本文選題：薯蕷皂苷元 + 薯蕷皂苷�。� 參考：《江蘇大學》2017年碩士論文

【摘要】：薯蕷皂苷元在藥物生產(chǎn)中是一種非常重要的前體化合物,是合成避孕藥、可的松、性激素、蛋白同化激素等甾體類藥物的主要原料,因此在醫(yī)藥界有“藥用黃金”和“激素之母”的美譽。此外,藥理研究表明,薯蕷皂苷元具有多種生物活性,包括抗癌、抗炎、提高免疫力、抗血栓、降血脂和抗病毒等。在我國,黃姜和穿山龍因薯蕷皂苷元的含量較高,是生產(chǎn)該化合物的主要原材料。植物中的薯蕷皂苷元主要以皂苷形式存在,因而生產(chǎn)薯蕷皂苷元必須使糖苷鍵水解。傳統(tǒng)方法生產(chǎn)薯蕷皂苷元導致了嚴重的環(huán)境污染,非皂苷部分得不到利用,而且薯蕷皂苷元收率較低。本論文研究旨在建立一種更清潔和高效地從黃姜和穿山龍中生產(chǎn)薯蕷皂苷元的方法,并提高藥用薯蕷資源的利用效率,已完成的研究工作主要包括:(1)建立了HPLC-UV測定薯蕷皂苷元含量的方法建立了HPLC色譜分析條件,即色譜柱為Waters XBridge Shield RP18(4.6mm×150 mm,5μm);流動相為乙腈:水(75:25);流速為1.0 mL/min;檢測波長為203 nm;進樣量為20μL;柱溫為40oC;分析時間為15 mins。在該條件下,薯蕷皂苷元可以與干擾成分實現(xiàn)基線分離(R1.5)。此后,進行了方法學考察,包括線性關(guān)系、精密度、穩(wěn)定性、重復性和加樣回收率。結(jié)果表明,薯蕷皂苷元在0.002~1.024 mg/mL范圍內(nèi)線性關(guān)系良好(r2=0.9999);精密度實驗RSD=1.02%(n=6);重復性實驗RSD=1.78%(n=6);平均加樣回收率分別為96.2%(RSD=1.17%)、100.4%(RSD=2.47%)和101.6%(RSD=1.09%);供試品溶液在24 hrs內(nèi)測定,RSD=1.93%。由此可見,所建立的HPLC分析方法是穩(wěn)定、可靠的,可用于薯蕷皂苷元的定量分析。(2)直接加壓雙相酸水解法從黃姜中萃取薯蕷皂苷元首先利用正交實驗設計對加壓雙相酸水解反應條件進行了優(yōu)化,考察了反應溫度、硫酸濃度、反應時間和料液比四個因素對薯蕷皂苷元收率的影響。利用極差分析和方差分析對4個因素的影響進行評價,并得到最佳提取條件。此后,驗證了最佳提取條件,并將直接加壓雙相酸水解法與兩種傳統(tǒng)方法和預發(fā)酵-雙相聯(lián)合酸水解法進行比較。此外,利用硅膠柱色譜和重結(jié)晶對雙相酸水解后的萃取物中的薯蕷皂苷元進行了分離與純化,并檢測了所得薯蕷皂苷元純度。結(jié)果表明,當反應溫度為140oc、硫酸濃度為0.2mol/l、反應時間為1.5hrs、料液比為2.5g/50ml時,薯蕷皂苷元的收率達到2.21%。采用新方法的薯蕷皂苷元收率比兩種傳統(tǒng)方法和預發(fā)酵-雙相水解法分別高出63.7%、70.4和20.8%,且所需硫酸濃度僅為傳統(tǒng)方法的約1/10。由此可見,利用直接加壓雙相酸水解法從黃姜中萃取薯蕷皂苷元的收率較高,硫酸用量明顯減低,反應時間縮短。(3)總皂苷提取—加壓雙相酸水解法從穿山龍中萃取薯蕷皂苷元首先以70%乙醇溶液對穿山龍中總皂苷進行索氏提取,再利用加壓雙相酸水解法水解皂苷產(chǎn)生薯蕷皂苷元。采用單因素實驗考察了料液比、硫酸濃度、反應溫度和反應時間四個影響因素,并進一步通過正交實驗設計對酸水解條件進行優(yōu)化,得到最佳反應條件,即料液比為8g/50ml、硫酸濃度為4μl/ml、反應溫度為150oc、反應時間為2.5hrs。與傳統(tǒng)方法相比,采用該方法的薯蕷皂苷元收率為1.67%,提高了66.02%,并且硫酸消耗量為1.497ml/g,降低了97.00%。由此可見,采用總皂苷提取-加壓雙相酸水解法,能更高效、更清潔地從穿山龍中萃取薯蕷皂苷元;也表明加壓雙相酸水解是從薯蕷屬植物中生產(chǎn)薯蕷皂苷元的一種有效的途徑。(4)綜合利用—加壓雙相酸水解法從新鮮黃姜從萃取薯蕷皂苷元首先采用物理法回收新鮮黃姜中的淀粉和纖維素,再將粗皂苷進行加壓雙相酸水解萃取薯蕷皂苷元。利用單因素實驗依次考察了料液比、硫酸濃度、萃取溶劑體積、反應溫度、反應時間、轉(zhuǎn)速以及石油醚沸程等因素對薯蕷皂苷元收率的影響,并優(yōu)化得到最佳反應條件。此后,以薯蕷皂苷元收率、硫酸消耗量以及產(chǎn)生廢水中的化學需氧量(cod)和總有機碳量(toc)為評價指標,將新方法和直接加壓雙相酸水解法以及傳統(tǒng)方法進行了比較。結(jié)果表明,當料液比為1g/100ml(粗皂苷粉末質(zhì)量/硫酸溶液體積)、硫酸濃度為2μl/ml、萃取試劑為30ml石油醚(90~120oc)、反應溫度為130oc、反應時間為2hrs、攪拌速度為100r/min時,薯蕷皂苷元的收率可達到4.17%。與傳統(tǒng)方法相比,薯蕷皂苷元收率提高了22.29%,硫酸消耗量降低了88.53%,而且廢水中的COD和TOC分別降低了50.15%和64.39%。由此可見,綜合利用—加壓雙相酸水解從新鮮黃姜中萃取薯蕷皂苷元的新方法是一種更為清潔和高效的途徑,具有較好的發(fā)展?jié)摿?在工業(yè)應用中應用前景良好。
[Abstract]:Diosgenin is a very important precursor compound in drug production. It is the main raw material for the synthesis of contraceptives, cortisone, sex hormone, protein assimilation hormone and so on. Therefore, it has the reputation of "medicinal gold" and "the mother of hormone" in the medical field. In addition, the pharmacological study shows that diosgenin has a variety of bioactivity. In our country, the diosgenin in the plant is mainly in the form of saponins, and the production of diosgenin must make the glycosides hydrolyze. The production of diosgenin must be hydrolyzed. The production of diosgenin in Huang Jianghe was produced by traditional methods. Diosgenin leads to serious environmental pollution, the non saponins can not be used, and the yield of diosgenin is low. The purpose of this study is to establish a more clean and efficient method to produce diosgenin from Zingiber rhizome and Dioscorea, and to improve the utilization efficiency of medicinal Dioscorea. The main research work has been completed. (1) the method of determining the content of diosgenin by HPLC-UV was established to establish the HPLC chromatographic analysis conditions, that is, the chromatographic column is Waters XBridge Shield RP18 (4.6mm x 150 mm, 5 u m); the mobile phase is acetonitrile: water (75:25); the flow rate is 1 mL/min; the detection wavelength is 203 nm; the sample volume is 20 mu; the column temperature is 15; the analysis time is 15 under this condition, Dioscorea The saponins could be separated from the interfering components (R1.5). After that, a methodological study was conducted, including linear, precision, stability, repeatability and recovery. The results showed that diosgenin had a good linear relationship in the range of 0.002~1.024 mg/mL (r2= 0.9999); the precision experiment RSD=1.02% (n=6); RSD=1.78% (n=6) for the repeatability experiment. The average recovery rate was 96.2% (RSD=1.17%), 100.4% (RSD=2.47%) and 101.6% (RSD=1.09%), and the test product solution was determined in 24 hrs. RSD=1.93%. can be seen from this, the established HPLC analysis method is stable and reliable, and can be used in quantitative analysis of diosgenin. (2) diosgenin extracted from rhizome of Dioscorea zingiberensis by direct pressure double phase acid hydrolysis First, the orthogonal experimental design was used to optimize the conditions of the pressure biphasic acid hydrolysis reaction. The effects of four factors, reaction temperature, sulfuric acid concentration, reaction time and liquid ratio, on the yield of diosgenin were investigated. The effects of 4 factors were evaluated by the difference analysis and variance analysis, and the optimum extraction conditions were obtained. After that, the results were verified. The optimum extraction conditions were compared with two traditional methods and pre fermentation biphasic acid hydrolysis. In addition, the Diosgenin was separated and purified by silica gel column chromatography and recrystallization, and the purity of diosgenin was detected. The results showed that the purity of diosgenin was obtained. The results showed that the purity of diosgenin was obtained. When the reaction temperature is 140oC, the concentration of sulfuric acid is 0.2mol/l, the reaction time is 1.5hrs, the yield of diosgenin is up to 2.5g/50ml, the yield of diosgenin is reached to 2.21%. by the new method, the yield of diosgenin is 63.7%, 70.4 and 20.8% higher than that of the two traditional methods and the prefermentation biphasic hydrolysis method, respectively, and the sulphuric acid concentration required is only about 1/10 of the traditional method. It can be seen that the yield of diosgenin extracted from Dioscorea Zingiberis by direct pressure biphasic acid hydrolysis is higher, the amount of sulfuric acid is reduced obviously and the reaction time is shortened. (3) the extraction of diosgenin from Dioscorea Zingiberis by the extraction of total saponins with pressure biphasic acid hydrolysis method first extract the total saponins from the Dioscorea from diosgenin by 70% ethanol solution and then the extraction of the total saponins in the Dioscorea The Diosgenin was hydrolyzed with pressure biphasic acid hydrolysis method to produce diosgenin. Four factors were investigated by single factor experiment, including the ratio of material to liquid, concentration of sulfuric acid, reaction temperature and reaction time, and the optimum reaction conditions were optimized by orthogonal design. The ratio of material to liquid was 8g/50ml, and the concentration of sulphuric acid was 4 mu. The reaction temperature was 150oC and the reaction time was 2.5hrs. compared with the traditional method, the yield of diosgenin was 1.67%, increased by 66.02%, and the consumption of sulphuric acid was 1.497ml/g, and 97.00%. was reduced. The Total Saponins Extracted and pressurized biphasic acid hydrolysis could be used to extract diosgenin more efficiently and cleanly from the Dioscorea It also indicates that pressure biphasic acid hydrolysis is an effective way to produce diosgenin from Dioscorea plants. (4) comprehensive utilization of pressure biphasic acid hydrolysis method from fresh ginger extract diosgenin from diosgenin by physical method to recover starch and cellulose from fresh yellow ginger by physical method, and then extract crude saponins by pressure biphasic acid hydrolysis extraction Diosgenin (diosgenin). The effects of the ratio of material to liquid, the concentration of sulfuric acid, the volume of the solvent, the reaction temperature, the reaction time, the speed and the boiling process of petroleum ether on the yield of diosgenin were investigated in turn, and the optimum reaction conditions were optimized. After that, the yield of diosgenin, the consumption of sulphuric acid and the production of the wastewater were produced. The evaluation of oxygen demand (COD) and total organic carbon content (TOC) is compared with the new method and direct pressurized biphasic acid hydrolysis and traditional method. The results show that the concentration of sulphuric acid is 2 mu l/ml, the extraction reagent is 30ml petroleum ether (90~120oc) and the reaction temperature is 130oc when the ratio of the feed to liquid is 1g/100ml (the mass of the crude saponins / sulphuric acid solution). When the reaction time is 2hrs and the stirring speed is 100r/min, the yield of diosgenin can be reached to 4.17%.. Compared with the traditional method, the yield of diosgenin is increased by 22.29%, the consumption of sulphuric acid is reduced by 88.53%, and the COD and TOC in the wastewater are reduced by 50.15% and 64.39%. respectively. The synthetic utilization of pressure diphasic acid hydrolysis from fresh yellow ginger The new method of extracting diosgenin is a more clean and efficient way. It has good potential for development and has good application prospects in industrial applications.

【學位授予單位】：江蘇大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：R284.1

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