【摘要】：本論文分為三個(gè)部分第一部分:文獻(xiàn)綜述對(duì)寬筋藤化學(xué)成分、藥理活性及臨床應(yīng)用進(jìn)行了綜述,并對(duì)其今后的研究方向進(jìn)行了展望,引用文獻(xiàn)34篇;對(duì)反式丁香苷植物分布、藥理活性及含量分析方法進(jìn)行了綜述,并對(duì)其今后的研究方向進(jìn)行了展望,引用文獻(xiàn)168篇。第二部分:寬筋藤化學(xué)成分研究采用多種分離純化方法和結(jié)構(gòu)鑒定手段(如ESI-MS、1H-NMR、13C-NMR等波譜學(xué)技術(shù)),對(duì)寬筋藤化學(xué)成分進(jìn)行了研究。共分離得到23個(gè)化合物,鑒定出22個(gè)化合物,包括6個(gè)苯丙素類,3個(gè)萜類,3個(gè)腦苷脂類,2個(gè)生物堿類,2個(gè)肽和氨基酸類和6個(gè)其他類成分。6個(gè)苯丙素類成分分別是反式丁香苷(trans-syringin),tinosinen,丁香脂素-4-O-β-D-葡萄糖苷(syringaresinol-4-O-β-D-glucopyranoside),tinosposide,開(kāi)環(huán)異落葉松脂素-9-O-β-D-葡萄糖苷(secoisolariciresinol-9-O-β-D-glucopyranoside)和異落葉松脂素-9-O-β-D-葡萄糖苷(isolariciresinol-9-O-β-D-glucopyranoside),3 個(gè)萜類分別是倍半萜tinocordiside,二萜tinosineside A 和三萜cycloeucalenone,3 個(gè)腦苷脂分別是 2-(2'-羥基二十四碳酰氨基)十八碳-1,3,4-三醇(2-(2'-hydroxytetracosanoylamino)octadecane-1,3,4-triol),soya-cerebroside Ⅰ 和 soya-cerebroside Ⅱ,2 個(gè)生物堿分別是反式-N-咖啡酰酪胺(trans-N-caffeoyltyramine)和偽巴馬丁(pseudopalmatine),1 個(gè)肽類環(huán)(酪氨酸-酪氨酸)(cyclo(tyrosyl-tyrosyl))和1個(gè)氨基酸L-焦谷氨酸(L-pyroglutamic acid),以及 6 個(gè)其他類成分 5-羥甲基-2-呋喃丙烯酸(5-hydroxymethyl-2-furanacrylic acid),鄰苯二甲酸-二(2-乙基-己基)酯(bis(2-ethylhexyl)phthalate),1,2-di-O-palmitoyl-3-Oβ-D-galactopyranosyl glycerol,3,4-二甲氧基苯基-β-D-葡萄糖苷(3,4-dimethoxyphenyl-β-D-glucoside),β-谷甾醇(β-sitosterol)和胡蘿卜苷(daucosterol)。經(jīng)SciFinder 檢索,5-羥甲基-2-呋喃丙烯酸(5-hydroxymethyl-2-furanacrylic acid)是首次從自然界分離得到的一個(gè)新天然化合物。化合物開(kāi)環(huán)異落葉松脂素-9-O-β-D-葡萄糖苷(secoisolariciresinol-9-O-β-D-glucopyranoside),cycloeucalenone,2-(2'-羥基二十四碳酰氨基)十八碳-1,3,4-三醇(2-(2'-hydroxytetracosanoylamino)octadecane-1,3,4-triol),soya-cerebroside Ⅰ,soya-cerebroside Ⅱ,反式-N-咖啡酰酪胺(trans-N-caffeoyltyramine),偽巴馬丁(pseudopalmatine),環(huán)(酪氨酸-酪氨酸)(cyclo(tyrosyl-tyrosyl)),L-焦谷氨酸(L-pyroglutamic acid),鄰苯二甲酸-二(2-乙基-己基)酯(bis(2-ethylhexyl)phthalate),1,2-di-O-palmitoyl-3-O-β-D-galactopyranosyl glycerol和3,4-二甲氧基苯基-β-D-葡萄糖苷(3,4-dimethoxyphenyl-β-D-glucoside)12個(gè)化合物是首次從寬筋藤中分離得到的。本研究結(jié)果豐富了寬筋藤中化學(xué)成分內(nèi)涵,為寬筋藤的藥效物質(zhì)基礎(chǔ)研究和質(zhì)量控制研究奠定基礎(chǔ)。第三部分:寬筋藤化學(xué)成分定量分析建立寬筋藤中反式丁香苷和Tinosinen的含量測(cè)定方法。采用HPLC法測(cè)定反式丁香苷和Tinosinen的含量,對(duì)提取工藝進(jìn)行單因素考察,優(yōu)選出最佳提取方法,并采用該方法測(cè)定不同地區(qū)市售寬筋藤藥材中反式丁香苷和Tinosinen的含量,結(jié)果確定寬筋藤藥材提取方法為,80倍量的30%甲醇回流提取90 min。不同地區(qū)市售寬筋藤藥材反式丁香苷和Tinosinen的含量分別在0.0076%～0.0248%、0.0562%～0.1427%之間,表明不同來(lái)源的藥材中兩個(gè)成分的含量存在一定差異,其規(guī)律性需要進(jìn)行大樣本分析。采用石油醚提取寬筋藤中的脂肪酸,經(jīng)甲酯化處理,采用GC-MS方法分離和鑒定脂肪酸,峰面積歸一化法定量分析。共分離鑒定出飽和脂肪酸成分13種,總含量達(dá)到檢出物的44.38%,其中棕櫚酸含量最高為16.17%,其次是十七烷酸含量為7.85%。不飽和脂肪酸有4種,總含量達(dá)到檢出物的28.43%,其中亞油酸含量為19.48%,11-十八烯酸含量為7.19%。特色與創(chuàng)新1.從寬筋藤中分離得到一個(gè)新天然化合物,5-羥甲基-2-呋喃丙烯酸(5-hydroxymethyl-2-fUranacrylic acid)。2.首次建立了寬筋藤中兩個(gè)苯丙素類成分反式丁香苷和Tinosinen的含量測(cè)定方法。
[Abstract]:This paper is divided into three parts: the first part of the literature review on the chemical constituents, pharmacological activities and clinical applications of Caulis Spatholobi, and its future research directions were prospected, 34 references were cited; the distribution of trans-syringin plants, pharmacological activities and content analysis methods were reviewed, and its future research directions were also discussed. Part 2: Chemical constituents of Caulis Spatholobi were isolated and purified by ESI-MS, 1H-NMR, 13C-NMR and other spectroscopic techniques. 23 compounds were isolated and 22 compounds were identified, including 6 phenylpropanoids, 3 terpenoids and 3 terpenoids. 6 phenylpropanoids are trans-syringin, tinosinen, syringaresinol-4-O-beta-D-glucopyranoside, tinosposide, ring-opening isolaricin-9-O-beta-D-glucoside, respectively. Resinol-9-O-beta-D-glucopyranoside and isolariciresinol-9-O-beta-D-glucopyranoside are sesquiterpene tinocordiside, diterpenoid tinosineside A and triterpenoid cycloeucalenone, and three cerebrosides are 2-(2'-hydroxy-tetracarbonyl amino) octadecanol-1,3,4-triol (2'-hyd-hyd-hyd-glucopyranoside). Roxytetracosanoylamino) octadecane-1,3,4-triol, soya-cerebroside I and soya-cerebroside II, two alkaloids are trans-N-caffeoyltyramine and pseudopalmatine, one peptide ring (tyrosine-tyrosine) (cyclo (osyl-tyrosyl)) and one amino acid L-pyroglutamic acid (L-pyroglutlutlutamic acid), respectively. Amic acid, 5-hydroxymethyl-2-furanacrylic acid, bis (2-ethylhexyl) phthalate, 1,2-di-O-palmitoyl-3-O-beta-galactopyranosyl glycerol, 3,4-dimethoxyphenyl-beta-D-glucoside Ide, beta-sitosterol and daucosterol. According to SciFinder, 5-hydroxymethyl-2-furanacrylic acid (5-hydroxymethyl-2-furanacrylic acid) is a new natural compound isolated from nature for the first time. Pyranoside, cycloeucalenone, 2-(2'-hydroxytetracosanoylamino) octadecane-1,3,4-triol, soya-cerebroside I, soya-cerebroside II, trans-N-caffeyltyramine, pseudopalmatine, cyclo-tyrosine Twelve compounds, namely, syl-tyrosyl, L-pyroglutamic acid, bis (2-ethylhexyl) phthalate, 1,2-di-O-palmitoyl-3-O-beta-D-galactopyranosyl glycerol and 3,4-dimethoxyphenyl-beta-D-glucoside, were isolated for the first time from Caulis spatholobi. The results of this study enriched the connotation of the chemical constituents in Caulis Spatholobi and laid a foundation for the study of the pharmacodynamics and quality control of Caulis Spatholobi. Part III: Quantitative analysis of the chemical constituents of Caulis Spatholobi was carried out to establish a method for the determination of trans-syringin and Tinosinen in Caulis Spatholobi. The contents of trans-syringin and Tinosinen The content of trans-syringin and Tinosinen were determined by this method. The results showed that the extraction method was 80 times of 30% methanol reflux extraction for 90 minutes. The contents of Tinosinen and Petroleum ether were 0.0076%-0.0248% and 0.0562%-0.1427% respectively, which indicated that there were some differences in the contents of the two components from different sources, and the regularity needed large sample analysis. A total of 13 kinds of saturated fatty acids were isolated and identified by normalized quantitative analysis. The content of palmitic acid and heptadecanoic acid reached 44.38%, 16.17% and 7.85% respectively. There were 4 kinds of unsaturated fatty acids, the total content of which reached 28.43%, of which linoleic acid and 11-octadecanoic acid were 19.48% and 7.19% respectively. A new natural compound, 5-hydroxymethyl-2-fUranacrylic acid, was isolated from Caulis Spatholobi. 2. A method for the determination of trans-eugenoside and Tinosinen was established for the first time.
【學(xué)位授予單位】：北京中醫(yī)藥大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：R284.1

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