从豆粕中提取大豆异黄酮的研究
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摘要
本文采用溶剂提取技术与超临界萃取技术,研究了从脱脂豆粕中提取大豆异黄酮的过程,并建立了相应的物理传质模型。建立了高效液相色谱法分析提取物中大豆异黄酮的方法。
本文先采用乙醇及其水溶液为溶剂,进行了溶剂提取大豆异黄酮的实验研究。在单因素实验的基础上,设计了的正交实验来确定溶剂提取大豆异黄酮的最佳工艺条件。经过对正交实验结果的极差分析表明,溶剂提取的最佳提取条件为:温度70℃、溶剂为70%乙醇水溶液、料液比为1:20,时间为4小时,此时总异黄酮提取量为2668.4μg/g。
基于Fick扩散第二定律,本文建立了溶剂提取大豆异黄酮的传质动力学模型。由于异黄酮在较高的温度下发生降解反应,在考虑了降解反应对异黄酮提取过程的影响的情况下,对模型进行了修正,提高了模型精度。
然后,采用超临界二氧化碳萃取技术,对异黄酮的提取进行了研究。本文首先采用了乙醇作为夹带剂,全面考察了乙醇浓度、夹带剂含量、原料粒径、温度、压力、二氧化碳流量和时间对异黄酮提取过程的影响。通过正交实验,确定了最佳提取工艺条件。
本文又采用了甲醇作为夹带剂进行研究。最佳提取条件为:温度为40℃,压力60MPa,二氧化碳流量10L/h,时间270分钟,此时总异黄酮提取量为2458.8μg/g。
基于异黄酮在豆粕颗粒的毛细孔中的吸附-脱附平衡假设,建立了吸附-脱附传质模型。在模型中只有一个吸附平衡常数需要根据实验数据来回归。模型计算结果与实验值吻合较好。
Supercritical fluid extraction and solvent extraction of soybean isoflavones from soybean meal were studied in the present thesis. The mathematical model of supercritical fluid extraction and solvent extraction were also established. The method of quantifying isoflavones in extracts using HPLC was established with Waters 1525 system.
Aqueous ethanol was employed in solvent extraction method. Based on single-factor experiments, orthogonal experiments were performed to optimize the extractive conditions. Based on range analysis of the experimental data, the optimized conditions of extraction were: 70% ethanol, solvent/sample ratio of 1:20, temperature of 70℃and 4 hours extraction. The largest amount of total isoflavones obtained was 2668.4μg/g.
According to Fick’s second law, the dynamic model of solvent extraction of isoflavones was established. Considering the degradation reaction of isoflavones, the kinetic equation was modified. The model accuracy was improved.
With aqueous ethanol as modifier, supercritical fluid extraction experiments were undertaken to investigate systematically the influence of the modifier composition, the modifier concentration, the particle size and the conditions of extraction (temperature, pressure, CO_2 flow rate and time). The orthogonal experiments were undertaken to optimize the conditions of extraction.
Aqueous methanol was also adopted to improve the extraction efficiency of total isoflavones. Optimized conditions of 40℃, 60 MPa, CO_2 flow rate of 10 L/h and 270 minutes was gotten and the yield was 2458.8μg/g.
Based on the hypothesis of adsorption-desorption equilibrium of solute in matrix pores, an adsorption-desorption mathematical model was established involving only one parameter, adsorption equilibrium coefficient, to be regressed from the experimental data. The deduced model fitted the experimental data very well.
本文先采用乙醇及其水溶液为溶剂,进行了溶剂提取大豆异黄酮的实验研究。在单因素实验的基础上,设计了的正交实验来确定溶剂提取大豆异黄酮的最佳工艺条件。经过对正交实验结果的极差分析表明,溶剂提取的最佳提取条件为:温度70℃、溶剂为70%乙醇水溶液、料液比为1:20,时间为4小时,此时总异黄酮提取量为2668.4μg/g。
基于Fick扩散第二定律,本文建立了溶剂提取大豆异黄酮的传质动力学模型。由于异黄酮在较高的温度下发生降解反应,在考虑了降解反应对异黄酮提取过程的影响的情况下,对模型进行了修正,提高了模型精度。
然后,采用超临界二氧化碳萃取技术,对异黄酮的提取进行了研究。本文首先采用了乙醇作为夹带剂,全面考察了乙醇浓度、夹带剂含量、原料粒径、温度、压力、二氧化碳流量和时间对异黄酮提取过程的影响。通过正交实验,确定了最佳提取工艺条件。
本文又采用了甲醇作为夹带剂进行研究。最佳提取条件为:温度为40℃,压力60MPa,二氧化碳流量10L/h,时间270分钟,此时总异黄酮提取量为2458.8μg/g。
基于异黄酮在豆粕颗粒的毛细孔中的吸附-脱附平衡假设,建立了吸附-脱附传质模型。在模型中只有一个吸附平衡常数需要根据实验数据来回归。模型计算结果与实验值吻合较好。
Supercritical fluid extraction and solvent extraction of soybean isoflavones from soybean meal were studied in the present thesis. The mathematical model of supercritical fluid extraction and solvent extraction were also established. The method of quantifying isoflavones in extracts using HPLC was established with Waters 1525 system.
Aqueous ethanol was employed in solvent extraction method. Based on single-factor experiments, orthogonal experiments were performed to optimize the extractive conditions. Based on range analysis of the experimental data, the optimized conditions of extraction were: 70% ethanol, solvent/sample ratio of 1:20, temperature of 70℃and 4 hours extraction. The largest amount of total isoflavones obtained was 2668.4μg/g.
According to Fick’s second law, the dynamic model of solvent extraction of isoflavones was established. Considering the degradation reaction of isoflavones, the kinetic equation was modified. The model accuracy was improved.
With aqueous ethanol as modifier, supercritical fluid extraction experiments were undertaken to investigate systematically the influence of the modifier composition, the modifier concentration, the particle size and the conditions of extraction (temperature, pressure, CO_2 flow rate and time). The orthogonal experiments were undertaken to optimize the conditions of extraction.
Aqueous methanol was also adopted to improve the extraction efficiency of total isoflavones. Optimized conditions of 40℃, 60 MPa, CO_2 flow rate of 10 L/h and 270 minutes was gotten and the yield was 2458.8μg/g.
Based on the hypothesis of adsorption-desorption equilibrium of solute in matrix pores, an adsorption-desorption mathematical model was established involving only one parameter, adsorption equilibrium coefficient, to be regressed from the experimental data. The deduced model fitted the experimental data very well.
引文
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