Genkwanin, a flavonoid that has anti-oxidant and antitumor activities, was isolated and purified from flowers of Daphne genkwa 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 experiments, 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.

中文翻译：

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简单高效大规模制备芫花素的方法研究。等ZUCC。使用正相快速色谱

Genkwanin 是一种具有抗氧化和抗肿瘤活性的黄酮类化合物，是从 Daphne genkwa Sieb 的花中分离纯化出来的。等祖克。通过正相快速色谱法 (NPFC) 进行大规模分析。在室温下用甲醇提取干燥的花蕾并浓缩。将残余物悬浮在水中，首先用石油醚萃取，然后用氯仿萃取。芫花宁浓缩在氯仿和不溶部分中。在薄层色谱（TLC）和溶解度实验的目标引导下，选择环己烷-丙酮（22：3，v/v）组成的溶剂体系。在30mL/min的流速下，分离不溶物和氯仿部分，分别得到1.5g和1.35g芫花素，经HPLC分析，纯度分别为98.3%和98.6%。通过ESI-MS和NMR鉴定了该化合物的化学结构。本研究结果表明，NPFC是一种制备规模大、速度快、工艺简单的分离技术，通过TLC条件改造找到合适的溶剂体系比例是可行的。