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东革阿里的化学成分分离与活性成分宽缨酮的提取纯化工艺研究

发布时间:2018-07-26 15:52
【摘要】:东革阿里(Eurycoma longifolia Jack)又称天然伟哥、马来参、乡土人参,在马来西亚与燕窝、锡器一起并称为三大国宝。东革阿里全株均可入药,但常以根为主要药用部位,在东南亚作为药品和补品已经有了数百年的历史,可作单味药、亦可作方中配药,具有抗癌、抗疟疾、改善男性性功能障碍等功效。东革阿里主要含有苦木素二萜和生物碱两类化学成分,苦木素二萜类是其主要活性成分,宽缨酮(Eurycomanone,EN)是其中最具代表性的一种。本论文系统性地研究了东革阿里的主要化学成分;建立了东革阿里药材中活性成分EN的HPLC含量测定方法;考察了药材中EN的提取及大孔树脂纯化工艺。为东革阿里提取物国际质量标准的制定以及后续开发利用提供科学依据,主要研究结果如下:1.东革阿里中主要化学成分的提取、分离与结构鉴定利用中压制备色谱、硅胶柱层析色谱、SephadexLH-20凝胶色谱和重结晶等方法从东革阿里中分离得到19个单体化合物。通过核磁和质谱等波谱学手段鉴定出它们的化学结构:16个为苦木素(Quassinoid)二萜类,其中EL15.2为新化合物;1个为东莨菪苷;1个为腺苷;1个为松柏苷,松柏苷为首次从东革阿里中分离得到。2.东革阿里药材、提取物中EN的含量测定以EN为对照品,利用高效液相色谱结合紫外检测器,建立了 EN的含量测定方法。利用新建立的方法测定了 8批东革阿里药材和5批提取物中EN的含量。结果发现东革阿里药材中EN的含量差别较大,最低为0.43‰,最高为1.64‰;而东革阿里提取物中EN的含量差别较小,约为1%。3.东革阿里中EN的提取工艺研究以EN转移率为指标,采用单因素实验和正交实验,考察乙醇浓度、溶剂用量、提取时间、提取次数对EN提取率的影响。优选出合理的提取工艺为:20倍量水回流提取2次,第一次2h,第二次1h。4.东革阿里中EN的大孔树脂纯化工艺研究利用动、静态吸附以及解吸附实验优选出适合的大孔树脂型号。以EN含量以及转移率为指标;采用单因素实验和正交实验优选出合理的纯化工艺为:选用HPD100树脂;70%饱和吸附量上样;上样液质量浓度为0.25g生药/mL;上样流速为3BV/h;洗脱溶剂为25%乙醇;洗脱流速为3BV/h。
[Abstract]:Ali (Eurycoma longifolia Jack), also known as natural Viagra, Malay ginseng and local ginseng, is known as the three national treasures in Malaysia along with bird's nest and tin. The whole strain of Dongguang Ali can be used as medicine, but the root is the main medicinal part. It has been used as medicine and tonic in Southeast Asia for hundreds of years. It can be used as a single medicine or a prescription. It has anticancer and anti-malaria properties. Improve male sexual dysfunction and other effects. There are two kinds of chemical constituents in EKA, such as diciterpenoids and alkaloids, of which Eurycomanoneone (Eurycomanoneone) is the most representative one. In this paper, the main chemical constituents of Ari were systematically studied, the HPLC method for the determination of the active component en was established, and the extraction of en and the purification process of macroporous resin were investigated. It provides a scientific basis for the formulation of the international quality standard and the further development and utilization of the extract. The main research results are as follows: 1. The extraction, separation and structure identification of the main chemical constituents from Dongguang Ali were studied. Nineteen monomers were isolated from Dongge Ali by silica gel column chromatography, Sephadex LH-20 gel chromatography and recrystallization. Their chemical structures were identified by NMR and MS spectra: 16 were (Quassinoid) diterpenoids, of which EL15.2 was a new compound, one was scopolamine, one was adenosine, and one was cyperidin. Cyperidin was first isolated from Ari. 2. The content of en in the extract of Ari was determined with en as reference substance. A method for the determination of en was established by high performance liquid chromatography (HPLC) combined with UV detector. The contents of en in 8 batches and 5 batches of extracts of Artemisia davidii were determined by a new method. The results showed that there was a great difference in the content of en, the lowest was 0.43 鈥,

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