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東革阿里的化學(xué)成分分離與活性成分寬纓酮的提取純化工藝研究

發(fā)布時(shí)間:2018-07-26 15:52
【摘要】:東革阿里(Eurycoma longifolia Jack)又稱天然偉哥、馬來參、鄉(xiāng)土人參,在馬來西亞與燕窩、錫器一起并稱為三大國(guó)寶。東革阿里全株均可入藥,但常以根為主要藥用部位,在東南亞作為藥品和補(bǔ)品已經(jīng)有了數(shù)百年的歷史,可作單味藥、亦可作方中配藥,具有抗癌、抗瘧疾、改善男性性功能障礙等功效。東革阿里主要含有苦木素二萜和生物堿兩類化學(xué)成分,苦木素二萜類是其主要活性成分,寬纓酮(Eurycomanone,EN)是其中最具代表性的一種。本論文系統(tǒng)性地研究了東革阿里的主要化學(xué)成分;建立了東革阿里藥材中活性成分EN的HPLC含量測(cè)定方法;考察了藥材中EN的提取及大孔樹脂純化工藝。為東革阿里提取物國(guó)際質(zhì)量標(biāo)準(zhǔn)的制定以及后續(xù)開發(fā)利用提供科學(xué)依據(jù),主要研究結(jié)果如下:1.東革阿里中主要化學(xué)成分的提取、分離與結(jié)構(gòu)鑒定利用中壓制備色譜、硅膠柱層析色譜、SephadexLH-20凝膠色譜和重結(jié)晶等方法從東革阿里中分離得到19個(gè)單體化合物。通過核磁和質(zhì)譜等波譜學(xué)手段鑒定出它們的化學(xué)結(jié)構(gòu):16個(gè)為苦木素(Quassinoid)二萜類,其中EL15.2為新化合物;1個(gè)為東莨菪苷;1個(gè)為腺苷;1個(gè)為松柏苷,松柏苷為首次從東革阿里中分離得到。2.東革阿里藥材、提取物中EN的含量測(cè)定以EN為對(duì)照品,利用高效液相色譜結(jié)合紫外檢測(cè)器,建立了 EN的含量測(cè)定方法。利用新建立的方法測(cè)定了 8批東革阿里藥材和5批提取物中EN的含量。結(jié)果發(fā)現(xiàn)東革阿里藥材中EN的含量差別較大,最低為0.43‰,最高為1.64‰;而東革阿里提取物中EN的含量差別較小,約為1%。3.東革阿里中EN的提取工藝研究以EN轉(zhuǎn)移率為指標(biāo),采用單因素實(shí)驗(yàn)和正交實(shí)驗(yàn),考察乙醇濃度、溶劑用量、提取時(shí)間、提取次數(shù)對(duì)EN提取率的影響。優(yōu)選出合理的提取工藝為:20倍量水回流提取2次,第一次2h,第二次1h。4.東革阿里中EN的大孔樹脂純化工藝研究利用動(dòng)、靜態(tài)吸附以及解吸附實(shí)驗(yàn)優(yōu)選出適合的大孔樹脂型號(hào)。以EN含量以及轉(zhuǎn)移率為指標(biāo);采用單因素實(shí)驗(yàn)和正交實(shí)驗(yàn)優(yōu)選出合理的純化工藝為:選用HPD100樹脂;70%飽和吸附量上樣;上樣液質(zhì)量濃度為0.25g生藥/mL;上樣流速為3BV/h;洗脫溶劑為25%乙醇;洗脫流速為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,

本文編號(hào):2146514

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