茯砖茶中黄酮类化合物的分离与鉴定

本文采用高速逆流色谱与制备液相联用技术分离茯砖茶中黄酮类化合物。高速逆流色谱以正丁醇/乙酸乙酯/乙腈/0.5%乙酸水=12:2:3:15(V/V)为溶剂体系，将茯砖茶提取物分成7个流分，各流分经制备液相分离，获到19个化合物，利用波谱方法鉴定了15个化合物，均为黄酮类化合物：分别为芹菜素-6,8-二-C-β-D-葡萄糖(1)，芹菜素-6-C-α-L-阿拉伯糖-8-C-β-D-葡萄糖(2)，芹菜素-7-O-β-D-半乳糖-8-C-β-D-葡萄糖苷(3)，槲皮素-3-O-葡萄糖-(1-3)-鼠李糖-(1-6)-葡萄糖(4)，山奈酚-3-O-β-D-葡萄糖-(1-3)-α-L-鼠李糖-(1-6)-β-D-葡萄糖苷(5)，芹菜素-7-O-α-L-鼠李糖-8-C-β-D-半乳糖(6)，芦丁(7)，山奈酚-3-O-α-L-鼠李糖(1-6)-β-D-葡萄糖苷(8)，Camelliquercetiside A(10)，杨梅素3-O-β-D-葡萄糖苷(12)，异牡荆苷(13)，牡荆苷(15)，槲皮素3-O-β-D-葡萄糖苷(16)，Camelliquercetiside C(17)，山奈酚-3-O-β-D-半乳糖苷(18)，其中化合物3和6为新黄酮碳苷化合物，化合物1为茶叶中首次发现。
A method for the preparative separation of flavone compounds from Fuzhuan tea using high-speed counter-current chromatography coupled with high-performance liquid chromatography (HSCCC-HPLC) is established in this study. The n-butanol-ethyl acetate-cetonitrile-0.5% acetic acid (12:2:3:15,V/V/) was used as the solvent system for HSCCC, and seven fractions were first separated by HSCCC. Subsequently, each fraction was isolated by the preparative HPLC and 19 compounds were obtained. Fifteen compounds were identified by the spectral methods and all of them were flavonoids: apigenin-bis-6,8-C-β-D-glucopyranoside (1), apigenin-6-C-α-L- arabinopyranosyl-8-C-β-D-glucopyranoside (2), apigenin-7-O-β-D-galactopyranosyl-8-C-β-D-glucopyranoside (3), quercetin-3-O-β-D- glucopyranosyl-(1-3)-L-rhamnopyranosyl-(1-6)-β-D-glucopyranoside (4), kaempferol-3-O-β-D-glucopyranosyl-(1-3)-α-L- rhamnopyranosyl- (1-6)-β-D-glucopyranoside (5), apigenin-7-O-α-L-rhamnopyranosyl -8-C-β-D-galactopyranoside (6), rutin (7), kaempferol-3 -O-α-L- rhamnopyranosyl-(1-6)-β-D-glucopyranoside (8), camelliquercetiside A (9), myricetin-3-O-β-D-glucopyranoside (10), isovitexin (11), vitexin (12), quercetin-3-O-β-D-glucopyranoside (13), camelliquercetiside C (14), kaempferol-3-O-β-D-galactopyranoside (15). Among them, compound 3 and compound 6 were new C-glycosyl flavones and compound 1 was isolated from tea for the first time.