玫瑰茄红色素论文：玫瑰茄红色素的提取纯化及性质研究.doc

玫瑰茄红色素论文：玫瑰茄红色素的提取纯化及性质研究【中文摘要】玫瑰茄红色素作为一种天然食用色素,具有颜色自然、艳丽、无毒副作用等特点,具有抑制氧化、抵抗肿瘤等功效,是着色剂和抗氧化剂的完美结合,属新型食品添加剂。玫瑰茄不仅具有清热解毒、降血压、降血脂等药用价值,还具有美容养颜的神奇功效。玫瑰茄花萼中含有大量的花青素,是制备玫瑰茄红色素的重要原料。本文主要介绍了玫瑰茄红色素的提取和纯化工艺,对其化学结构、稳定性及抗氧化性进行了初步研究。其主要研究内容和结果如下：玫瑰茄干花萼经过粉碎过筛后,采用醇水溶液提取,除去一部分多糖、蛋白质等杂质,得到玫瑰茄红色素粗品。采用pH示差法测定提取物中的总花色苷含量,通过单因素实验和响应面设计优化了提取工艺条件,结果显示影响玫瑰茄红色素提取效果的因素中,影响最大的是料液比,其次是提取时间,最后是提取温度；最佳提取工艺参数为：料液比1：24.8g/mL、提取时间1.52h、提取温度48.74,相应提取液中总花色苷含量487.6mg/100g。通过综合比较XDA-7、AB-8、D101、DA-201、X-5五种树脂对玫瑰茄红色素的吸附率和解吸率,选定吸附分离法纯化玫瑰茄红色素的大孔树脂吸附。结果表明,XDA-7树脂对玫瑰茄红色素的吸附选择性最佳、纯化效果最好,选用XDA-7树脂纯化玫瑰茄红色素。通过单因素和正交试验得出XDA-7树脂纯化纯化玫瑰茄红色素的最佳条件为：最佳吸附条件为上样浓度为2mg/mL,上样流速为1.75mL/min, pH值为2.76,吸附率为90.1%。最佳解吸条件为洗脱剂浓度为75%,洗脱剂pH值为3,洗脱流速1.5mL/min,洗脱剂用量为60mL,解吸率为94.6%。经纯化后的玫瑰茄红色素的色价为52.6,是未纯化的玫瑰茄红色素的7倍左右。采用紫外、红外、液质联用测定方法对纯化后的玫瑰茄红色素进行测定分析。玫瑰茄红色素的紫外-可见扫描光谱测定分析表明,玫瑰茄红色素属于花色苷类色素；玫瑰茄红色素的红外测定分析表明,玫瑰茄红色素为矢车菊-葡萄糖苷类或者飞燕草-葡萄糖苷类色素；液质联用测定分析结果表明,玫瑰茄红色素主要含有两种组分；综合分析质谱图和红外图谱测定结果可知,组分(21.55min)分子量为449.3,包含一个葡萄糖苷,是矢车菊-葡萄糖苷类色素；组分(38.23min)的分子量为580.8,是一种通过C4-C6、C4-C8键结合形成的低聚合花青素类。对玫瑰茄红色素的稳定性进行研究,结果表明：(1)在pH5的条件下,玫瑰茄红色素的色价变化很大,极不稳定。(2)玫瑰茄红色素在60以下保持稳定,当温度高于80时极不稳定,耐热性一般。(3)室内光照射下,玫瑰茄红色素的色价变化较小,具有一定的耐光性,但在太阳光照射下,玫瑰茄红色素的色价变化较大,加工储藏室应避免强光直射。(4)大多数金属阳离子对玫瑰茄红色素有影响,Mg2+, Zn2+, Ca2+对玫瑰茄色素的影响较小,Cu2+, Al3+等离子具有增色作用,而Fe3+会引起吸收峰红移现象。因此,玫瑰茄红色素应尽量避免与铜铁铝器皿接触。对玫瑰茄红色素的抗氧化性进行研究,结果表明：(1)玫瑰茄红色素随着浓度的增大,对DPPH、超氧阴离子和羟自由基的清除能力逐渐增大,虽然略低于Vc,但是在高浓度时分别可以达到Vc的86.1%、78.5%、88.1%。因此,玫瑰茄既可以作为改进食品和药品的色泽、提高食欲的食品和药品着色剂,又可以作为抗氧化剂添加于食品和药品中,有效地清除体内的有害自由基、延缓衰老。(2)随玫瑰茄红色素浓度的增加,清除能力也逐渐增强,当浓度较低时,玫瑰茄红色素清除亚硝酸盐的能力是Vc的11%,当浓度达到1.25%时,玫瑰茄红色素清除能力是Vc的73.9%。【英文摘要】The roselle red pigment is a natural edible pigment, which has natural colors, non-toxic and harmless, it also has the effect of antioxidant and anti-tumor. It is a perfect combination of the coloring agent and antioxidants. And it becomes a new food additive which has great potential development.Roselle is a native plant of Africa and other tropical regions, gradually introduced into China in recent years, and grown in Fujian, Jiangxi and other areas. Roselle has detoxification, lowering blood pressure and blood fat, beauty and other effects. Roselle calyx is rich in anthocyanins, which is a ideal raw material to produce the Roselle red pigment.In this paper, the extraction and purification technics, the structure, stability and oxidation resistance of the roselle red pigment were studied systematically. The main process parameters and conclusions were as follows:After being smashed and screened, the roselle calyx extracted by alcohol solution to remove part of the polysaccharide, protein and other impurities, and got the crude roselle red pigment. The experiment determined the total anthocyanin content by pH-differential method under 520nm, and optimized the extraction process parameters by the single factor and response surface methodology. The conclusion was following:Among the effect factors, solid to liquid ratio was the main factor, the extraction time and temperature was the secondary factors. The optimum extraction conditions process parameters were the following:solid to liquid ratio is 1:24.8g/mL, extraction time is 1.52h, extraction temperature is 48.74, and the corresponding total anthocyanin content is 487.6mg/100g.After comparing the adsorption and desorption rate of XDA-7, AB-8, D101, DA-201, X-5, it showed that XDA-7 was the optimum resin to purify the roselle red pigment. Through the single factor and orthogonal test, the optimum adsorption conditions were that the concentration of the sample was 2mg/mL, the flow rate was 1.75mL/min, pH was 2.76, the adsorption rate was 90.1%. The optimum desorption conditions were that concentration of eluent was 75%, pH of eluent was 3, elution rate 1.5mL/min, the volume of elution was 60mL, and the desorption rate was 94.6%. After the purification, the color value of roselle red pigment was 52.6, which was 7 times as much as which was not purified.The roselle red pigment was identified by UV, IR, and LC-MS. Roselle red pigment was anthocyanin pigment though analyzing the scanning spectrum of UV. It could preliminary be determined the pigment was cornflower-glucoside or delphinium-glucoside though analyzing the spectrum of IR. There were two main components in the pigment through analyzing the result of LC-MS. The molecular weight of Component I (21.55min) was 449.3, which contained a glucoside, it should be cornflower-glucoside pigments. The molecular weight of Component II (38.23min) was 580.8, it should be polymer anthocyanin pigments which bonded through C4-C6, C4-C8.The studies on the stability of the roselle red pigment were showed that:(1) The roselle red pigment remained a relatively stable state under the conditions of pH5, the color value changed greatly and the pigment became unstable. (2) The red pigment had a general heat resistance, which remained a relatively stable state when T80. (3) It also had some light resistance, the pigment would lightly effect under the conditions of dark and room light but not under the sunlight condition, so it should avoid sunlight during processing and storage process. (4) Most of the cations had effect to this red pigment. Mg2+, Zn2+, Ca2+ had little effect to the red pigment, however, Cu2+, Al3+ had a hyperchromic effect, Fe3+ had red shift of absorption peak. So it should avoid contacting with vessels made by Copper, Iron and Aluminum.The studies on the inoxidizability of the roselle red pigment were showed that:(1) As the concentration of the red pigment increasing, the ability of eliminating DPPH, superoxide anion and hydroxyl radical experiment became stronger, and could be achieved to 86.1%,78.5% and 88.1% of Vc when in high concentration although slightly lower than Vc. Therefore, roselle not only could be as a food colorants which could increase humans appetite, but also could be as an antioxidant added into the food to effectively remove the harmful free radicals of body, in one word, it can prevent aging. (2) As the concentration of red pigment increasing, the ability of eliminating became stronger. when the concentration is low, the ability to remove nitrite of the red pigment was 11% of Vc, but when the concentration became 1.25%, the ability could be achieved to 73.9% of Vc.【关键词】玫瑰茄红色素 提取 纯化 结构 稳定性 抗氧化性【英文关键词】Roselle red pigment extraction purification structure stability oxidative stability【目录】玫瑰茄红色素的提取纯化及性质研究摘要3-5ABSTRACT5-7第1章 绪论11-241.1 国内外食用色素的研究现状11-161.1.1 天然食用色素的特点及应用11-121.1.2 合成色素的研究情况12-131.1.3 天然食用色素的发展趋势13-141.1.4 花青素与花色苷简介14-161.2 天然色素的提取及纯化方法16-191.2.1 目前天然食用色素主要的提取方法16-171.2.2 天然食用色素的纯化17-191.3 玫瑰茄的研究现状19-221.3.1 玫瑰茄概述19-201.3.2 玫瑰茄的营养成分、保健和药用价值20-211.3.3 国内外玫瑰茄的生产及利用情况21-221.3.4 玫瑰茄红色素介绍及应用现状221.4 研究内容及意义22-241.4.1 主要研究内容22-231.4.2 研究意义23-24第2章 玫瑰茄红色素的提取工艺研究24-352.1 引言242.2 材料与设备24-252.2.1 材料与试剂242.2.2 仪器与设备24-252.3 实验方法25-272.3.1 玫瑰茄红色素的提取工艺步骤252.3.2 玫瑰茄红色素提取效果评价25-262.3.3 确定吸收波长262.3.4