高速逆流色谱分离制备杭白菊中黄酮类成分(英文)

Preparative Isolation and Purification of Flavonoids from the Flower of Chrysanthemum morifolium Ramat. by High-speed Counter-current Chromatography

建立高速逆流色谱分离纯化杭白菊总黄酮结晶中芹菜素-7-O-芸香糖、木犀草素-7-O-葡萄糖、芹菜素-7-O-葡萄糖以及金合欢素-7-O-葡萄糖4种黄酮类化合物。高速逆流分离过程分为两步,分别采用乙酸乙酯-乙醇-水-乙酸(体积比4∶1∶5∶0.2)和氯仿-甲醇-水(体积比4∶3∶2)两个体系。在第一步中,100 mg的总黄酮结晶分离得到了11.2 mg的芹菜素-7-O-芸香糖、15.3 mg的木犀草素-7-O-葡萄糖、28.2 mg的芹菜素-7-O-葡萄糖。然后收集到尾吹液,旋蒸至干得到35 mg的浸膏。在第二步中,当采用氯仿-甲醇-水(体积比4∶3∶2)体系时,从35 mg的浸膏中分离纯化得到14.5 mg的金合欢素-7-O-葡萄糖。4个化合物的纯度分别为99.4%、93.6%、99.1%和99.5%,电喷雾电离质谱和氢、碳核磁共振波谱鉴定化合物的结构。

High-speed counter-current chromatography （ HSCCC） method for isolation and purification of flavonoids crystalloid, i. e. apigenin-7-O-rutinoside（ Ⅰ） , luteolin-7-O-glucoside（ Ⅱ） , apigenin-7-O-glucoside（ Ⅲ） and acacetin-7-O-glucoside（ Ⅳ） from Chrysanthemum morifolium Ramat. was established successfully. The separation was performed in two steps with two different types of solvent systems： ethyl acetate-ethanol-water-acetic acid （4：1：5：0. 2, v/v） and chloroform-methanol-water （4：3：2, v/v）. In the first separation step, 100 mg of the flavonoids crystalloid yielded 11. 2 mg of apigenin-7-O-rutinoside, 15. 3 mg of luteolin-7-O-glucoside, and 28. 2 mg of apigenin-7-O-glucoside. Then we collected tail blowing fluid and obtained 35 mg of extract by evaporation to dryness. In the second step, when we used [ chloroform-methanol-water （4：3：2, v/v）] solvent system to separate the 35 mg of extract, 14. 5 mg of acacetin-7-O-glucoside could be obtained. Their four compounds purities were 99. 4 %, 93. 6 %, 99. 1% and 99. 5%, respectively. Their structures were identified by ESI-MS, 1H NMR, and 13C NMR.