苦丁茶中熊果酸的提取分离及分析方法的研究

【作者】 汤小胜；

【导师】 周春山；

【作者基本信息】 中南大学 ， 分析化学， 2004， 硕士

【摘要】 本文研究了苦丁茶（Ilex Kudingcha C.J.Tseng）中熊果酸的提取、纯化、及测定方法：（1）通过单因素条件实验和正交实验筛选出熊果酸的最佳提取工艺条件。用95％乙醇，料液比为1：12，每次回流3h，共回流3次，熊果酸的提取率为90.7％。（2）研究了脱色剂脱色、重结晶等对产品中熊果酸含量的影响。确定的最佳工艺条件为：水沉用量为原提取液体积的0.4倍，水沉时间为2h，水沉3次；石油醚用量为原提取液体积的0.2倍，石油醚洗涤两次；脱色剂与脱色溶液的比例为4％（w／v），脱色时pH调到9，脱色时间为30min，脱色两次；重结晶3次。（3）确定了苦丁茶中熊果酸的高效液相色谱法的最佳测定条件是：λ=220nm，C₁₈色谱柱（250mm×4.6mm，10um）；流动相为甲醇—水（90：10），进样量在0.8320～0.0416mg／mL范围内，回归方程Y=-2213.604+417140.349×X，r=0.9994，线性关系良好，平均回收率为102.4％。 同时，本文采用酸碱法对废脱色剂进行再生试验。通过正交试验分别确定了碱处理和酸处理废脱色剂的最佳条件。碱处理和酸处理废脱色剂的最佳条件分别为：碱处理浓度为6％，处理时间为60 min，处理温度为100℃；酸处理浓度为3％，处理时间为40 min，处理温度为25℃（其中酸处理中使用的脱色剂是按碱处理最佳工艺条件进行二次碱处理后的再生脱色剂）。本文还进行新脱色剂、再生脱色剂脱色的比较试验。结果表明：5％（脱色剂与脱色溶液的比例，w／v）的再生脱色剂和4％的新脱色剂脱色效果相当。更多还原

【Abstract】 The extraction purification and analysis method of ursolic acid in Ilex kudingcha C.J. Tseng were investigated:(l) To screen the optimum extracting technique of ursolic acid through the single factor experiments and the orthogonal methods. The extraction rate reached 90.7% when extracted three times using 95% ethanol for three hours each time and the ratio volume of ethanol per g raw material is 1 : 12.(2) Effects of decolorization of decoloring agent,recrystallization et al on the content of ursolic acid in the product were studied.The best result was as follows: the volume of water is 0.4 multiple of the raw extracting solution, water precipitation three times and 2h each time; the volume of petroleum ether is 0.2 multiple of the raw extracting solution and washing twice;the ratio of decoloring agent and decolourized solution is 4 % (w/v),decoloration twice and 30min per time at the PH 9;recrystallization three times.(3) The best analysis condition of ursolic acid by HPLC was as follows:Methanol-water(90:10,v/v), detection wavelength 220nm,the calibration curve was linear in the range of the value of 0.8320 ~ 0.0416mg/mL, Y= - 2213.604+417140.34 X X ,r=0.9994 ,and the average recovery ratio was 102.4%.The regeneration of decoloring agent was experimented through the acid-alkali method and the optimized conditions of alkali and acid treatments were respectively determined by the orthogonal methods. The best result can be achieved at 6% alkali solution twice,the temperature 100 C for 60min and 3 % acid solution , the temperature 25 C for 40min.The comparison of decolorization of regenerated decoloring agent and original decoloring agent showed that the 5% (the ratio of decoloring agent and decolourized solution,w/v) regenerated decoloring agent have the same effect of decolorization as that of the 4 % original decoloring agent.更多还原