桂枝化学成分的分离鉴定

目的:明确桂枝的活性组分,对75%乙醇提浸膏进行系统化学成分分离与纯化,以期找到抑制necroptosis的目标小分子化合物。方法:取干燥桂枝20 kg,粉碎后用75%乙醇冷浸提取,提取4次,7 d 1次,减压回收溶剂得到总浸膏。将所得总浸膏,运用D101大孔吸附树脂柱色谱进行分离,依次用水,30%乙醇,50%乙醇,70%乙醇,90%乙醇洗脱,减压回收溶剂得水部分,30%乙醇部分,50%乙醇部分,70%乙醇部分,90%乙醇部分。对30%乙醇部分,50%乙醇部分联合采用常压硅胶柱色谱,LH-20型羟丙基葡聚糖凝胶(Sephadex LH-20)柱色谱,高压制备色谱,重结晶等方法进行分离纯化,并根据单体化合物理化性质与波谱学数据(~1H-NMR,~(13))C-NMR,MS)等进行结构鉴定。结果和结论:从桂枝中分离得到13个化合物,分别鉴定为(+)-丁香脂素(1),(+)-南烛木树脂酚(2),山橘脂酸(3),裂异落叶松脂醇(4),ovafolinin B(5),原儿茶醛(6),原儿茶酸(7),丁香醛(8),香草酸(9),原儿茶酸乙酯(10),丁香酸(11),没食子酸乙酯(12),2-(3',4'-二羟苯基)-1,3-胡椒环-5-醛(13)。其中1～5,10～13为首次从该植物中分离得到。

Isolation and Identification of Chemical Constituents from Cinnamomi Ramulus

Objective:The research group found in the early stage that the 75%alcohol extract of the Cinnamomi Ramulus had a significant physiological activity in inhibiting necroptosis by screening out the self-built sample library of 100 kinds of traditional Chinese medicines in Jiangxi. To identify the active components and find the target compounds,the 75%alcohol extracts of Cinnamomi Ramulus were isolated and studied systemically in chemistry. Method:The 20 kg dry Cinnamomi Ramulus was crushed into coarse powder,and extracted with 75%alcohol for four times, one time every 7 d. Then total extracts were obtained after solvent was recycled under decompression. The extract was separated by D101 macroporous resin column chromatography and eluted by water,30%ethanol,50%ethanol,70%ethanol,90%ethanol,so as to get the corresponding fraction finally. The compounds in the 30%ethanol and 50%ethanol fraction were isolated and purified by chromatography on silica gel,Sephadex LH-20 column and high pressure preparative chromatography,and their structures were determined according to physicochemical properties and spectral analysis. Result and Conclusion:Thirteen compounds were isolated and identified as (+)-syringaresinol (1),(+)-lyoniresinol (2),spicatolignan B (3),(-)-secoisolariciresinol (4),ovafolinin B (5),protocatechualdehyde (6),protocatechuic acid (7),syringaldehyde (8),vanillic acid (9),ethyl protocatechuate (10),syringic acid (11),ethyl gallate (12),2-(3'',4''-dihydroxyphenyl)-1,3-pepper ring-5-aldehyde (13). Compounds 1-5,10-13 were isolated from this plant for the first time.