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1.江西中医药大学 药学院,南昌 330004;
2.江西中医药大学 研究生院,南昌 330004;
3.樟树市人民医院,江西 樟树 331200;
4.江西中医药大学 附属医院,南昌 330006
朱伶俐,在读硕士,从事天然药物分离与活性物质的筛选研究,E-mail:jzzll99@126.com
刘峰,硕士,副主任中医师,从事临床教学与科研工作,Tel:0791-86817063,E-mail:liufeng019369@163.com;
刘华,博士,教授,博士生导师,从事天然产物的药效物质基础及活性研究,E-mail:winner616@163.com
收稿日期:2018-10-21,
网络出版日期:2018-12-19,
纸质出版日期:2019-07-20
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朱伶俐, 艾志福, 徐丽, 等. 桂枝化学成分的分离鉴定[J]. 中国实验方剂学杂志, 2019,25(14):173-178.
Ling-li ZHU, Zhi-fu AI, Li XU, et al. Isolation and Identification of Chemical Constituents from Cinnamomi Ramulus[J]. Chinese journal of experimental traditional medical formulae, 2019, 25(14): 173-178.
朱伶俐, 艾志福, 徐丽, 等. 桂枝化学成分的分离鉴定[J]. 中国实验方剂学杂志, 2019,25(14):173-178. DOI: 10.13422/j.cnki.syfjx.20190712.
Ling-li ZHU, Zhi-fu AI, Li XU, et al. Isolation and Identification of Chemical Constituents from Cinnamomi Ramulus[J]. Chinese journal of experimental traditional medical formulae, 2019, 25(14): 173-178. DOI: 10.13422/j.cnki.syfjx.20190712.
目的:
2
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:
2
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(
1
H-NMR,
13
C-NMR,MS)等进行结构鉴定。
结果和结论:
2
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。
Objective:
2
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:
2
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:
2
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.
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