苦荞麦麸油的提取及β-环糊精包合工艺研究
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摘要
苦荞又名鞑靼荞麦[F.tataricum(Linn)Gaench],是一种药食兼用植物,有很高的营养价值和药用价值。苦荞中脂类物质含量约9～11%,其中不饱和脂肪酸含量约80%,其中含油酸47.1%,亚油酸36.1%,不皂化物6.56%,β-生育酚1.41%。动物试验研究表明:苦荞油具有显著降低血清甘油三酯与胆固醇及防止低密度脂蛋白氧化、延缓或减轻动脉粥样硬化等功效。但是由于苦荞麦麸油的不饱和程度高,易受空气、水、日光等外界因素的影响,发生氧化变质,不仅会产生不良风味,破坏油的营养物质,也会使油脂的流动性变差,大大限制了其在食品中的应用。因此,研究苦荞麦麸油的提取工艺对促进苦荞资源综合利用和开发新的降脂保健食品都有积极意义。为此,本文以苦荞麦麸皮为原料,分别对苦荞麦麸油的溶剂提取工艺及超临界CO_2萃取工艺进行了优化,且对比分析苦荞麦麸油的脂肪酸组成;研究苦荞麦麸油β-环糊精包合工艺,并考察了包合物的红外图谱及抗氧化稳定性。本论文的研究结果对苦荞资源的综合利用和新型荞麦保健品的开发具有相当的参考价值。
论文的主要研究结果:
(1)苦荞麦麸油溶剂法提取工艺研究
本试验所采用的苦荞麦麸皮苦荞麦麸油平均含量为9.23±0.29%;采用单因素试验和响应曲面法中的Box-Behnken模式对苦荞麦麸粉油溶剂法提取工艺进行了研究。结果表明,料液比、提取时间是苦荞麦麸油提取工艺的极显著影响因子;经检验,建立的提取工艺回归模型准确有效,优化得出的最佳工艺条件为料液比1:11,提取时间141min,提取温度52℃,得率为6.821%,萃取率为73.89%。
(2)苦荞麦麸油超临界CO_2萃取工艺研究
通过二次回归正交旋转组合设计建立了苦荞麦麸油萃取的萃取压力、萃取温度、萃取时间3因素的回归方程,此模型在试验范围内能准确地预测苦荞麦麸油的得率。在试验范围内,对苦荞麦麸油得率影响最大的因素是萃取压力,其次是萃取时间,萃取温度影响最小。通过对萃取条件的优化得出最佳萃取工艺参数为萃取压力22MPa,萃取温度36℃,萃取时间105min,在此条件下苦荞麦麸油得率为8.07%,萃取率为87.43%。
(3)不同提取工艺所得苦荞麦麸油脂肪酸组成研究
采用气相色谱法对溶剂法和超临界CO_2提取苦荞麦麸油进行脂肪酸组成进行研究,试验结果表明:从溶剂法提取苦荞麦麸油中,鉴定出9种脂肪酸,总不饱和脂肪酸含量为80.05%,其中油酸39.91%,亚油酸35.80%;超临界CO_2萃取苦荞麦麸油,共分离出10脂肪酸,总不饱和脂肪酸含量达71.11%,其中油酸39.40%,亚油酸28.04%。超临界CO_2萃取所得苦荞麦麸油呈浅黄绿色,透明状液体,流动性较好,杂质少,具有荞麦油独特的香味。
(4)采用饱和溶液法、超声波法及胶体磨法对研究β-环糊精苦荞麦麸油的包合效果,最终确定胶体磨法的包合效果最好。采用响应曲面法中的Box-Behnken模式,对苦荞麦麸油的β-环糊精胶体磨包合工艺进行了优化,建立了该工艺的二次多项式模型,由该模型得到最佳工艺条件为:包合时间21min;β-环糊精与苦荞麦麸油质量比为5.7:1;水与β-环糊精体积质量比为4.2:1。经过验证,该工艺条件下包合物的含油率为8.07%,油利用率为76.55%。包合物的红外物相鉴别、显微结构观察及抗氧化稳定性试验结果表明:该工艺可以对苦荞麦麸油进行有效包合,不仅能显著提高苦荞麦麸油的稳定性,而且工艺简单,便于操作,具有相当的实用价值。
Tartary buckwheat,Fagopyrum tataricum(Linn)Gaench,is one of culture varieties of the genus Fagopyrum.Tartary buckwheat is not a cereal but is usually grouped with cereals due to its ways of cultivation and utilization, it has been used both as a food and a traditional medicine. According to the published reports, tartary buckwheat has been shown to exhibit significant lowering effects for serum lipids,hepatic lipids,and effect of antioxidantion for its abundance in fat. The content of oil in tartary buckwheat is about9～11%, and unsaturated fatty acids ratio was beyond 80%.(oleic acid47.1%,linoleic acid 36.1%) and the content of unsaponifiable matters in tartary buckwheat seed oil was 6.56%.
Tarary buckwheat oil exhibits significant lowering effects for serum lipids and hepatic total cholesterol.To prevent low density lipoprotein cholesterol was oxidanted and to lessen artherosclerosis.So tartary buckwheat is an excellent material for functional food developing.Tartary buckwheat bran is the mainly byproduct in tartary buckwheat processing,and it has high content of fat.Generally,tartary buckwheat bran is used as feedstuff and waste.
In order to make full use of tartary buckwheat,the ehtraction technology of oil in tartary buckwheat bran was investigated in this paper.Organic solvent extraction technology and supercritical CO_2 extraction technology were optimized and compared,and the compositions of fatty acid in oil were analyzed by GC.Theβ-cyclodextrin inclusion technology of tartary buckwheat bran oil was studied and optimized with Box-Behnken concept of response surface methodology (RSM). And the inclusion compound was identified by infrared spectroscopy and scanning electron microscopy. In addition,the antioxidation stability of the inclusion compound was evaluated.
The main results of this paper:
(1) The solvent-extraction technology of tartary buckwheat bran oil was studied, and all experiment were designed and optimized with Box-Behnken concept of response surface methodlogy.The restlts showed that the significant order of the factors in this experiment is as follows: ratio of material to solvent >treat time>temperament; The model for this extraction technology was established, and also verified with the check experiments. the optimum conditions of the extraction technology were obtained as follows: the ration of material to solvent was 1:11,treat time 141min, temperature 51℃.
(2) The extraction of tartary buckwheat bran oil by supercritical CO_2 was studied,and all experiments were designed and optimized with dual quadratic rotary combination design.The optimum conditions of the extraction technology were obtained as follows: treatment pressure 22MPa,temperature 36℃,time 105min.Using the technological conditions,the extraction yield of oil was 8.07%, and the extraction rate was 87.49%.
(3) The chemical constituents and relative contents in the tartary buckwheat bran oil was measured by GC,In the solvent-extracted tartary buckwheat bran oil, 9 compounds were identified and unsaturated fatty acids ratio was 80.044%.And in the supercritical CO_2 extracted tartary buckwheat bran oil,10 chemical constituents were separared and unsaturated fatty acids ratio was 71.12%.
(4) In order to avoid the oxidation of tartary buckwheat bran oil,theβ-cyclodextrin inclusion technology of tartary buckwheat bran oil was studied and optimized with Box-Behnken concept of response surface methodology (RSM). The inclusion compound was identified by infrared spectroscopy and scanning electron microscopy. The antioxidation stability of the inclusion compound was evaluated. The optimum conditions of the inclusion technology were obtained as follows: inclusion time 21 min, the ratio ofβ-cyclodextrin to tartary buckwheat bran oil 5.7:1(m/m), the ratio of water toβ-cyclodextrin 4.2:1(V/m). Using the optimum conditions, the content of oil in inclusion compound was 8.07%, and the utilization rate of oil was 76.55%. The results showed that tartary buckwheat bran oil could be included effectively and the stability of the inclusion compounds could be improved significantly compared with the tartary buckwheat bran oil. The technology is feasible and fit for industrialized production, with the advantages of simplicity, low energy consumption and high antioxidantion activity.
论文的主要研究结果:
(1)苦荞麦麸油溶剂法提取工艺研究
本试验所采用的苦荞麦麸皮苦荞麦麸油平均含量为9.23±0.29%;采用单因素试验和响应曲面法中的Box-Behnken模式对苦荞麦麸粉油溶剂法提取工艺进行了研究。结果表明,料液比、提取时间是苦荞麦麸油提取工艺的极显著影响因子;经检验,建立的提取工艺回归模型准确有效,优化得出的最佳工艺条件为料液比1:11,提取时间141min,提取温度52℃,得率为6.821%,萃取率为73.89%。
(2)苦荞麦麸油超临界CO_2萃取工艺研究
通过二次回归正交旋转组合设计建立了苦荞麦麸油萃取的萃取压力、萃取温度、萃取时间3因素的回归方程,此模型在试验范围内能准确地预测苦荞麦麸油的得率。在试验范围内,对苦荞麦麸油得率影响最大的因素是萃取压力,其次是萃取时间,萃取温度影响最小。通过对萃取条件的优化得出最佳萃取工艺参数为萃取压力22MPa,萃取温度36℃,萃取时间105min,在此条件下苦荞麦麸油得率为8.07%,萃取率为87.43%。
(3)不同提取工艺所得苦荞麦麸油脂肪酸组成研究
采用气相色谱法对溶剂法和超临界CO_2提取苦荞麦麸油进行脂肪酸组成进行研究,试验结果表明:从溶剂法提取苦荞麦麸油中,鉴定出9种脂肪酸,总不饱和脂肪酸含量为80.05%,其中油酸39.91%,亚油酸35.80%;超临界CO_2萃取苦荞麦麸油,共分离出10脂肪酸,总不饱和脂肪酸含量达71.11%,其中油酸39.40%,亚油酸28.04%。超临界CO_2萃取所得苦荞麦麸油呈浅黄绿色,透明状液体,流动性较好,杂质少,具有荞麦油独特的香味。
(4)采用饱和溶液法、超声波法及胶体磨法对研究β-环糊精苦荞麦麸油的包合效果,最终确定胶体磨法的包合效果最好。采用响应曲面法中的Box-Behnken模式,对苦荞麦麸油的β-环糊精胶体磨包合工艺进行了优化,建立了该工艺的二次多项式模型,由该模型得到最佳工艺条件为:包合时间21min;β-环糊精与苦荞麦麸油质量比为5.7:1;水与β-环糊精体积质量比为4.2:1。经过验证,该工艺条件下包合物的含油率为8.07%,油利用率为76.55%。包合物的红外物相鉴别、显微结构观察及抗氧化稳定性试验结果表明:该工艺可以对苦荞麦麸油进行有效包合,不仅能显著提高苦荞麦麸油的稳定性,而且工艺简单,便于操作,具有相当的实用价值。
Tartary buckwheat,Fagopyrum tataricum(Linn)Gaench,is one of culture varieties of the genus Fagopyrum.Tartary buckwheat is not a cereal but is usually grouped with cereals due to its ways of cultivation and utilization, it has been used both as a food and a traditional medicine. According to the published reports, tartary buckwheat has been shown to exhibit significant lowering effects for serum lipids,hepatic lipids,and effect of antioxidantion for its abundance in fat. The content of oil in tartary buckwheat is about9～11%, and unsaturated fatty acids ratio was beyond 80%.(oleic acid47.1%,linoleic acid 36.1%) and the content of unsaponifiable matters in tartary buckwheat seed oil was 6.56%.
Tarary buckwheat oil exhibits significant lowering effects for serum lipids and hepatic total cholesterol.To prevent low density lipoprotein cholesterol was oxidanted and to lessen artherosclerosis.So tartary buckwheat is an excellent material for functional food developing.Tartary buckwheat bran is the mainly byproduct in tartary buckwheat processing,and it has high content of fat.Generally,tartary buckwheat bran is used as feedstuff and waste.
In order to make full use of tartary buckwheat,the ehtraction technology of oil in tartary buckwheat bran was investigated in this paper.Organic solvent extraction technology and supercritical CO_2 extraction technology were optimized and compared,and the compositions of fatty acid in oil were analyzed by GC.Theβ-cyclodextrin inclusion technology of tartary buckwheat bran oil was studied and optimized with Box-Behnken concept of response surface methodology (RSM). And the inclusion compound was identified by infrared spectroscopy and scanning electron microscopy. In addition,the antioxidation stability of the inclusion compound was evaluated.
The main results of this paper:
(1) The solvent-extraction technology of tartary buckwheat bran oil was studied, and all experiment were designed and optimized with Box-Behnken concept of response surface methodlogy.The restlts showed that the significant order of the factors in this experiment is as follows: ratio of material to solvent >treat time>temperament; The model for this extraction technology was established, and also verified with the check experiments. the optimum conditions of the extraction technology were obtained as follows: the ration of material to solvent was 1:11,treat time 141min, temperature 51℃.
(2) The extraction of tartary buckwheat bran oil by supercritical CO_2 was studied,and all experiments were designed and optimized with dual quadratic rotary combination design.The optimum conditions of the extraction technology were obtained as follows: treatment pressure 22MPa,temperature 36℃,time 105min.Using the technological conditions,the extraction yield of oil was 8.07%, and the extraction rate was 87.49%.
(3) The chemical constituents and relative contents in the tartary buckwheat bran oil was measured by GC,In the solvent-extracted tartary buckwheat bran oil, 9 compounds were identified and unsaturated fatty acids ratio was 80.044%.And in the supercritical CO_2 extracted tartary buckwheat bran oil,10 chemical constituents were separared and unsaturated fatty acids ratio was 71.12%.
(4) In order to avoid the oxidation of tartary buckwheat bran oil,theβ-cyclodextrin inclusion technology of tartary buckwheat bran oil was studied and optimized with Box-Behnken concept of response surface methodology (RSM). The inclusion compound was identified by infrared spectroscopy and scanning electron microscopy. The antioxidation stability of the inclusion compound was evaluated. The optimum conditions of the inclusion technology were obtained as follows: inclusion time 21 min, the ratio ofβ-cyclodextrin to tartary buckwheat bran oil 5.7:1(m/m), the ratio of water toβ-cyclodextrin 4.2:1(V/m). Using the optimum conditions, the content of oil in inclusion compound was 8.07%, and the utilization rate of oil was 76.55%. The results showed that tartary buckwheat bran oil could be included effectively and the stability of the inclusion compounds could be improved significantly compared with the tartary buckwheat bran oil. The technology is feasible and fit for industrialized production, with the advantages of simplicity, low energy consumption and high antioxidantion activity.
引文
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