本文選題：逆流色譜 + 黃酮��； 參考：《北京化工大學(xué)》2017年博士論文

【摘要】：入侵植物可以產(chǎn)生有各種醫(yī)藥功能的代謝產(chǎn)物。我們實驗室曾經(jīng)研究建立了簡單而成功的分析方法來鑒定有用的目標黃酮類成分,這是獲得入侵植物的提取物中有效成分的重要一步。建立了制備分離十種總黃酮的方法。選擇D4020樹脂,因為它具有高吸附和解吸能力。根據(jù)以下優(yōu)化的參數(shù)進行動態(tài)吸附/解吸過程:黃頂菊提取物濃度為2.72mg/mL, pH 4.50,處理量16BV,流速2.12mL/min,水(4BV)和乙醇:水溶液(90:10, v/v) 5BV。根據(jù)上述條件,提取物中總黃酮含量從4.30%到30%,提高了 7倍,使用D4020樹脂的回收率為90%。此外,對于分離3-硫酸異鼠李素和黃芪苷,通過使用樹脂D4020研究其動態(tài)吸附和解吸過程。3-硫酸異鼠李素的含量8.7%,回收率74.15%,黃芪苷的含量30.8%,回收率92.2%。此外,采用制備型HSCCC分離提純,得到96.48%的3-硫酸異鼠李素4.5mg和24.4mg純度為98.46%的黃芪苷。在第二個部分中,建立了選定的溶劑體系正相與溶劑洗脫-擠出操作的兩步HSCCC方法。第一步中,通過使用正己烷:乙酸乙酯:甲醇:水(4:6:4:6, v/v)的溶劑體系得到3.7mg沒食子酸(98.87%) , 3.9mg沒食子酸乙酯(99.55%),以及鞣花酸、乙基沒食子酸酯的混合物。在第二步中,通過洗脫和擠出高速逆流色譜操作后,使用二氯甲烷-甲醇-水(4: 3: 2, v/v)進行混合物的進一步純化。分離出3.8mg純度為98.68%乙基沒食子酸酯的和5.7mg純度為99.7%的鞣花酸。通過高效液相色譜,超高壓液相色譜-四極桿-飛行時間串聯(lián)質(zhì)譜法,核磁碳譜和核磁氫譜分析確認分離的酚類化合物的結(jié)構(gòu)。在第三部分研究中,研究了分離的化合物的DPPH抗氧化以及粗提物的抗菌敏感性實驗。研究表明沒食子酸乙酯的抗氧化能力好,芒果花的醇提取物可抑制多種病原菌的生長。在濃度為20mg/mL的大腸桿菌,克雷伯菌和金黃色葡萄球菌的保留帶分別為13.20mm, 19.80mm和23.00mm,而仙人掌顯示出最顯著的保留帶26.OOmm。因此,觀察到每個測試生物體的最小抑制區(qū)(MIC)從1.00至2.50mg/mL變化。MIC值不同的原因可能是提取物中發(fā)現(xiàn)的各類具有生物活性的化感物質(zhì)的反應(yīng)機理不一樣,而合成抗生素的抑制機制具有特異性和單一性。從研究結(jié)果中可以得到結(jié)論,上述生物活性成分的分離方法可以擴展到其他天然產(chǎn)物中活性物質(zhì)的分離。
[Abstract]:Invasive plants can produce metabolic products with various medical functions. Our laboratory has studied and established a simple and successful analytical method to identify useful target flavonoids. This is an important step in obtaining effective components from the extracts of invasive plants. A method for preparing ten kinds of total flavonoids was established. Because it has the ability of high adsorption and desorption, the dynamic adsorption / desorption process based on the following optimized parameters: the concentration of the extract of anathea is 2.72mg/mL, pH 4.50, the amount of treatment 16BV, the flow rate 2.12mL/min, water (4BV) and ethanol: the aqueous solution (90:10, v/v) 5BV. based on the above conditions, the content of total flavonoids in the extract is from 4.30% to 30%, which has increased by 7 times, so that the content of total flavonoids in the extract is increased by 7 times. The recovery rate of D4020 resin was 90%.. For the separation of 3- and astragaloside, the content of.3- sulfate was 8.7%, the recovery rate was 74.15%, the content of astragaloside was 30.8%, the recovery rate was 92.2%., and 96.48% 3- sulphuric acid was obtained by using the prepared HSCCC. ISO rhamnin 4.5mg and 24.4mg were 98.46% of astragaloside. In second parts, the selected solvent system positive phase and the two step HSCCC method of solvent elution and extrusion operation were established. In the first step, 3.7mg gallic acid (98.87%), 3.9mg gallic acid was obtained by using hexane: ethyl acetate: methanol: water (4:6:4:6, v/v) solution system. Ethyl (99.55%), as well as a mixture of ellagic acid, ethyl gallate. In the second step, the mixture was further purified using dichloromethane methanol water (4: 3: 2, v/v) by elution and extrusion high speed counter flow chromatography. The purity of 3.8mg was 98.68% ethyl gallate and 5.7mg was 99.7% tannic acid. High performance liquid chromatography, high pressure liquid chromatography - quadrupole flight time tandem mass spectrometry, nuclear magnetic carbon and nuclear magnetic hydrogen spectrum analysis confirmed the structure of separated phenolic compounds. In the third part, the antioxidation of the separated compounds and the antimicrobial susceptibility test of the crude extracts were studied in the third part of the study. The study showed the resistance of ethyl gallate. The alcohol extract of the mango flower could inhibit the growth of various pathogens. In the Escherichia coli with a concentration of 20mg/mL, the retention zones of Klebsiella and Staphylococcus aureus were 13.20mm, 19.80mm and 23.00mm, respectively, while the cactus showed the most significant reservation zone of 26.OOmm., which observed the minimum inhibitory area of each test organism. MIC) the variation of.MIC values from 1 to 2.50mg/mL may be due to the different mechanisms of the bioactive allelochemicals found in the extracts, while the inhibition mechanism of the synthetic antibiotics is specific and unitary. The separation of active substances from other natural products.
【學(xué)位授予單位】：北京化工大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2017
【分類號】：O652.6;TQ28

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