高速逆流色谱法从蛇床子中制备分离和纯化香豆素
Preparative isolation and purification of coumarins from Cnidium monnieri (L.) Cusson by high-speed counter-current chromatography.
作者信息
Liu Renmin, Feng Lei, Sun Ailing, Kong Lingyi
机构信息
College of Chemistry and Chemical Engineering, Liaocheng University, 252059 Liaocheng, China.
出版信息
J Chromatogr A. 2004 Nov 5;1055(1-2):71-6. doi: 10.1016/j.chroma.2004.09.017.
A high-speed counter-current chromatography (HSCCC) method for separation and purification of coumarins from Cnidium monnieri (L.) Cusson was developed by using stepwise elution with a pair of two-phase solvent system composed of light petroleum-ethyl acetate-methanol-water at volume ratios of 5:5:5:5, 5:5:6:4 and 5:5:6.5:3.5. Five kinds of coumarins were obtained and yielded 7.6 mg of xanthotoxin(I), 7.6 mg of isopimpinellin(II), 9.7 mg of bergapten(III), 60.5 mg of imperatorin(IV), 50.6 mg of osthole(V) and 10.2 mg of one unknown compound from 150mg crude sample. The purity of these compounds was 95.0%, 99.6%, 99.7%, 100%, 100% and 98.1%, respectively, as determined by HPLC. Their structures were identified by 1H NMR.
采用由体积比为5:5:5:5、5:5:6:4和5:5:6.5:3.5的石油醚 - 乙酸乙酯 - 甲醇 - 水组成的两相溶剂系统进行梯度洗脱，建立了从蛇床子中分离纯化香豆素的高速逆流色谱（HSCCC）方法。从150mg粗样品中获得了5种香豆素，分别得到7.6mg花椒毒素（I）、7.6mg异茴芹内酯（II）、9.7mg佛手柑内酯（III）、60.5mg欧前胡素（IV）、50.6mg蛇床子素（V）和10.2mg一种未知化合物。通过高效液相色谱法测定，这些化合物的纯度分别为95.0%、99.6%、99.7%、100%、100%和98.1%。它们的结构通过1H NMR进行了鉴定。
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