本文選題：甜菊糖苷 + 純化�。� 參考：《南昌大學》2012年碩士論文

【摘要】：甜菊糖是一類糖苷物質,來源于甜葉菊葉片的提取物,它的純度以及其主要成分甜菊苷和萊鮑迪甙A(RA)在甜菊糖中的比例直接影響著甜菊糖的品質。目前,國內對甜菊糖的深加工還有所欠缺,甜菊糖生產以初級加工為主,產品多作為原材料出口國外,并且生產過程中的能耗問題、環(huán)保問題和綠色安全問題比較突出。本研究以江西贛縣的甜葉菊葉為原料,對甜菊糖的水提工藝進行了優(yōu)化,采用較為環(huán)保的聚合氯化鋁(PAC)對水提液進行絮凝除雜,運用乙醇重結晶甜菊糖來提高產品純度和RA的含量,研究結果可為工業(yè)化生產提供理論支持和數據參考。主要研究內容如下： (1)研究了甜菊糖的測定方法。通過探討甜菊糖的檢測方法,確定了葸酮-硫酸法測定甜菊糖含量的方法為：1mL樣液中加入4mL的3.3%葸酮-硫酸試劑,邊加邊混勻,立即置于冰水浴中,待所有樣品加完后,一起置于100℃的水浴中7min,然后一起取出置于冰水浴中冷卻10min,在620nm處測定吸光度；確定了分析甜菊糖苷混合物的液相色譜條件為：Inertsil NH2柱(4.6×250mm,5μm)流動相乙腈：水(70：30),流速1mL/min,進樣量20gL,室溫操作；并確定了甜菊糖苷的簡單紫外檢測法,可適合脫色好且膠質和蛋白質含量低的甜菊糖苷產品的總糖苷含量測定。 (2)優(yōu)化了甜菊糖苷水提工藝。以甜葉菊糖苷的水提得率為評價標準,通過單因素和正交試驗優(yōu)化了甜菊糖苷的水提參數,得到水提的最優(yōu)條件為：提取溫度為70℃、提取時間為3h、料液比為1：15,在此條件下甜葉菊糖苷的水提得率可達到97%。 (3)確定了甜菊糖苷的絮凝條件。以甜菊糖苷損失率、水提液的脫色率和透光率為評價指標,對三種絮凝劑的絮凝效果進行比較,研究表明：PAC可用于甜葉菊水提液的澄清處理；對其澄清影響因素進行研究,確定最佳絮凝條件為：水浴溫度65℃,絮凝劑添加量18mg/mL,輔助攪拌20min,作用時間1h,25℃離心。 (4)建立了甜菊糖苷的最佳重結晶響應面模型。在單因素的基礎上,通過四因素三水平回歸方程建立重結晶響應面模型。各響應值(Yi)對X1、X2、X3、X4的回歸方程分別為：Y1(結晶率)=-282.71467+4.94347X1+0.92322X2+18.20933X3+11.45667X4-10-3X1X2-4×10-3X1X3-2×10-3X1X4-6.56882×10-16X2X3-1.66667×10-3X2X4+1.07692×10-14X3X4-0.02928X12-4.11111×10-3X22-2.172X32-0.543X42Y2(純度)=-420.08083+9.709X1+1.61417X2-6.93167X3+2.4725X4+1.6667×10-3X1X2+0.155X1X3+0.081X1X4+0.10417X2X3+0.010417X2X4+0.3X3X4-0.068X12-0.010816X22-2.02X32-0.50938X42Y3(RA/Total)=-14.54122+0.27694X1+0.046239X2+0.12993X3+0.23999X4+2.30496×104X1X2+3.06965×10-3X1X3-1.37227×10-3X1X4+3.00937×10-4X2X3+5.43917×10-4X2X4+2.01963×10-3X3X4-1.82752×10-3X12-3.60353×10-4X22-0.048684X32-0.010284X42 研究表明,各因素對結晶率響應值影響的強弱依次為：X1(溶解溫度)X4(乙醇含水量)X3(液固比)X2(重結晶時間)；對重結晶產品純度響應值影響的強弱依次為：X3(液固比)X2(重結晶時間)X1(溶解溫度)X4(乙醇含水量)；對RA/Total含量響應值影響的強弱依次為：X3(液固比)X4(乙醇含水量)X1(溶解溫度)X2(重結晶時間)。
[Abstract]:Stevioside is a kind of glycoside, which is derived from the extract of leaves of Stevia. Its purity and the proportion of stevioside and A (RA) in stevioside directly affect the quality of stevioside. At present, the deep processing of stevioside is still lacking in our country. The production of stevioside is mainly in primary processing, and the products are used as raw materials. The problem of energy consumption, environmental protection and green safety are more prominent in the process of production. In this study, the water extraction process of steviodies was optimized by using chrysanthemum leaves in Ganxian, Jiangxi. The water extraction was flocculated by environmentally friendly polyaluminum chloride (PAC) and alcohol was recrystallized with steviodies. High product purity and RA content can provide theoretical support and data reference for industrial production.
(1) the method for determination of steviodies was studied. By exploring the method of detecting stevioside sugar, the method of determining the content of steviodie by acetone sulfuric acid method was as follows: the 4mL in 1mL sample was added with 3.3% ketone sulphuric acid reagents, and mixed evenly, and immediately placed in the ice water bath. After all the samples were added, it was placed together in a water bath of 100 degrees centigrade, and then taken together, and then taken together. In the ice water bath, the 10min was cooled and the absorbance was measured at 620nm. The liquid chromatography conditions for the analysis of the mixture of stevioside were determined as: Inertsil NH2 column (4.6 x 250mm, 5 uh m) mobile phase acetonitrile: water (70:30), velocity 1mL/min, sample volume 20gL, room temperature operation, and a simple UV detection method for stevioside, which was suitable for decolorization. Determination of total glucoside content of stevioside products with low colloid and protein content.
(2) optimize the water extraction process of stevioside. With the water extraction rate of stevioside as the evaluation standard, the water extraction parameters of stevioside were optimized by single factor and orthogonal test. The optimum conditions of the water extraction were as follows: the extraction temperature was 70, the extraction time was 3h, the ratio of the material to liquid was 1:15, and the water extraction rate of stevioside could reach 9 under this condition. 7%.
(3) the flocculation conditions of stevioside were determined. With the loss rate of stevioside, the decolorization rate and the transmittance of the water as the evaluation index, the flocculation effect of the three flocculants was compared. The study showed that PAC could be used in the clarification treatment of the extract of the sweet leaf chrysanthemum, and the influence of the factors on the clarification was studied and the optimum flocculation condition was to determine the temperature of the water bath. 65 18mg/mL, 20min, 1H and 25 C centrifugation.
(4) the optimum recrystallization response surface model of stevioside was established. On the basis of single factor, the recrystallized response surface model was established by four factors and three level regression equations. The regression equations of each response value (Yi) to X1, X2, X3 and X4 were Y1 (crystallization rate) =-282.71467+ 4.94347X1+0.92322X2+18.20933X3+11.45667X4-10-3X1X2-4 x 10-3X1X3-2 x 1, respectively. 0-3X1X4-6.56882 * 10-16X2X3-1.66667 * 10-3X2X4+1.07692 x 10-14X3X4-0.02928X12-4.11111 x 10-3X22-2.172X32-0.543X42Y2 (purity) =-420.08083+9.709X1+1.61417X2-6.93167X3+2.4725X4+1.6667 * 10-3X1X2+0.155X1X3+0.081X1X4+0.10417X2X3+0.010417X2X4+ 0.3X3X4-0.068X12-0.010816X22-2.02X32-0.50938X42Y3 (RA/Total) =-14.54122 +0.27694X1+0.046239X2+0.12993X3+0.23999X4+2.30496 * 104X1X2+3.06965 * 10-3X1X3-1.37227 x 10-3X1X4+3.00937 * 10-4X2X3+5.43917 * 10-4X2X4+2.01963 x 10-3X3X4-1.82752 x 10-3X12-3.60353 * 10-4X22-0.048684X32-0.010284X42
The results show that the strong and weak factors affecting the response value of crystallization rate are X1 (dissolved temperature) X4 (ethanol water content) X3 (liquid solid ratio) X2 (recrystallization time), and the intensity of the response to the purity of the recrystallized products is X3 (liquid-solid ratio) X2 (recrystallization time) X1 (dissolution temperature) X4 (ethanol water content), and the response to RA/Total content in response value. The intensity is X3 (liquid to solid ratio) X4 (water content of ethanol) X1 (dissolution temperature) X2 (recrystallization time).
【學位授予單位】：南昌大學
【學位級別】：碩士
【學位授予年份】：2012
【分類號】：R151

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