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黑莓色素超声波提取、纯化及特性研究

Reasearch on the Ultrasonic Extraction, Purification Process and the Property of Blackberry Pigment

【作者】 闫宁环

【导师】 徐怀德;

【作者基本信息】 西北农林科技大学 , 食品科学, 2007, 硕士

【摘要】 黑莓属于蔷薇科悬钩子属植物,是具有发展前景的第三代水果。黑莓果实具有亮丽的紫红色,可以作为良好的天然食用色素来源。本研究对黑莓色素超声波提取、大孔吸附树脂分离纯化工艺、色素的理化及光谱特性、黑莓色素清除自由基等体外抗氧化性及外界因素对色素的影响进行了研究,为该色素的工业化生产和色素使用提供理论依据。本论文的主要研究结果如下:(1)利用响应面曲面法对影响超声波提取工艺的关键因子及其相互作用进行分析,表明超声波提取温度是影响提取效果的最显著因子,其次是料液比、超声波功率和提取时间。优化得出的工艺参数为:超声波提取温度为71℃,料液比为1:9,提取时间为31min,超声波作用的功率为527W。模型回归方程为:Y=13.34667+1.11125*X1-0.520167*X2+0.071667*X3+0.093417*X4-2.8715*X12+0.4165*X1*X2+0.673*X1*X3-0.21025*X1*X4-1.618125*X22+0.019*X2*X3+0.3625*X2*X4-1.304125*X32-0.231*X3*X4-1.319*X42。结合静态试验和动态试验,从15种大孔吸附树脂中优选出最适合分离纯化黑莓色素的HPD-100A型号的树脂,优化的工艺参数为:上柱液的pH值为2.0~3.0,样液浓度为0.671mg/mL,吸附流速为1.0mL/min,以60%的乙醇为解吸剂,洗脱流速为0.7mL/min。(2)不同pH值的黑莓色素的紫外光谱特性研究表明:pH1.0~5.0的黑莓色素溶液的紫外光谱的峰形相近,而pH6.0~14.0的黑莓色素溶液在紫外和可见光范围内的特征吸收峰消失。(3)黑莓色素对·O(2-0、·OH、DPPH自由基的清除效果依次为:DPPH>·O2->·OH,且清除效果与黑莓色素浓度之间存在量效关系。与茶多酚相比,黑莓色素具有较强的清除自由基及还原能力。黑莓色素与其它物质的抗氧化协同实验结果表明:二者复配对DPPH自由基的抑制效果:黑莓色素+Vc>黑莓色素+茶多酚>黑莓色素>茶多酚>Vc。三者复配对DPPH自由基的清除效果比较:黑莓色素+茶多酚+酒石酸>黑莓色素+茶多酚+柠檬酸>黑莓色素+Vc+柠檬酸>黑莓色素+Vc+酒石酸,且对DPPH自由基的抑制率与黑莓色素浓度存在量效关系。(4)黑莓色素稳定性进行研究结果表明:第一,黑莓色素吸光度的保存率及还原能力随加热和光照时间延长而衰减,温度越高、光照强度越强,色素吸光度的保存率及还原能力衰减越快。第二,pH值是影响色素性质的关键因子。第三,H2O2、Na2SO3、Vc、Fe2+和Fe3+的添加对色素吸光度的保存率及还原能力有显著影响;而葡萄糖、蔗糖、木糖、山梨酸钾、苯甲酸钠及K+、Ca2+、Al3+、Na+、Mg2+、Mn2+、Pn2+、Cu2+、Zn2+等金属离子的添加对色素吸光度的保存率及其还原能力无显著影响;柠檬酸、苹果酸及酒石酸的添加有一定的增色作用。

【Abstract】 With the trend of returning to nature and paying attention to food safety, more and more people prefer to natural edible pigment. Blackberry is such a perfect resources. In this paper, the technology of extraction with ultrasonic and purification with resins were studied. The physical and chemical specialty and the character of spectrum were also analyzed, and the ability of scavenging the free radicals and the effects of external factors on the stability of color and antioxidation were also researched, the purpose of this study is to afford the theoretically gists for industrial production and the betterment of this pigment.The results showed as follows:(1) First, the experiment were carried out for researching the technologies of ultrasonic extraction and purification with resins. Response surface methodology experiment was designed to analysis technology of extraction. The result indicated that the effect of temperature was significant. And the optimum parameters of extraction technology were: the temperature is 71℃, the solvent volume is 1:9, the time is 31min, the power of ultrasonic was 527w.And the equition of the regression of is:Y=13.34667+1.11125*X1-0.520167*X2+0.071667*X3+0.093417*X4-2.8715*X12+0.4165*X1*X2+0.673*X1*X3-0.21025*X1*X4-1.618125*X22+0.019*X2*X3+0.3625*X2*X4-1.304125*X32-0.231*X3*X4-1.319*X42。For purification method, the contrast tests of 15 resins were performed, and the results showed that the type of HPD-100A was the best resin. The optimum purification technological parameters were: the pH value was about 2.0~3.0,the concentration was 0.67mg/mL,the rate of absorption was 1.0mL/min,the appropriate stripping solvent was 60% ethanol, and the rate of wiping out the pigment was 0.7mL/min.(2) The spectrum of Blackberry with different pH value were: the UV spectrum of pH1.0~5.0 were similar, when the pH value was about 6.0~14.0, the diagnostic peak had disappeared.(3) The order of scavenging effect of free radicals was: DPPH·>·O2->·OH, and displaying the dose-effect relationship. And the antioxidant ability of Blackberry pigment was better than tea Hydroxybenzene.The results of scavenging DPPH radicals of Blackberry pigment with other antioxidant were:Blackberry pigment + Vc>Blackberry pigment + Tea hydroxybenzene>Blackberry pigment>Tea hydroxybenzene>Vc.The results of scavenging DPPH radicals of blackberry pigment with other two antioxidants were:Blackberry pigment + Tea hydroxybenzene+ Tartaric acid>Blackberry pigment + Tea hydroxybenzene + Citric acid>Blackberry pigment +Vc + Citric acid>Blackberry pigment +Vc.+ Tartaric.(4) Finally, the research has been made on the stability of Blackberry pigment. Conclusion was drawn that light and heat could lead to the attenuation of its stability of color and antioxidant, the higher the temperature, the strong the illumination, the more they were decreased. Secondly, pH value was the critical factor to the Blackberry pigment. Thirdly, the addition of H2O2、Na2SO3、Vc、Fe2+and Fe3+had badly destroyed the stability of Blackberry pigment. While the glucose、saccharose、xylose、preservative sodium benzoate and metal ions of K+、Ca(2+0、Al3+、Na+、Mg2+、Mn2+、Pn2+、Cu2+、Zn2+had no significant effects on the stability of color and antioxidant of blackberry pigment. And the addition of acid such as the citric acid、malic acid and tartaric acid could add the color and the ability of antioxidant of the Blackberry pigment.

【关键词】 黑莓色素超声波提取分离特性
【Key words】 Blackberrypigmentultrasonic extractionisolationcharacter
  • 【分类号】S663.2
  • 【被引频次】30
  • 【下载频次】1005
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