高速逆流色谱分离研究吴茱萸、肾蕨的药用化学成分

发布时间：2018-07-06 11:09

本文选题：高速逆流色谱 + 吴茱萸　；参考：《上海师范大学》2017年硕士论文

【摘要】：高速逆流色谱法(High-speed counter-current chromatography)是色谱分离法的一个分支,简称HSCCC,起源于多极液-液萃取,在上世纪80年代迅速发展,近年来被广泛地用于分离与制备天然产物。吴茱萸是传统中药,为芸香科吴茱萸属植物,目前已有大量对吴茱萸化学成分的研究报道,而生物碱则是吴茱萸中的主要的活性成分。蕨类植物肾蕨,以其全草或块茎入药,目前对其药用价值的研究尚处于起步的阶段。本论文运用HSCCC研究了上述植物材料的化学成分,对分离产物进行了结构鉴定,并探究了部分分离产物与牛血清蛋白(BSA)的亲和力。实验主要研究结果如下:(1)使用反复重结晶方法从吴茱萸果实(0.5 kg)的乙醇提取物中快速分离得到了5440 mg吴茱萸碱与160 mg吴茱萸次碱,此方法操作简便,效率高,可代替前人使用柱色谱制备分离这两种吲哚类生物碱的技术。(2)应用高速逆流色谱法从0.5 kg吴茱萸果实的乙醇提取物中分离得到了7种喹啉类生物碱,分别为:1-methyl-2((6Z,9Z)-pentadecadienyl)-4(1H)-quinolone(1,8.4 mg),dihydroevocarpine(2,27.0 mg),1-methyl-2-pentadecyl-4(1H)-quinolone(3,18.8 mg),1-methyl-2-undecylquinolin-4(1H)-one(4,13.7 mg),(Z)-1-methyl-2-(tridec-5-en-1-yl)quinolin-4(1H)-one(5,14.0 mg),(Z)-1-methyl-2-(undec-6-en-1-yl)quinolin-4(1H)-one和(Z)-1-methyl-2-(undec-5-en-1-yl)quinolin-4(1H)-one的同分异构混合物(6a和6b,8.3 mg),1-methyl-2-nonylquinolin-4(1H)-one(7,15.1 mg).这些化合物与BSA亲和力的实验表明,吴茱萸喹啉碱碳链上的不饱和双键可以增强吴茱萸喹啉碱与BSA的结合能力,碳链过长或过短都不利于喹啉碱与BSA的结合。(3)采用DPPH和ABTS自由基清除实验证明了肾蕨乙醇提取物具备较好的抗氧化活性,用高速逆流色谱仪从12 kg肾蕨乙醇提取物的乙酸乙酯部位中一次分离得到4个化合物,分别为3,4-二羟基苯甲醛、3,4-二羟基苯甲酸甲酯和对羟基苯丙烯酸,另一化合物结构有待结构鉴定,试验证明肾蕨富含酚酸类化合物。
[Abstract]:This paper deals with the chemical constituents of evodia fruit ( 0.5 kg ) . The results are as follows : ( 1 ) Using high - speed countercurrent chromatography to separate the two indole alkaloids from evodia fruit ( 0 . 5 kg ) , this method is simple and convenient to operate and has high efficiency . The experiments of affinity of these compounds with BSA indicated that the unsaturated double bond on the carbon chain of the Evodia rutaus could enhance the binding ability of the quinoline alkaloid and BSA , and the carbon chain was too long or too short to bind the quinoline base with BSA . ( 3 ) The extract of ethanol from 12 kg of Shenndia ethanol was separated from the ethyl acetate part of 12 kg of the kidney fern ethanol extract by high speed countercurrent chromatography to obtain 4 compounds , respectively , which were 3,4 - dihydroxybenzaldehyde , 3,4 - dihydroxybenzoate and p - hydroxyphenylacrylic acid .
【学位授予单位】：上海师范大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O652.63;R284

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