菠萝皮中色素、果胶的提取纯化及性质研究
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摘要
天然色素和果胶是具有广泛应用前景的农副产品提取物,为了促进菠萝皮的综合利用,本论文对菠萝皮色素的提取、精制、产品成分和稳定性进行了系统全面的研究,并建立了菠萝皮联产色素、果胶工艺流程。
研究采用单因素和正交实验确立了有机溶剂浸提菠萝皮干粉和鲜皮色素2条工艺,通过对比,选择干粉色素浸提工艺并采用响应面进一步优化工艺参数,确定最终优化工艺为浸提溶剂75%乙醇,料液比1:60(g/mL),温度70℃,破碎度过10目,浸提级数2级,1级浸提时间2h,2级浸提时间0.5h。采用此工艺得到的菠萝皮水溶性色素和黄酮粗品总黄酮含量分别为2.451mg/g和245.966 mg/g,油溶性色素粗品总类胡萝卜素含量为3.149 mg/g。
研究分别采用AB-8、D101大孔吸附树脂、聚酰胺、氧化镁和硅胶对菠萝皮水溶性色素、黄酮、油溶性色素粗品进行精制。精制后的菠萝皮水溶性色素和黄酮产品总黄酮含量分别为90.558 mg/g和321.222 mg/g,油溶性色素产品总类胡萝卜素含量为7.834 mg/g。成分初步分析的结果表明菠萝皮水溶性色素精制品中可能含有黄酮、二氢黄酮和黄酮醇类物质,并含有低浓度花色素。菠萝皮黄酮精制品可能含有二氢黄酮和查耳酮类物质。菠萝皮油溶性色素精制品中含有类胡萝卜素成分。
菠萝皮黄酮和水溶性色素的稳定性实验结果表明:菠萝皮黄酮对加热、(钠、钙、镁、锌)离子、糖、抗氧剂Vc稳定,对光照、pH、(铝、铜、亚铁)离子、常用防腐剂苯甲酸钠及山梨酸钾和氧化剂不稳定。菠萝皮水溶性色素对光照、加热、金属离子(钠、钙、镁、锌、铝、铜、亚铁离子)、糖、抗氧化剂Vc,防腐剂苯甲酸钠、山梨酸钾稳定,对pH和氧化剂较不稳定。对比可知:菠萝皮黄酮稳定性较好,菠萝皮水溶性色素稳定性很好,后者比前者更稳定。
研究通过单因素和正交优化实验确立菠萝皮干粉果胶提取工艺和浸提色素后的菠萝皮残渣浸提果胶工艺。建立菠萝皮联产色素、果胶工艺路线,采用此工艺,过10目的菠萝皮粉100g(水分含量11.77%)可得到菠萝皮水溶性色素产品1.68g,菠萝皮黄酮产品0.30g,菠萝皮油溶性色素产品0.55g,菠萝皮果胶1.12g。果胶产品半乳糖醛酸含量为69.43%,质量符合国家标准。
The natural pigment and pectin are extractive of agricultural by-products which have wide prospect in application. In order to promote the comprehensive utilization of pineapple[Ananas Comosus(L.) Merr.] peel, the extraction, purification, component analysis and stability of pigme- nt from pineapple peel were systematically studied, and a joint production process was established for the production of pigment and pectin from pineapple peel.
By single factor and orthogonal tests, 2 organic solvent extraction process of both fresh and dry pineapple peel were determined. By contrast, the process of dry pineapple peel was chosen and its process parameters were further optimized by the response surface method, the ultimate optimal process is: 75% ethanol as extraction solvent, liquid and solid ratio:60(mL/g), extraction temperature:70℃, degrees of fragmentation:through 10 meshes, the number of extraction cycles: 2, extraction time of cycle 1: 2 hours, cycle 2: 0.5 hour. The products got by applying this proce- ss are as follow: crude water-soluble pigment of pineapple peel, its total content of flavonoids: 2.451 mg/g; crude flavonoid of pineapple peel, its total content of flavonoids: 245.966 mg/g; crude oil-soluble pigment of pineapple peel, its total content of carotenoids: 3.149 mg/g.
Using AB-8, D101 macroporous resin, polyamide, magnesium oxide and silica gel, the cru- de pineapple peel water-soluble pigment, flavonoid and oil-soluble pigment were refined, respec- tively. After purification, the total content of flavonoids of refined water-soluble pigment and fla- vonoid are 90.558 mg/g and 321.222 mg/g, respectively; total content of carotenoids of refined oil-soluble pigments is 7.834 mg/g. Preliminary component analysis showed that refined pineapple peel water-soluble pigment may contain flavone, flavanone and flavonol, and a low concentratio- ns of anthocyanin. Refined pineapple peel flavonoid may contain flavanone and chalcone. Refin- ed pineapple peel oil-soluble pigment has carotenoid.
Results of stability experiments of pineapple peel flavonoid and water-soluble pigment showed: refined pineapple peel flavonoid is stable with heating, (sodium, calcium, magnesium, zinc)ions, sugar and Vc; astable with lighting, pH, (aluminum, copper, ferrous) ions, commonly used preservative:sodium benzoate and potassium sorbate, and oxidants. Refined pineapple peel water-soluble pigment is stable with lighting, heating, metal ions (sodium, calcium, magnesium, zinc, aluminum, copper, ferrous ion), sugar, Vc, sodium benzoate and potassium sorbate, less stable with pH and oxidant. The stability of refined pineapple peel flavonoid is good, the stability of refined pineapple peel water-soluble pigment which is more stable than the former is very good.
Through single factor and orthogonal experiments, 2 pectin extraction process of pineappl- e peel powder and pineapple peel residue after pigment extraction were determined. A joint production process was established for the production of pigment and pectin from pineapple peel. Using this process, 100g pineapple peel powder(water content 11.77%) which is through 10 mesh could obtain water-soluble pigments: 1.68g, flavonoids: 0.30g, oil-soluble pigments: 0.55g, pectin: 1.12g. The content of galacturonic acid of pineapple peel pectin is 69.43%, and the quality of pectin meet national standard.
研究采用单因素和正交实验确立了有机溶剂浸提菠萝皮干粉和鲜皮色素2条工艺,通过对比,选择干粉色素浸提工艺并采用响应面进一步优化工艺参数,确定最终优化工艺为浸提溶剂75%乙醇,料液比1:60(g/mL),温度70℃,破碎度过10目,浸提级数2级,1级浸提时间2h,2级浸提时间0.5h。采用此工艺得到的菠萝皮水溶性色素和黄酮粗品总黄酮含量分别为2.451mg/g和245.966 mg/g,油溶性色素粗品总类胡萝卜素含量为3.149 mg/g。
研究分别采用AB-8、D101大孔吸附树脂、聚酰胺、氧化镁和硅胶对菠萝皮水溶性色素、黄酮、油溶性色素粗品进行精制。精制后的菠萝皮水溶性色素和黄酮产品总黄酮含量分别为90.558 mg/g和321.222 mg/g,油溶性色素产品总类胡萝卜素含量为7.834 mg/g。成分初步分析的结果表明菠萝皮水溶性色素精制品中可能含有黄酮、二氢黄酮和黄酮醇类物质,并含有低浓度花色素。菠萝皮黄酮精制品可能含有二氢黄酮和查耳酮类物质。菠萝皮油溶性色素精制品中含有类胡萝卜素成分。
菠萝皮黄酮和水溶性色素的稳定性实验结果表明:菠萝皮黄酮对加热、(钠、钙、镁、锌)离子、糖、抗氧剂Vc稳定,对光照、pH、(铝、铜、亚铁)离子、常用防腐剂苯甲酸钠及山梨酸钾和氧化剂不稳定。菠萝皮水溶性色素对光照、加热、金属离子(钠、钙、镁、锌、铝、铜、亚铁离子)、糖、抗氧化剂Vc,防腐剂苯甲酸钠、山梨酸钾稳定,对pH和氧化剂较不稳定。对比可知:菠萝皮黄酮稳定性较好,菠萝皮水溶性色素稳定性很好,后者比前者更稳定。
研究通过单因素和正交优化实验确立菠萝皮干粉果胶提取工艺和浸提色素后的菠萝皮残渣浸提果胶工艺。建立菠萝皮联产色素、果胶工艺路线,采用此工艺,过10目的菠萝皮粉100g(水分含量11.77%)可得到菠萝皮水溶性色素产品1.68g,菠萝皮黄酮产品0.30g,菠萝皮油溶性色素产品0.55g,菠萝皮果胶1.12g。果胶产品半乳糖醛酸含量为69.43%,质量符合国家标准。
The natural pigment and pectin are extractive of agricultural by-products which have wide prospect in application. In order to promote the comprehensive utilization of pineapple[Ananas Comosus(L.) Merr.] peel, the extraction, purification, component analysis and stability of pigme- nt from pineapple peel were systematically studied, and a joint production process was established for the production of pigment and pectin from pineapple peel.
By single factor and orthogonal tests, 2 organic solvent extraction process of both fresh and dry pineapple peel were determined. By contrast, the process of dry pineapple peel was chosen and its process parameters were further optimized by the response surface method, the ultimate optimal process is: 75% ethanol as extraction solvent, liquid and solid ratio:60(mL/g), extraction temperature:70℃, degrees of fragmentation:through 10 meshes, the number of extraction cycles: 2, extraction time of cycle 1: 2 hours, cycle 2: 0.5 hour. The products got by applying this proce- ss are as follow: crude water-soluble pigment of pineapple peel, its total content of flavonoids: 2.451 mg/g; crude flavonoid of pineapple peel, its total content of flavonoids: 245.966 mg/g; crude oil-soluble pigment of pineapple peel, its total content of carotenoids: 3.149 mg/g.
Using AB-8, D101 macroporous resin, polyamide, magnesium oxide and silica gel, the cru- de pineapple peel water-soluble pigment, flavonoid and oil-soluble pigment were refined, respec- tively. After purification, the total content of flavonoids of refined water-soluble pigment and fla- vonoid are 90.558 mg/g and 321.222 mg/g, respectively; total content of carotenoids of refined oil-soluble pigments is 7.834 mg/g. Preliminary component analysis showed that refined pineapple peel water-soluble pigment may contain flavone, flavanone and flavonol, and a low concentratio- ns of anthocyanin. Refined pineapple peel flavonoid may contain flavanone and chalcone. Refin- ed pineapple peel oil-soluble pigment has carotenoid.
Results of stability experiments of pineapple peel flavonoid and water-soluble pigment showed: refined pineapple peel flavonoid is stable with heating, (sodium, calcium, magnesium, zinc)ions, sugar and Vc; astable with lighting, pH, (aluminum, copper, ferrous) ions, commonly used preservative:sodium benzoate and potassium sorbate, and oxidants. Refined pineapple peel water-soluble pigment is stable with lighting, heating, metal ions (sodium, calcium, magnesium, zinc, aluminum, copper, ferrous ion), sugar, Vc, sodium benzoate and potassium sorbate, less stable with pH and oxidant. The stability of refined pineapple peel flavonoid is good, the stability of refined pineapple peel water-soluble pigment which is more stable than the former is very good.
Through single factor and orthogonal experiments, 2 pectin extraction process of pineappl- e peel powder and pineapple peel residue after pigment extraction were determined. A joint production process was established for the production of pigment and pectin from pineapple peel. Using this process, 100g pineapple peel powder(water content 11.77%) which is through 10 mesh could obtain water-soluble pigments: 1.68g, flavonoids: 0.30g, oil-soluble pigments: 0.55g, pectin: 1.12g. The content of galacturonic acid of pineapple peel pectin is 69.43%, and the quality of pectin meet national standard.
引文
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