糖蜜酒精废液酚类物的分离及其抗氧化活性的研究
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摘要
糖蜜酒精废液是一种高浓度有机废水,它含有较多的色素,这种色素颜色深、难于降解,是造成废液中COD、BOD含量高的主要原因。然而糖蜜酒精废液色素是一种天然色素,是甘蔗生长和制糖加工过程中逐步产生的一种混合色素,主要包括酚类色素、焦糖色素和美拉德色素等。其中的酚类色素是一种多酚类物质,它具有一定的抗氧化活性,有很高的经济价值,可以作为一种天然抗氧化剂,广泛应用于食品、医药、化妆品等行业。因此,研究从酒精废液色素中分离出酚类色素,既可以降低酒精废液对环境的污染,又可以回收有价值的资源,降低治理污染的成本,一举两得。本课题研究的主要内容与相关结论如下:
1.研究乙醇对酒精废液酚类色素粉末的提取粗酚类色素的效果,通过单因素及正交实验表明,最佳条件是乙醇浓度95%、温度50℃,固液比为1∶15,时间为1h,浸提次数为3次。
2.采用膜分离、聚酰胺树脂分离的方法对酚类色素样品进行纯化。通过分级膜纯化试验发现,分子量处于300D～800D的截留物中酚类色素含量最高,属于强抗氧化成分。通过聚酰胺树脂纯化试验,可知最佳纯化条件是:室温,吸附时间70min,聚酰胺目数60～80目,洗脱液90%乙醇,1g树脂最多能吸附90.5mg酚类物。
3.通过四种不同的体系(油脂、·OH、DPPH.、亚油酸),研究了酒精废液酚类色素的抗氧化活性,结果表明试样A、B都有抗氧化活性。在油脂体系中,抗氧化活性大小关系为:V_c＞试样B＞试样A。在·OH体系中,抗氧化活性大小关系为:试样B＞V_c＞试样A,且当试样浓度超过1.6mg/mL时,清除·OH的能力逐渐趋于稳定。在DPPH.体系中,对自由基的清除效果为:V_c＞试样B＞试样A,最佳反应时间是30min,最佳pH5。在亚油酸体系中,抗氧化能力为:V_c＞试样B＞试样A,且V_c的抗氧化能力远大于试样A和试样B。
4.紫外检测显示,分离物都具有类黄酮类结构;红外光谱检测显示分离物都含有-OH、苯环、C=O,具有酚类化合物的典型谱图特征;高效液相分析显示,分离物B1可能含有没食子酸、芦丁、绿原酸,分离物B2含有没食子酸、槲皮素、儿茶素、绿原酸,且分离物B1中黄酮含量较多,分离物B2中黄酮苷含量较多。
Alcohol wastewater is a high-concentration organic wastewater with pigments.The colour of pigments is very deep,very hardly degradned,and it is the important reason that COD and BOD is so high in alcohol wastewater.The pigment from molasses alcohol wastewater is a natural pigment,which is formed and accumulated in the sugar growing and processing.It includes polyphenol pigment,caramel pigment and maillard pigment.It is reported that polyphenol pigment has the antioxidant activity and is used as a nature antioxidant,which is used generally much vocation(Food,Medicine,Cosmetics).So it is important to extract polyphenol pigment from alcohol wastewater.It is advantageous for us to solve pollution problem when attain the antioxidant with high additional value.The main research contents and results of this thesis are reported as following:
1.The extracting result of alcohol was studied on powdery pigment from alcohol wastewater.By the one factor and orthogonal experiment, the best extracting condition is:95%aqueous ethanol,temperature 50℃, ratio of liquid/solid as 1:15,time 1h,degree 3.
2.The samples were separated and purified with membrane and polyamide.By membrabe experiment,it was found that 300D～800D group had strongest antioxidant activity.By polyamide experiment the best purification condition is:temperature 40℃,adsorption time 30min, 60～80 orders polyamide,90%ethnol solution desorption,the large adsorption capacity was 90.5mg per polyamide.
3.The antioxidant activity of samples was studied by four different system(oil,·OH,DPPH·and linoleic acid).The result showed that samples had certain antioxidant activity.In all system the antioxidant activity of the sample A was less power than the sample B.Their antioxidant activity enhanced with adding of concentration.
4.The detection of UV showed that samples contained flavonoids. The detection of IR showed that samples contained hydroxy,phenyl,carbonyl and had typical character spectrum of phenol compound.The detection of HPLC showed that samples contained different matters.Sample B1 contained galic acid,rutin,chlorogenic acid,while sample B2 contained galic acid,quercetin,catechin and chlorogenic acid.Sample B1 contained more flavone,while sample B2 contained more flavonid glycoside.
1.研究乙醇对酒精废液酚类色素粉末的提取粗酚类色素的效果,通过单因素及正交实验表明,最佳条件是乙醇浓度95%、温度50℃,固液比为1∶15,时间为1h,浸提次数为3次。
2.采用膜分离、聚酰胺树脂分离的方法对酚类色素样品进行纯化。通过分级膜纯化试验发现,分子量处于300D～800D的截留物中酚类色素含量最高,属于强抗氧化成分。通过聚酰胺树脂纯化试验,可知最佳纯化条件是:室温,吸附时间70min,聚酰胺目数60～80目,洗脱液90%乙醇,1g树脂最多能吸附90.5mg酚类物。
3.通过四种不同的体系(油脂、·OH、DPPH.、亚油酸),研究了酒精废液酚类色素的抗氧化活性,结果表明试样A、B都有抗氧化活性。在油脂体系中,抗氧化活性大小关系为:V_c＞试样B＞试样A。在·OH体系中,抗氧化活性大小关系为:试样B＞V_c＞试样A,且当试样浓度超过1.6mg/mL时,清除·OH的能力逐渐趋于稳定。在DPPH.体系中,对自由基的清除效果为:V_c＞试样B＞试样A,最佳反应时间是30min,最佳pH5。在亚油酸体系中,抗氧化能力为:V_c＞试样B＞试样A,且V_c的抗氧化能力远大于试样A和试样B。
4.紫外检测显示,分离物都具有类黄酮类结构;红外光谱检测显示分离物都含有-OH、苯环、C=O,具有酚类化合物的典型谱图特征;高效液相分析显示,分离物B1可能含有没食子酸、芦丁、绿原酸,分离物B2含有没食子酸、槲皮素、儿茶素、绿原酸,且分离物B1中黄酮含量较多,分离物B2中黄酮苷含量较多。
Alcohol wastewater is a high-concentration organic wastewater with pigments.The colour of pigments is very deep,very hardly degradned,and it is the important reason that COD and BOD is so high in alcohol wastewater.The pigment from molasses alcohol wastewater is a natural pigment,which is formed and accumulated in the sugar growing and processing.It includes polyphenol pigment,caramel pigment and maillard pigment.It is reported that polyphenol pigment has the antioxidant activity and is used as a nature antioxidant,which is used generally much vocation(Food,Medicine,Cosmetics).So it is important to extract polyphenol pigment from alcohol wastewater.It is advantageous for us to solve pollution problem when attain the antioxidant with high additional value.The main research contents and results of this thesis are reported as following:
1.The extracting result of alcohol was studied on powdery pigment from alcohol wastewater.By the one factor and orthogonal experiment, the best extracting condition is:95%aqueous ethanol,temperature 50℃, ratio of liquid/solid as 1:15,time 1h,degree 3.
2.The samples were separated and purified with membrane and polyamide.By membrabe experiment,it was found that 300D～800D group had strongest antioxidant activity.By polyamide experiment the best purification condition is:temperature 40℃,adsorption time 30min, 60～80 orders polyamide,90%ethnol solution desorption,the large adsorption capacity was 90.5mg per polyamide.
3.The antioxidant activity of samples was studied by four different system(oil,·OH,DPPH·and linoleic acid).The result showed that samples had certain antioxidant activity.In all system the antioxidant activity of the sample A was less power than the sample B.Their antioxidant activity enhanced with adding of concentration.
4.The detection of UV showed that samples contained flavonoids. The detection of IR showed that samples contained hydroxy,phenyl,carbonyl and had typical character spectrum of phenol compound.The detection of HPLC showed that samples contained different matters.Sample B1 contained galic acid,rutin,chlorogenic acid,while sample B2 contained galic acid,quercetin,catechin and chlorogenic acid.Sample B1 contained more flavone,while sample B2 contained more flavonid glycoside.
引文
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[3]霍汉镇.甘蔗糖业[M],1991(4):40-48
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[5]韦丰红等.DPPH 法测甘蔗提取物抗氧化活性研究[J].甘蔗糖业,2003(1):31-33
[6]张吉等.甘蔗糖蜜酒精废液中总黄酮物质含量的测定研究[J].广西轻工业.2005(2):18-20
[7]王标诗,酒精废液中色素物抗氧化活性的研究[硕士论文],广西大学,2005
[8]Joaquim Maur Icio Duarte-almeida.Antioxidant Activity of Phenoliolics Compounds From Sugar Cane(Saccharum oddicinarum L.)Juice,Plant Foods for Human Nutrition(2006)61:187-192
[9]Sandra M.Bettin,William Deodato Isique Douglas W.Fraco.Phenols and metals in sugar-canespirts,Quantitative analysis and effect on radical formation and radical scavenging,Eur Food Res Technol(2002)215:169-175
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[12]石碧,狄莹.植物多酚[M].北京:科学出版社,2000,30-31
[13]葛蕾.苹果渣多酚浸提物及其抗氧化性研究[硕士论文].西北农林科技大学,2005
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