菊芋菊糖的提取纯化、抗氧化活性及菊糖复合饮料工艺研究
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摘要
菊糖是一种从药食同源的植物-菊芋中提取的天然果聚糖,它以自身优良的保健和药用价值成为国际上热门的功能性食品。近年来,菊糖在中国的市场规模也逐步扩大。但国内关于菊芋菊糖的抗氧化活性、急性毒性及成品应用方面鲜有报道。
本论文以菊芋块茎为原料,通过对菊芋菊糖的研究现状分析,结合具体实验条件,对菊糖的定性定量分析、提取纯化工艺、抗氧化活性、急毒以及菊糖水解生产高果糖浆进行了较为系统的研究,并初步研制了一种菊糖复合成品,为今后菊芋资源的综合利用奠定良好基础,创造出它应有的社会效益与经济价值。主要研究结果如下：
1.在菊糖含量分析上采用了分光光度法,通过分别测定菊芋提取液中总糖含量与还原糖含量来确定菊糖含量。总糖的测定采用苯酚-硫酸法,还原糖的测定采用3,5-二硝基水杨酸法。此法具有准确性高、重现性好、操作简便、快速等优点。
2.采用热水浸提法对菊糖进行了提取。通过单因素试验、正交试验和方差分析确定了提取菊糖的最佳条件为：固液比1：30,在90℃下加热50min,提取2次,菊糖得率为78.36%。预先经超声波辅助强化处理10min,菊糖得率可达85.48%；预先经微波强化处理4min,菊糖得率可达86.21%。
3.采用氢氧化钙-磷酸除杂法,通过正交试验和方差分析确定了除杂的最佳条件为：加Ca(OH)2调后的pH值为10,加磷酸调后的pH值为6,澄清温度控制在80℃。在此条件下,透光率为86.0%,菊糖得率为72.58%。
4.研究了不同树脂及活性碳对菊芋提取液脱色的影响。结果表明,D301-G树脂的脱色效果较好；最佳脱色条件为：提取液浓度控制在0.20gmL,脱色温度30℃,上柱流速2BV/h,树脂用量为10g/50mL。与732型阳离子树脂联用,最终脱色率为69.8%,菊糖保留率为95.2%,透光率为93%。
5.研究了酸水解菊糖制备高果糖浆的工艺。确定了最佳制备工艺为：磷酸比2%,于80℃下水解40min。在此条件下,高果糖浆中还原糖含量高达67.83%。
6.菊糖样品经凝胶过滤法鉴定为均一组分,纯度较高,单糖组成仅含有果糖及少量葡萄糖,具有菊糖类物质的一般特征。
7.采用两种自由基体系对菊糖、粗菊糖的体外抗氧化性能的研究表明,二者均有不同程度的清除羟自由基和超氧阴离子自由基的能力,且其清除效率随着菊糖浓度的增大而逐渐上升。经急性毒性实验证明,菊糖日常推荐口服剂量是安全的。
8.菊糖复合饮料配方：菊花和山楂提取液比为3：2,蜂蜜4%,白砂糖3%,菊芋菊糖2%,CMC-Na0.1%和海藻酸钠0.05%。
The inulin is the natural levan which withdraws from the medicinal and edible plant Jerusalem artichoke. Because of its good health and medicinal value, inulin has become an internationally popular functional food. In recent years, the Chinese inulin market is also growing. But the anti-oxidation activity, acute toxicity and finished applications about Jerusalem artichoke inulin are rarely reported.
The paper took the Jerusalem artichoke tuber as a raw material, with the research on current situation of inulin, combined with the specific experimental conditions, the qualitative and quantitative analysis, extraction and purification process, anti-oxidation activity, acute toxicity of inulin as well as the production of high fruit syrup by inulin hydrolisis were all systematic studied, and one kind of inulin compound product had been initially developed. That would lay the foundation for the future Jerusalem artichoke resources'utilization and development, and create the desired social benefits and its economic value. The major findings were as follows:
1. Using spectrophotometry to analyse the inulin content. Total carbohydrate was determined by the method of phenol-sulfuric acid, reducing sugar was determined by the method of 3,5-dinitrosalicylic acid. The method was accurate, repeatable, simple and rapid.
2. Used the hot water to extract inulin. The optimal conditions were determined through single-factor test, orthogonal test and analysis of variance:the ratio of sample to water was 1:30, temperature 90℃, time 50 min and the times of extraction was 2. Under this condition, the extract ratio was 78.36%. Strengthening to process 10min by ultrasound in advance, inulin yield could reach to 85.48%. Strengthening to process 4min by microwave in advance, inulin yield could reach to 86.21%.
3. The method of calcium hydroxide-phosphoric acid was used to eliminate mixed. The optimal conditions were determined through orthogonal test and analysis of variance:using Ca (OH)2 to adjust pH to 10, using phosphoric acid to adjust pH to 6 and clarify temperature was 80℃.Under this condition, transmittance was 86.0%, the yield of inulin was 72.58%.
4. Studied the effects of different resins and activated carbon for decolorization of extract. The results showed that the decolorization effect of D301-G resin was good. The optimal conditions were:inulin concentration 0.20g/mL, feeding temperature 30℃feeding rate 2BV/h, resin consumption 10g/50mL. Used with 732 resin together, decolorization rate was 69.8%, inulin retention rate was 95.2%, transmittance was 93%.
5. Studied the preparation of high fructose syrup from inulin with the treatment of acid hydrolysis. The optimum preparation process was:phosphoric acid ratio 2%, temperature 80℃and time 40min. Under this condition, reducing sugar content could reach to 67.83%.
6. Inulin sample was identified as homogeneous component by gel filtration, and the purity was high. The monosaccharide composition only included the fructose and the little glucose, and it had the general characteristic of inulin class material.
7. Two kind of free radical systems were used to study the antioxidation of inulin and crude inulin. The result indicated that they all had different capability to remove hydroxyl free radicals and superoxide negion, which improved with the increase of inulin concentration. The acute toxicity experiment showed that the daily oral dose of inulin recommended was safe.
8.The optimum formula of Inulin compound drink was determined as follows:The ratio of extracts about the chrysanthemum to the Chinese hawthorn was 3:2, Honey 4%, sugar 3%, Inulin2%, CMC-Na 0.1%and alginate 0.05%.
本论文以菊芋块茎为原料,通过对菊芋菊糖的研究现状分析,结合具体实验条件,对菊糖的定性定量分析、提取纯化工艺、抗氧化活性、急毒以及菊糖水解生产高果糖浆进行了较为系统的研究,并初步研制了一种菊糖复合成品,为今后菊芋资源的综合利用奠定良好基础,创造出它应有的社会效益与经济价值。主要研究结果如下：
1.在菊糖含量分析上采用了分光光度法,通过分别测定菊芋提取液中总糖含量与还原糖含量来确定菊糖含量。总糖的测定采用苯酚-硫酸法,还原糖的测定采用3,5-二硝基水杨酸法。此法具有准确性高、重现性好、操作简便、快速等优点。
2.采用热水浸提法对菊糖进行了提取。通过单因素试验、正交试验和方差分析确定了提取菊糖的最佳条件为：固液比1：30,在90℃下加热50min,提取2次,菊糖得率为78.36%。预先经超声波辅助强化处理10min,菊糖得率可达85.48%；预先经微波强化处理4min,菊糖得率可达86.21%。
3.采用氢氧化钙-磷酸除杂法,通过正交试验和方差分析确定了除杂的最佳条件为：加Ca(OH)2调后的pH值为10,加磷酸调后的pH值为6,澄清温度控制在80℃。在此条件下,透光率为86.0%,菊糖得率为72.58%。
4.研究了不同树脂及活性碳对菊芋提取液脱色的影响。结果表明,D301-G树脂的脱色效果较好；最佳脱色条件为：提取液浓度控制在0.20gmL,脱色温度30℃,上柱流速2BV/h,树脂用量为10g/50mL。与732型阳离子树脂联用,最终脱色率为69.8%,菊糖保留率为95.2%,透光率为93%。
5.研究了酸水解菊糖制备高果糖浆的工艺。确定了最佳制备工艺为：磷酸比2%,于80℃下水解40min。在此条件下,高果糖浆中还原糖含量高达67.83%。
6.菊糖样品经凝胶过滤法鉴定为均一组分,纯度较高,单糖组成仅含有果糖及少量葡萄糖,具有菊糖类物质的一般特征。
7.采用两种自由基体系对菊糖、粗菊糖的体外抗氧化性能的研究表明,二者均有不同程度的清除羟自由基和超氧阴离子自由基的能力,且其清除效率随着菊糖浓度的增大而逐渐上升。经急性毒性实验证明,菊糖日常推荐口服剂量是安全的。
8.菊糖复合饮料配方：菊花和山楂提取液比为3：2,蜂蜜4%,白砂糖3%,菊芋菊糖2%,CMC-Na0.1%和海藻酸钠0.05%。
The inulin is the natural levan which withdraws from the medicinal and edible plant Jerusalem artichoke. Because of its good health and medicinal value, inulin has become an internationally popular functional food. In recent years, the Chinese inulin market is also growing. But the anti-oxidation activity, acute toxicity and finished applications about Jerusalem artichoke inulin are rarely reported.
The paper took the Jerusalem artichoke tuber as a raw material, with the research on current situation of inulin, combined with the specific experimental conditions, the qualitative and quantitative analysis, extraction and purification process, anti-oxidation activity, acute toxicity of inulin as well as the production of high fruit syrup by inulin hydrolisis were all systematic studied, and one kind of inulin compound product had been initially developed. That would lay the foundation for the future Jerusalem artichoke resources'utilization and development, and create the desired social benefits and its economic value. The major findings were as follows:
1. Using spectrophotometry to analyse the inulin content. Total carbohydrate was determined by the method of phenol-sulfuric acid, reducing sugar was determined by the method of 3,5-dinitrosalicylic acid. The method was accurate, repeatable, simple and rapid.
2. Used the hot water to extract inulin. The optimal conditions were determined through single-factor test, orthogonal test and analysis of variance:the ratio of sample to water was 1:30, temperature 90℃, time 50 min and the times of extraction was 2. Under this condition, the extract ratio was 78.36%. Strengthening to process 10min by ultrasound in advance, inulin yield could reach to 85.48%. Strengthening to process 4min by microwave in advance, inulin yield could reach to 86.21%.
3. The method of calcium hydroxide-phosphoric acid was used to eliminate mixed. The optimal conditions were determined through orthogonal test and analysis of variance:using Ca (OH)2 to adjust pH to 10, using phosphoric acid to adjust pH to 6 and clarify temperature was 80℃.Under this condition, transmittance was 86.0%, the yield of inulin was 72.58%.
4. Studied the effects of different resins and activated carbon for decolorization of extract. The results showed that the decolorization effect of D301-G resin was good. The optimal conditions were:inulin concentration 0.20g/mL, feeding temperature 30℃feeding rate 2BV/h, resin consumption 10g/50mL. Used with 732 resin together, decolorization rate was 69.8%, inulin retention rate was 95.2%, transmittance was 93%.
5. Studied the preparation of high fructose syrup from inulin with the treatment of acid hydrolysis. The optimum preparation process was:phosphoric acid ratio 2%, temperature 80℃and time 40min. Under this condition, reducing sugar content could reach to 67.83%.
6. Inulin sample was identified as homogeneous component by gel filtration, and the purity was high. The monosaccharide composition only included the fructose and the little glucose, and it had the general characteristic of inulin class material.
7. Two kind of free radical systems were used to study the antioxidation of inulin and crude inulin. The result indicated that they all had different capability to remove hydroxyl free radicals and superoxide negion, which improved with the increase of inulin concentration. The acute toxicity experiment showed that the daily oral dose of inulin recommended was safe.
8.The optimum formula of Inulin compound drink was determined as follows:The ratio of extracts about the chrysanthemum to the Chinese hawthorn was 3:2, Honey 4%, sugar 3%, Inulin2%, CMC-Na 0.1%and alginate 0.05%.
引文
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