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纸质出版日期:2018
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宁火华, 袁铭铭, 邬秋萍, 等. 多花黄精化学成分分离鉴定[J]. 中国实验方剂学杂志, 2018,24(22):77-82.
NING Huo-hua, YUAN Ming-ming, WU Qiu-ping, et al. Identification of Chemical Constituents from [J]. Chinese journal of experimental traditional medical formulae, 2018, 24(22): 77-82.
宁火华, 袁铭铭, 邬秋萍, 等. 多花黄精化学成分分离鉴定[J]. 中国实验方剂学杂志, 2018,24(22):77-82. DOI: 10.13422/j.cnki.syfjx.20181912.
NING Huo-hua, YUAN Ming-ming, WU Qiu-ping, et al. Identification of Chemical Constituents from [J]. Chinese journal of experimental traditional medical formulae, 2018, 24(22): 77-82. DOI: 10.13422/j.cnki.syfjx.20181912.
目的:对多花黄精根茎的正丁醇和二氯甲烷部位的化学成分进行分离,并对所得化合物进行结构鉴定。方法:多花黄精的干燥根茎经江西建昌帮传统炮制方法-炆法炮制,60℃烘干,粉碎,70%乙醇浸泡1 h,加热回流提取2次,滤过,提取液合并浓缩,依次用两倍体积的二氯甲烷、乙酸乙酯、正丁醇溶液分别萃取3次,萃取液分别减压浓缩至干,得二氯甲烷萃取部分、乙酸乙酯萃取部分和正丁醇萃取部分。用大孔吸附树脂,反复硅胶柱,LH-20型羟丙基葡聚糖凝胶(Sephadex LH-20),YMC-HPLC制备柱等技术对多花黄精根茎的正丁醇和二氯甲烷部位进行分离纯化,根据化合物的理化常数测定及波谱数据分析鉴定化合物结构。结果:从多花黄精根茎的正丁醇和二氯甲烷萃取部位中分离得到14个化合物,分别鉴定为(25S)spirostan-5-en-12-one-3-O-D-glucopyranosyl-(1→2)-O-[β-D-xylopyranosyl(1→3)]-O-β-D-glucopyranosyl(1→4)-β-D-galactopyranoside(1),(25S)spirostan-5-en-12-one-3-O-β-D-glucopyranosyl-(1→2)-O-[β-D-glucopyranosyl-(1→3)]-O-β-D-glucopyranosyl-(1→4)-β-D-galactopyranoside(2),邻苯二甲酸二丁酯(3),胡萝卜苷(4),β-谷甾醇(5),hypofuran B(6),(25R)-3-β-hydroxyspirost-5-en-12-one(7),(+)-medioresinol(8),黄精碱A(9),5-羟甲基糠醛(10),5-羟基麦芽酚(11),2-(4-羟苯基)乙醇(12),1H-吲哚-3-甲醛(13),黄精碱B(14)。结论:化合物4,5,9,14为首次从多花黄精中分离得到,化合物6,8,12,13为首次从黄精属植物中分离得到。该研究为多花黄精综合开发及天然植物药理活性研究提供化学依据和物质参考。
Objective:To separate the chemical constituents of n-butanol and dichloromethane ether fractions from Polygonatum cyrtonema and identify the structures of the compounds. Method:Rhizomes of P. cyrtonema were dried and crushed at 60℃ saccording to the traditional processing method of Jiangxi Jianchang
soaked by 70% ethanol for 1 hour
extracted for 2 times
filtered
and then extracted by three times with the two times volume of dichloromethane
ethyl acetate and n -butanol respectively. The extraction solution was decompressed and concentrated to obtain the dichloromethane fraction
ethyl acetate fraction and n -butanol fraction. The n -butanol and dichloromethane ether fractions from P. cyrtonema were isolated by macroporous adsorption resin chromatography
silica gelcolumn
re-crystallization
Sephadex LH-20 column
reversed phase high-performance liquid chromatography and their structures were identified according to physicochemical properties and spectral evidences. Result:Fourteen compounds were isolated from n -butanol and dichloromethane ether fractions of Polygonatum cyrtonema and elucidated as (25 S)spirostan-5-en-12-one-3-O-D -glucopyranosyl-(1→2)-O -[β-D -xylopyranosyl(1→3)]-O-β-D -glucopyranosyl(1→4)-β-D -galactopyranoside(1)
(25 S)spirostan-5-en-12-one-3-O-β-D -glucopyranosyl-(1→2)-O -[β-D -glucopyranosyl-(1→3)]-O-β-D -glucopyranosyl-(1→4)-β-D -galactopyranoside(2)
dibutyl phthalate(3)
daucosterol(4)
β -Sitosterol(5)
hypofuran B(6)
(25 R)-3-β-hydroxyspirost-5-en-12-one(7)
(+)-medioresinol(8)
polygonatine A(9)
5-hydroxymethyl furfural(10)
5-hydroxy maltol(11)
2-(4-hydroxyphenyl)-ethanol(12)
1H-indole-3-carboxaldehyde(13)
and polygonatine B(14). Conclusion:Compounds 4
5
9 and 14 were firstly obtained from P. cyrtonema
and compounds 6
8
12 and 13 were isolated from the plants of Polygonatum for the first time
providing chemical basis and foundation for the comprehensive development and the research on active substances of natural plant.
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