摘要
采用正相硅胶柱色谱、反相硅胶柱色谱、半制备型高效液相色谱和Sephadex LH-20凝胶柱色谱等分离技术对仿刺参(Apostichopus japonicus)内脏中的化学成分进行分离和纯化.通过1H NMR、13C NMR、HSQC、HMBC、1H-1H COSY、HR-ESI-MS等波谱技术,结合文献数据比对,从仿刺参内脏95％乙醇提取液中鉴定出14个单体化合物,分别为(E)-dec-5-en-1-yl sulfate(1)、(Z)-dec-5-en-1-yl sulfate(2)、7-methyloctyl sulfate(3)、(S)-2,6-dimethylheptyl sulfate(4)、N-lactoyl-phenylalanine(5)、(1S,3S)-1-methyl-1,2,3,4-tetrahydro-β-carboline-3-carboxylic acid(6)、(1R,3S)-1-methyl-1,2,3,4-tetrahydro-β-carboline-3-carboxylic acid(7)、L-phenylalanine(8)、tyramine(9)、tryptamine(10)、L-trypto-phan(11)、8-oxo-tryptamine(12)、3-(2-aminoethyl)-3-hydroxyindolin-2-one(13)、β-carboline(14).其中,化合物 1 为新化合物,化合物5～14首次分离自仿刺参内脏.
Abstract
To study the chemical constituents of the viscera of Apostichopus japonicus,column chromatography,such as silica gel,ODS columns,semipreparative HPLC,and Sephadex LH-20 column chromatography,has been used to isolate the seconda-ry metabolites.Their structures were characterized on the basis of multiple spectrometric and spectroscopic techniques,inclu-ding 1H NMR,13C NMR,HSQC,HMBC,1H-1H COSY,NOESY,and HR-ESI-MS.As a result,fourteen compounds were isola-ted from the 95％ethanol extract of the viscera of A.japonicus.These compounds were identified as(E)-dec-5-en-1-yl sulfate(1),(Z)-dec-5-en-l-yl sulfate(2),7-methyloctyl sulfate(3),(S)-2,6-dimethylheptyl sulfate(4),N-lactoyl-phenylala-nine(5),(1S,3S)-1-methyl-1,2,3,4-tetrahydro-β-carboline-3-carboxylic acid(6),(1R,3S)-1-methyl-1,2,3,4-tetra-hydro-β-carboline-3-carboxylic acid(7),L-phenylalanine(8),tyramine(9),tryptamine(10),L-tryptophan(11),8-oxo-tryptamine(12),3-(2-aminoethyl)-3-hydroxyindolin-2-one(13),β-carboline(14).Compound 1 was a novel compound.Compounds 5-14 were obtained from A.japonicus for the first time.
基金项目
中国科学院科技服务网络计划(STS计划)(KFJ-STS-ZDTP-077)
国家自然科学基金面上项目(32270533)
维普
万方数据