摘要
首次利用离线二维高速逆流色谱法从湖北海棠叶中分离制备3种黄酮化合物。第一次分离以正己烷-乙酸乙酯-甲醇-水(1:4:1:4,v/v)为溶剂系统,在2.5 h内分离得到纯度为96.5%的3-羟基根皮苷;第二次分离以正己烷-乙酸乙酯-甲醇-0.1mol/L Cu2+水溶液(1:4:1:4,v/v)为溶剂系统,在2.0 h内分离得到纯度98.1%的槲皮素和纯度98.9%的根皮苷。最终,成功从200 mg湖北海棠叶乙酸乙酯萃取部位中制备25.4mg的3-羟基根皮苷,8.5 mg的槲皮素,31.3 mg的根皮苷。利用HPLC、ESI-MS和1H NMR对分离物进行结构鉴定。
Three flavonoids were successfully separated and purified from the dried Malus hupehensis leaves for the first time by off- line two - dimensional high - speed countercurrent chromatography （ off - line 2D HSCCC）. Hexane - ethyl acetate - methanol - water （ 1：4 ： 1：4, v/v） was selected as the optimum two - phase solvent system for the first dimensional HSCCC separation and 3 -hydroxy phloridzin was obtained with purity of 96.5% in 2.5 h. Then quereetin and phlorid- zin were further isolated and purified in 2.0 h using the second dimensional HSCCC with hexane - ethyl acetate - methanol -0. lmol · L-1Cu2＋ （1：4：1：4,v/v） as the optimum two - phase solvent system, and the purities were 98.1% and 98. 9%, respectively. As a result, 25.3 mg 3-hydroxy phloridzin, 8.5rag quereetin, 31.3 mg phloridzin were yielded from 200 mg crude sample of Malus hupeheusis leaves. The chemical structures were identified by using HPLC, ESI - MS and 1H NMR.
出处
《江西化工》
2014年第1期115-121,共7页
Jiangxi Chemical Industry
关键词
湖北海棠叶
离线二维高速逆流色谱
乙酸乙酯萃取
黄酮
Malus hupehensis leaves off - line two - dimensional high - speed countercurrent chromatography ethyl ac-etate extract flavonoids
