水酶法在菜籽加工中的应用研究
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摘要
菜籽水酶法提油工艺在国内外很多文献都有相关报道，但是使用酶的品种多、酶添加量大、反应周期长而且提油率较低，这些因素限制了水酶法提油工艺的工业化推广。本论文对水酶法提取菜籽油和菜籽蛋白的方法及相关机理进行了研究，以实现同时提取菜籽油和菜籽蛋白，并对油及蛋白质的品质进行了研究，为其工业应用打下理论基础。
本文对水相酶法制备菜籽油的工艺进行研究，研究内容包括四个部分：菜籽预处理对水酶法制备菜籽油的影响；酶解方法与酶解影响因素的研究；破乳对得油率影响的研究以及酶解对菜籽油和菜籽品质的影响的研究。
菜籽在酶解前的预处理对菜籽油的收率有很大的影响。采用于碾磨和湿磨相结合的方法，先将油籽破碎粒度控制在60-80目后进行热处理后采用组织匀浆机匀浆，达到适宜酶促反应所需的破碎度。通过试验得出，最佳热处理的时间为1.5h～2.0h，加热温度为90℃，合适的捣碎时间为10～15min。
研究了两种酶解方法，酶解提油，酶解提油再酶解再提油，酶解后用无水乙醚萃取油脂，在试验确定的最适酶解和萃取条件下提油率分别为：86.75％，90.82％。水相酶解提油的效果与体系的pH、料液比、温度、粉碎度、以及酶的添加量等因素有关。由单因数试验得出，酶的最适添加量为2％，pH为7.0，酶处理时间为4h，最佳料液比为1：6，酶作用温度为50℃；在此条件下菜籽的提取率为86.97％，在单因素基础上进行正交试验得出影响因数的主次表：酶的添加量＞pH＞时间＞温度。经过优化以后的菜籽油最高提取率为88.56％。
研究了三种破乳工艺，即不同离心条件、溶剂、离心与溶剂结合对破乳的影响，通过对三种破乳工艺条件的单因素分析及进行正交优化，从结果中看出，三种方法均有较好的破乳效果，优化后的得油率均80％以上，尤其是离心破乳与有机溶剂萃取结合起来，其破乳效果更佳，经验证其最高得油率为96.56％，乳液中的乳化脂肪几乎全部分离了出来。比较三种破乳方法，单独采用离心或是有机溶剂破乳其效果并不是很理想，而将二者结合起来其效果更佳，但由于离心与有机溶剂萃取相结合的破乳工艺，将会因为有机溶剂消耗以及需要添置高速离心设备而增加相应成本。因此考虑到经济的可行性，则可采用低速离心设备(5000r／min)，萃取剂用量控制在60％，如离心与有机溶剂相结合破乳正交实验2号实验组合A_1B_2C_2D_2，其出油率亦可达到90.18％。
从对酶解后油和蛋白质的品质研究结果可知，酶解对菜籽油品质有一定影响，采用水酶法制得的油品质都可以达到国家二级油标准，酶解后菜籽油与浸出菜籽油相对密度、折射率没有太大的变化，酶解后酸价、碘值和过氧化值有所提高，这可能与酶解前热处理有一定关系，皂化价有所下降。在菜籽等电点区域内溶解性、持水性、发泡性、乳化性较低，偏离这个等电区域，在等电点左边的pH区域内，随着pH值的降低而升高；在其右边的pH区域内，随pH值的升高而升高。泡沫稳定性与以上情况相反，在等电区域泡沫稳定性好。在水相酶解法工艺过程中，菜籽蛋白发生水解，酶解对菜籽蛋白的功能特性有一定的影响，表现为低度改性，和水剂法工艺相比较，它能显著提高菜籽蛋白溶解性、持水性、发泡性、乳化性、吸油性，但泡沫稳定性和黏度比传统水剂法菜籽蛋白有所降低，这些功能特性的变化使之更有利于用做食品原料。
Aqueous enzymatic extraction technology of rapeseed oil and rapeseed protein has been reported in many literatures in domestic and foreign countries, however, it can not be applied in industry scale because of its disadvantage such as a large variety of enzymes used, a mass of enzymes added, a long time reaction period and low oil yielding. In the dissertation, the optimum technology and mechanism of aqueous enzymatic extraction of rapeseed oil and rapeseed protein have been studied, in order to extract the rapeseed oil and the rapeseed protein simultaneity. The quality of the rapeseed oil and the rapeseed protein has also been researched, on the base of this, it can do a basic theory of the industry application.
This paper studies the process of aqueous enzymatic extraction of rapeseed-oil. The paper includes four parts as follows: the influence of the pretreatment to the aqueous enzymatic extraction of rapeseed-oil,the different methods of enzymolysis and the effect factors, the effect of demulsification to the extraction rate of rapeseed oil,finally we do a research about the effect of enzymolysis to the quality of rapeseed oil anf rapeseed protein.
The pretreatment before enzymolysis has a great influence to the extraction rate of rapeseed oil. Adopt The method of combineing dry grinding and wet grinding,first control the rapeseed grain size about 60-80 mesh ,after heat processing then adopt Tissues homogenate machine to homogenate the rapeseed to be the feasible size of enzymatic reaction. The experiment shows that,the highest quantity could be obtained in the condition of the heating time of ol.5h - 2h, the heating temperature of 90°C and the grinding time of 15 minutes.
Two enzymolysis methods have been discussed in this research,these are: enzymolysis-extracting; enzymolysis_extracting and re-enzymolysis_re-extracting, at the optimum enzymolysis and extraction conditions ,the extraction rate of rapeseed oil are 86.75%, 90.82% respectively. the extraction rate of rapeseed oil is determined by the following factors: the pH of the system, the solid to liquid ratio, the temperature, the degree of grinding and the dosage of enzyme.In the single factor experiments,the optimum conditions of enzymolysis are: When the enzyme dosage is 2%, pH is 7.0 the treatment time is 4h, the solid to liquid ratio is 1:6,the treatment temperature is 50°C,at this condition the rapeseed oil extracting rate is 86.97%,base on the single factor experiments,we do a orthogonal experiment,then we find that the effect factor primary and secondary list is: the content of enzyme > pH>time> temperature;through optimization the rapeseed oil extraction rate reaches 88.56%.
Three demulsification technologies have been researched,those are: the different conditions of centrifugation, Solvents and the combining of centrifugation and Solvents.The results of the experiments showed that: three methods all have a good effect to demulsification, after optimization the extraction ratio are all above 80%, especially the combining of centrifugation and Solvents. The effect is very prominent.The highest extraction rate is96.56%, almost all oil is breakout. Compare three methods, the effect of use single centrifugation or single Solvents is not very ideal,so we should combine them together ,but the technology of the combition may increase cost ,because the large consume of Solvents and need high speed centrifugation machine. we can adopt lower speed centrifugation machine (5000r/min) ,the dosage of Solvents control in 60%,just as the orthogonal experiment 2th the extraction rate of rapeseed oil may reaches 90.18%.
The research results of the quality of rapeseed oil and rapeseed protein showes that enzymolysis, may affect the quality of rapeseed oil ,the oil which is made by enzymolysis can achieve the National secondary standard,there are no remarkable change about the relative density、index of refraction between enzymolysis and non- enzymolysis,but the acid value, iodine value、peroxide value is higher than non-enzymolysis,this may has some to do with the heat treatment ,however, the saponification value is lower than non-enzymolysis.In the isoelectric point area of rapeseed, the solubility、moisture retention、foamability, emulsibility are relative lower ,beyond this area ,on the left area of the isoelectric point,the lower of the pH,the higher of the value , on the left area of the isoelectric point area,the higher of the pH,the higher of the value , but foam-stability is opposite, in the isoelectric point area,the foam stability is good. On the processing of aqueous enzymatic extraction,the rapeseed protein hydrolyzed, enzymolysis has some thing to do with the functional characteristic,that is Low-Grade modification,compare to aqueous extraction ,it can improve the solubility、moisture、retention、foamability、emulsibility、oil absorption ability ,but the foam stability and viscosity are lower than traditional extraction ,these changes make them more favorable for food material.
本文对水相酶法制备菜籽油的工艺进行研究，研究内容包括四个部分：菜籽预处理对水酶法制备菜籽油的影响；酶解方法与酶解影响因素的研究；破乳对得油率影响的研究以及酶解对菜籽油和菜籽品质的影响的研究。
菜籽在酶解前的预处理对菜籽油的收率有很大的影响。采用于碾磨和湿磨相结合的方法，先将油籽破碎粒度控制在60-80目后进行热处理后采用组织匀浆机匀浆，达到适宜酶促反应所需的破碎度。通过试验得出，最佳热处理的时间为1.5h～2.0h，加热温度为90℃，合适的捣碎时间为10～15min。
研究了两种酶解方法，酶解提油，酶解提油再酶解再提油，酶解后用无水乙醚萃取油脂，在试验确定的最适酶解和萃取条件下提油率分别为：86.75％，90.82％。水相酶解提油的效果与体系的pH、料液比、温度、粉碎度、以及酶的添加量等因素有关。由单因数试验得出，酶的最适添加量为2％，pH为7.0，酶处理时间为4h，最佳料液比为1：6，酶作用温度为50℃；在此条件下菜籽的提取率为86.97％，在单因素基础上进行正交试验得出影响因数的主次表：酶的添加量＞pH＞时间＞温度。经过优化以后的菜籽油最高提取率为88.56％。
研究了三种破乳工艺，即不同离心条件、溶剂、离心与溶剂结合对破乳的影响，通过对三种破乳工艺条件的单因素分析及进行正交优化，从结果中看出，三种方法均有较好的破乳效果，优化后的得油率均80％以上，尤其是离心破乳与有机溶剂萃取结合起来，其破乳效果更佳，经验证其最高得油率为96.56％，乳液中的乳化脂肪几乎全部分离了出来。比较三种破乳方法，单独采用离心或是有机溶剂破乳其效果并不是很理想，而将二者结合起来其效果更佳，但由于离心与有机溶剂萃取相结合的破乳工艺，将会因为有机溶剂消耗以及需要添置高速离心设备而增加相应成本。因此考虑到经济的可行性，则可采用低速离心设备(5000r／min)，萃取剂用量控制在60％，如离心与有机溶剂相结合破乳正交实验2号实验组合A_1B_2C_2D_2，其出油率亦可达到90.18％。
从对酶解后油和蛋白质的品质研究结果可知，酶解对菜籽油品质有一定影响，采用水酶法制得的油品质都可以达到国家二级油标准，酶解后菜籽油与浸出菜籽油相对密度、折射率没有太大的变化，酶解后酸价、碘值和过氧化值有所提高，这可能与酶解前热处理有一定关系，皂化价有所下降。在菜籽等电点区域内溶解性、持水性、发泡性、乳化性较低，偏离这个等电区域，在等电点左边的pH区域内，随着pH值的降低而升高；在其右边的pH区域内，随pH值的升高而升高。泡沫稳定性与以上情况相反，在等电区域泡沫稳定性好。在水相酶解法工艺过程中，菜籽蛋白发生水解，酶解对菜籽蛋白的功能特性有一定的影响，表现为低度改性，和水剂法工艺相比较，它能显著提高菜籽蛋白溶解性、持水性、发泡性、乳化性、吸油性，但泡沫稳定性和黏度比传统水剂法菜籽蛋白有所降低，这些功能特性的变化使之更有利于用做食品原料。
Aqueous enzymatic extraction technology of rapeseed oil and rapeseed protein has been reported in many literatures in domestic and foreign countries, however, it can not be applied in industry scale because of its disadvantage such as a large variety of enzymes used, a mass of enzymes added, a long time reaction period and low oil yielding. In the dissertation, the optimum technology and mechanism of aqueous enzymatic extraction of rapeseed oil and rapeseed protein have been studied, in order to extract the rapeseed oil and the rapeseed protein simultaneity. The quality of the rapeseed oil and the rapeseed protein has also been researched, on the base of this, it can do a basic theory of the industry application.
This paper studies the process of aqueous enzymatic extraction of rapeseed-oil. The paper includes four parts as follows: the influence of the pretreatment to the aqueous enzymatic extraction of rapeseed-oil,the different methods of enzymolysis and the effect factors, the effect of demulsification to the extraction rate of rapeseed oil,finally we do a research about the effect of enzymolysis to the quality of rapeseed oil anf rapeseed protein.
The pretreatment before enzymolysis has a great influence to the extraction rate of rapeseed oil. Adopt The method of combineing dry grinding and wet grinding,first control the rapeseed grain size about 60-80 mesh ,after heat processing then adopt Tissues homogenate machine to homogenate the rapeseed to be the feasible size of enzymatic reaction. The experiment shows that,the highest quantity could be obtained in the condition of the heating time of ol.5h - 2h, the heating temperature of 90°C and the grinding time of 15 minutes.
Two enzymolysis methods have been discussed in this research,these are: enzymolysis-extracting; enzymolysis_extracting and re-enzymolysis_re-extracting, at the optimum enzymolysis and extraction conditions ,the extraction rate of rapeseed oil are 86.75%, 90.82% respectively. the extraction rate of rapeseed oil is determined by the following factors: the pH of the system, the solid to liquid ratio, the temperature, the degree of grinding and the dosage of enzyme.In the single factor experiments,the optimum conditions of enzymolysis are: When the enzyme dosage is 2%, pH is 7.0 the treatment time is 4h, the solid to liquid ratio is 1:6,the treatment temperature is 50°C,at this condition the rapeseed oil extracting rate is 86.97%,base on the single factor experiments,we do a orthogonal experiment,then we find that the effect factor primary and secondary list is: the content of enzyme > pH>time> temperature;through optimization the rapeseed oil extraction rate reaches 88.56%.
Three demulsification technologies have been researched,those are: the different conditions of centrifugation, Solvents and the combining of centrifugation and Solvents.The results of the experiments showed that: three methods all have a good effect to demulsification, after optimization the extraction ratio are all above 80%, especially the combining of centrifugation and Solvents. The effect is very prominent.The highest extraction rate is96.56%, almost all oil is breakout. Compare three methods, the effect of use single centrifugation or single Solvents is not very ideal,so we should combine them together ,but the technology of the combition may increase cost ,because the large consume of Solvents and need high speed centrifugation machine. we can adopt lower speed centrifugation machine (5000r/min) ,the dosage of Solvents control in 60%,just as the orthogonal experiment 2th the extraction rate of rapeseed oil may reaches 90.18%.
The research results of the quality of rapeseed oil and rapeseed protein showes that enzymolysis, may affect the quality of rapeseed oil ,the oil which is made by enzymolysis can achieve the National secondary standard,there are no remarkable change about the relative density、index of refraction between enzymolysis and non- enzymolysis,but the acid value, iodine value、peroxide value is higher than non-enzymolysis,this may has some to do with the heat treatment ,however, the saponification value is lower than non-enzymolysis.In the isoelectric point area of rapeseed, the solubility、moisture retention、foamability, emulsibility are relative lower ,beyond this area ,on the left area of the isoelectric point,the lower of the pH,the higher of the value , on the left area of the isoelectric point area,the higher of the pH,the higher of the value , but foam-stability is opposite, in the isoelectric point area,the foam stability is good. On the processing of aqueous enzymatic extraction,the rapeseed protein hydrolyzed, enzymolysis has some thing to do with the functional characteristic,that is Low-Grade modification,compare to aqueous extraction ,it can improve the solubility、moisture、retention、foamability、emulsibility、oil absorption ability ,but the foam stability and viscosity are lower than traditional extraction ,these changes make them more favorable for food material.
引文
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