分离纯化得到。干燥的花芽在室温下用甲醇提取并浓缩。将残留物悬浮于水中，先用石油醚萃取，再用氯仿萃取。芫花素集中在氯仿和不溶部分。在薄层色谱（TLC）的目标导向以及溶解度的作用下，选择了由环己烷 - 丙酮（22:3，v/v）组成的溶剂系统。以30 mL/min的流速，分离不溶部分和氯仿部分，通过HPLC分析分别得到1.5 g和1.35 g纯度分别为98.3%和98.6%的高纯度芫花素。该化合物的化学结构通过ESI-MS和NMR鉴定。本研究结果表明，NPFC是一种大规模制备、快速且简单的过程分离技术，通过从TLC条件转化来找到合适的溶剂系统比例是可行的。
