CN103589502A - Preparation method for blend oil with balanced fatty acid ratio - Google Patents
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Abstract
一种脂肪酸配比均衡调和油的制备方法属于植物油脂提取加工技术,该方法包括以下步骤:(1)将大豆、菜籽、紫苏、火麻子和月见草籽清理、粉碎后按比例混合得混合油料;(2)将混合油料加水配成混合液,然后将混合液进行超声预处理;(3)向超声预处理后的混合液中加入复合酶进行酶解破壁;(4)向复合酶酶解后的混合液中加入蛋白酶进行酶解,酶解后离心分离得到游离油、水解液、乳状液和残渣,乳状液经冷冻解冻破乳后得游离油,合并两次得到的游离油即为脂肪酸配比均衡的调和油;本发明将五种油料按比例混合后利用超声结合酶解制备脂肪酸配比均衡的调和油,脂肪酸配比接近SFA:MUFA:PUFA=0.27:1:1,Omega6:Omega3=1-5:1,能够满足不同人群的营养需求。
A method for preparing blended oil with a balanced ratio of fatty acids belongs to the vegetable oil extraction and processing technology, and the method includes the following steps: (1) Cleaning and crushing soybeans, rapeseeds, perilla, hemp seeds and evening primrose seeds and mixing them in proportion (2) Add water to the mixed oil to form a mixed solution, and then perform ultrasonic pretreatment on the mixed solution; (3) Add complex enzymes to the ultrasonic pretreated mixed solution to break the wall; Protease is added to the mixed solution after compound enzyme enzymolysis for enzymolysis. After enzymolysis, free oil, hydrolyzate, emulsion and residue are obtained by centrifugation. The emulsion is frozen, thawed and demulsified to obtain free oil. The oil is a blended oil with a balanced ratio of fatty acids; the present invention mixes five kinds of oils in proportion and uses ultrasound combined with enzymatic hydrolysis to prepare a blended oil with a balanced ratio of fatty acids, and the ratio of fatty acids is close to SFA:MUFA:PUFA=0.27:1:1 , Omega6:Omega3=1-5:1, which can meet the nutritional needs of different groups of people.
Description
技术领域 technical field
本发明属于植物油脂提取加工技术领域,主要涉及一种脂肪酸配比均衡调和油的制备方法。 The invention belongs to the technical field of vegetable oil extraction and processing, and mainly relates to a method for preparing a blended oil with balanced fatty acid ratio.
背景技术 Background technique
目前,全民健康意识显著提高,而油脂的摄入则是日常生活必不可少的重要部分。近年来,由于高血脂、动脉硬化、冠心病等疾病日益增加,引起人们的关注。而引起这些疾病与人们食用脂肪酸不均衡的油脂有重要关系,过量摄取十二碳以上饱和脂肪酸(不包括硬脂酸)的油脂不但导致人体胆固醇升高,同时引发严重危害人体健康的动脉硬化和冠心病;按适量摄取富含n-6系列(亚油酸、γ- 亚麻酸、花生四烯酸)和n-3系列(α-亚麻酸、EPA、DHA)多不饱和脂肪酸油脂,则具有降低胆固醇含量和低密度脂蛋白(LDL)水平的功能。因此,科学合理均衡的摄入种类不同的脂肪酸,对维持组织的良好功能,保障持久的健康是极为必要的。为此,WHO以及中国营养学会提出脂肪酸的比例参考膳食标准:SFA∶MUFA∶PUFA=0.27:1:1;Omega 6∶Omega 3=1-5:1。 At present, the health awareness of the whole people has been significantly improved, and the intake of fat is an essential part of daily life. In recent years, due to the increasing number of diseases such as hyperlipidemia, arteriosclerosis, and coronary heart disease, it has attracted people's attention. The cause of these diseases is closely related to the unbalanced fatty acid consumption of people. Excessive intake of saturated fatty acids with more than twelve carbons (excluding stearic acid) will not only lead to elevated cholesterol in the human body, but also cause serious damage to human health. Arteriosclerosis and Coronary heart disease; intake of polyunsaturated fatty acids rich in n-6 series (linoleic acid, gamma-linolenic acid, arachidonic acid) and n-3 series (alpha-linolenic acid, EPA, DHA) in an appropriate amount, has Function to lower cholesterol levels and low-density lipoprotein (LDL) levels. Therefore, a scientific, reasonable and balanced intake of different types of fatty acids is extremely necessary to maintain the good function of tissues and ensure long-lasting health. For this reason, the WHO and the Chinese Nutrition Society proposed a reference dietary standard for the ratio of fatty acids: SFA:MUFA:PUFA=0.27:1:1; Omega 6:Omega 3=1-5:1.
传统的调和油生产方法将单一油脂提出后,再按比例调和,此方法不但效率低,成本高,且并未明确高油料作物预处理的方法,从而不能获得较高的提油率,在生产过程中造成大量的原料损失。 The traditional blending oil production method extracts a single oil and then blends it in proportion. This method not only has low efficiency and high cost, but also does not specify the pretreatment method for high-oil crops, so it cannot obtain a higher oil extraction rate. In production A large amount of raw material loss is caused in the process.
本发明的设计的原理是把食用油的脂肪酸比例设计成符合中国营养学会对中国居民的膳食总脂肪酸的摄入比例即:饱和脂肪酸∶单不饱和脂肪酸∶多不饱和脂肪酸=(0-1)∶1∶1,n-6多不饱和脂肪酸∶n-3多不饱和脂肪酸=(1-5)∶1。三种脂肪酸比例尽量接近0.27∶1∶1,且保证Omega 6∶Omega 3比例接近1-5∶1。为解决单一天然油脂的脂肪酸不均衡,以及高油料作物缺少预处理方法的问题,本发明以大豆、菜籽、紫苏、火麻子、月见草籽为原料,先按比例混合后,混合油料进行超声处理结合生物酶法制取脂肪酸配比均衡(SFA∶MUFA∶PUFA=0.27:1:1,Omega 6∶Omega 3=1-5:1)调和油。 The principle of design of the present invention is that the ratio of fatty acid of edible oil is designed to meet the intake ratio of the total dietary fatty acid of Chinese resident by Chinese Nutrition Society: saturated fatty acid: monounsaturated fatty acid: polyunsaturated fatty acid=(0-1) : 1: 1, n-6 polyunsaturated fatty acid: n-3 polyunsaturated fatty acid = (1-5): 1. The ratio of the three fatty acids should be as close to 0.27:1:1 as possible, and the ratio of Omega 6:Omega 3 should be close to 1-5:1. In order to solve the unbalanced fatty acid of a single natural oil and the lack of pretreatment methods for high-oil crops, the present invention uses soybeans, rapeseeds, perilla, hempseeds, and evening primrose seeds as raw materials, and then mixes them in proportion. Ultrasonic treatment combined with bio-enzyme method is used to prepare blended oil with balanced ratio of fatty acids (SFA: MUFA: PUFA = 0.27: 1: 1, Omega 6: Omega 3 = 1-5: 1).
本发明独创将五种原料按比例混合后利用超声波及酶组合双重预处理方式破坏原料细胞壁,提高油脂释放率的同时降低了生物活性物质的损失,即同时获得高营养活性和脂肪酸平衡的调和油。本发明制得调和油脂肪酸比例接近(SFA∶MUFA∶PUFA=0.27:1:1,Omega 6∶Omega 3=1-5:1),能够满足不同人群的生理及营养需求,且仅需一条生产线即可直接制取,价格低廉,营养均衡,脂肪酸比例协调。 The present invention mixes five kinds of raw materials in proportion and then uses ultrasonic and enzyme combination double pretreatment method to destroy raw material cell walls, increase the oil release rate and reduce the loss of biologically active substances, that is to say, the blended oil with high nutritional activity and fatty acid balance can be obtained at the same time . The fatty acid ratio of the blended oil prepared by the present invention is close (SFA: MUFA: PUFA = 0.27: 1: 1, Omega 6: Omega 3 = 1-5: 1), which can meet the physiological and nutritional needs of different groups of people, and only needs one production line It can be directly prepared, and the price is low, the nutrition is balanced, and the fatty acid ratio is coordinated.
发明内容 Contents of the invention
本发明所要解决的技术问题是克服现有技术的不足,为满足人类膳食营养需求,提供一种脂肪酸配比均衡调和油的制备方法。 The technical problem to be solved by the present invention is to overcome the deficiencies of the prior art and provide a method for preparing a blended oil with a balanced ratio of fatty acids in order to meet the dietary nutritional needs of human beings.
本发明所要解决的技术问题是通过以下技术方案来实现的: The technical problem to be solved by the present invention is achieved through the following technical solutions:
一种脂肪酸配比均衡调和油的制备方法,该方法包括以下步骤:(1)将大豆、菜籽、紫苏、火麻子和月见草籽清理后用旋风粉碎机进行粉碎,粉碎后按比例混合得混合油料,所述的混合油料按重量计各成分所占的百分比为:大豆添加量1.1%,菜籽添加量32.5%,紫苏添加量2.3%,火麻子添加量40.5%,月见草籽添加量23.6%;(2)将步骤(1)中得到的混合油料加水配成混合液,所述的混合液料液比为1:5,将混合液进行超声预处理,所述的超声时间为20-60min,超声温度为30-70℃,超声强度为100-500W;(3)将步骤(2)中超声预处理后的混合液调节pH至5.5,然后向混合液中加入复合酶进行酶解破壁,所述的混合酶为果胶酶、纤维素酶和β-葡聚糖酶以质量比4:1:1的比例混合,复合酶添加量为混合液质量的2.6%,酶解温度为55℃,酶解时间为3.5h;(4)将步骤(3)中复合酶酶解后的混合液调节pH至8.1,然后向混合液中加入Alcalase 2.4L碱性蛋白酶进行酶解,所述的蛋白酶添加量为混合液质量的1.88%,酶解温度为48℃,酶解时间为3.5h,酶解后在4500r/min下离心分离30min,得到游离油、水解液、乳状液和残渣,乳状液经冷冻解冻破乳后得游离油,合并两次得到的游离油即为脂肪酸配比均衡的调和油。 A method for preparing blended oil with a balanced ratio of fatty acids, the method comprising the following steps: (1) After cleaning soybeans, rapeseed, perilla, hempseed and evening primrose seeds, they are pulverized with a cyclone mill, and after pulverization, they are proportionally The mixed oil is obtained by mixing, and the percentage of each component by weight of the mixed oil is as follows: 1.1% soybean addition, 32.5% rapeseed addition, 2.3% perilla addition, 40.5% hemp seed addition, monthly see The amount of grass seeds added is 23.6%; (2) The mixed oil obtained in step (1) is added with water to form a mixed solution, the ratio of the mixed solution to liquid is 1:5, and the mixed solution is subjected to ultrasonic pretreatment. The ultrasonic time is 20-60min, the ultrasonic temperature is 30-70°C, and the ultrasonic intensity is 100-500W; (3) Adjust the pH of the mixture after ultrasonic pretreatment in step (2) to 5.5, and then add compound The enzyme is used to enzymatically break the wall, and the mixed enzyme is pectinase, cellulase and β-glucanase mixed in a mass ratio of 4:1:1, and the amount of the compound enzyme added is 2.6% of the mass of the mixed solution , the enzymolysis temperature is 55°C, and the enzymolysis time is 3.5h; (4) Adjust the pH of the mixed solution after the compound enzyme enzymolysis in step (3) to 8.1, and then add Alcalase 2.4L alkaline protease to the mixed solution to carry out Enzymolysis, the amount of protease added is 1.88% of the mass of the mixture, the enzymolysis temperature is 48°C, and the enzymolysis time is 3.5h. After enzymolysis, it is centrifuged at 4500r/min for 30min to obtain free oil, hydrolyzate, Emulsion and residue, the free oil is obtained after the emulsion is frozen, thawed and demulsified, and the free oil obtained by merging twice is the blended oil with a balanced fatty acid ratio.
所述的超声预处理优选参数为:超声时间49.79min,超声温度60.46℃,超声强度408.55W。 The preferred parameters of the ultrasonic pretreatment are: ultrasonic time 49.79min, ultrasonic temperature 60.46°C, ultrasonic intensity 408.55W.
本发明方法是在机械粉碎的基础上,利用超声波作用产生的空泡在爆裂的时候可以产生巨大的剪切力,因此可以有效的破坏油料籽的细胞壁,并使细胞壁内的物质得到释放。而水酶法应用水作为提取媒介,酶作为水解包裹在油脂外面的蛋白,将油脂从油料籽细胞中分离出来。与传统的溶剂浸提相比,超声辅助水酶法提取油脂,操作简单、浸提温度低、提取时间短、节省溶剂、提油率高。 The method of the invention is based on mechanical pulverization, and the cavitation generated by ultrasonic action can generate huge shearing force when bursting, so the cell wall of the oilseed can be effectively destroyed and the substances in the cell wall can be released. The aqueous enzymatic method uses water as the extraction medium, and the enzyme hydrolyzes the protein wrapped around the oil to separate the oil from the oilseed cells. Compared with traditional solvent extraction, ultrasonic-assisted aqueous enzymatic extraction of oil has the advantages of simple operation, low extraction temperature, short extraction time, solvent saving and high oil extraction rate.
本发明方法仅利用一条工艺流程就可以完成油脂的提取。且作用条件温和(常温、无有机溶剂、无剧烈化学反应),体系中的降解产物一般不会与提取物发生反应,可以有效地保护油脂、蛋白质以及胶质等可利用成分的品质。在提取过程中有效利用高新预处理技术,使油脂提油率大大提高。 The method of the invention can complete the oil extraction by using only one process flow. And the action conditions are mild (normal temperature, no organic solvent, no violent chemical reaction), and the degradation products in the system generally do not react with the extract, which can effectively protect the quality of available components such as oil, protein and gum. In the extraction process, the high-tech pretreatment technology is effectively used to greatly increase the oil extraction rate of oil.
本发明与传统制调和油工艺相比主要具有以下工艺优点 : Compared with the traditional blending oil process, the present invention mainly has the following process advantages:
①原料配比混合,仅用一条生产线即可完成提取油脂,大大减少成本。 ① Raw materials are mixed in proportion, and only one production line can be used to complete the oil extraction, which greatly reduces the cost.
②应用高新预处理技术,减少生物活性化合物损失。 ②Application of high-tech pretreatment technology to reduce the loss of biologically active compounds.
③提油技术设备简单、操作安全、效率高。 ③ The oil lifting technology has simple equipment, safe operation and high efficiency.
④所得的毛油质量高、色泽浅、易于精炼。处理条件温和,能生产出脱毒的蛋白产品。 ④The obtained crude oil is of high quality, light in color and easy to refine. Mild treatment conditions can produce detoxified protein products.
⑤生产过程相对能耗低;废水中BOD与COD值大为下降,污染少,易处理。 ⑤ Relatively low energy consumption in the production process; BOD and COD values in wastewater are greatly reduced, less pollution, and easy to handle.
⑥单一利用水酶法提油得到的主要是乳化油,超声与酶结合使用能够很好的破碎细胞,提高油脂提取率,减少乳状液的生成。 ⑥Emulsified oil is mainly obtained by single use of aqueous enzymatic oil extraction. The combination of ultrasound and enzyme can break cells well, improve oil extraction rate, and reduce the formation of emulsion.
附图说明 Description of drawings
图1 本发明总工艺路线图; Fig. 1 general process roadmap of the present invention;
图2 超声时间对混合物料的提油率的影响; Fig. 2 The influence of ultrasonic time on the oil extraction rate of mixed materials;
图3 超声温度对混合物料的提油率的影响图; Fig. 3 The effect diagram of the ultrasonic temperature on the oil extraction rate of the mixed material;
图4 超声强度对混合物料的提油率的影响; Fig. 4 The influence of ultrasonic intensity on the oil extraction rate of mixed materials;
图5 超声时间与超声温度交互作用对总油提取率的相应面分析; Fig. 5 Corresponding surface analysis of the interaction between ultrasonic time and ultrasonic temperature on the extraction rate of total oil;
图6 超声温度与超声强度交互作用对总油提取率的相应面分析。 Fig. 6 Corresponding surface analysis of the interaction between ultrasonic temperature and ultrasonic intensity on the total oil extraction rate.
具体实施方式 Detailed ways
下面结合附图对本发明具体实施例进行详细描述: The specific embodiment of the present invention is described in detail below in conjunction with accompanying drawing:
一种脂肪酸配比均衡调和油的制备方法,该方法包括以下步骤:(1)将大豆、菜籽、紫苏、火麻子和月见草籽清理后用旋风粉碎机进行粉碎,粉碎后按比例混合得混合油料,所述的混合油料按重量计各成分所占的百分比为:大豆添加量1.1%,菜籽添加量32.5%,紫苏添加量2.3%,火麻子添加量40.5%,月见草籽添加量23.6%;(2)将步骤(1)中得到的混合油料加水配成混合液,所述的混合液料液比为1:5,将混合液进行超声预处理,所述的超声时间为20-60min,超声温度为30-70℃,超声强度为100-500W;(3)将步骤(2)中超声预处理后的混合液调节pH至5.5,然后向混合液中加入复合酶进行酶解破壁,所述的混合酶为果胶酶、纤维素酶和β-葡聚糖酶以质量比4:1:1的比例混合,复合酶添加量为混合液质量的2.6%,酶解温度为55℃,酶解时间为3.5h;(4)将步骤(3)中复合酶酶解后的混合液调节pH至8.1,然后向混合液中加入Alcalase 2.4L碱性蛋白酶进行酶解,所述的蛋白酶添加量为混合液质量的1.88%,酶解温度为48℃,酶解时间为3.5h,酶解后在4500r/min下离心分离30min,得到游离油、水解液、乳状液和残渣,乳状液经冷冻解冻破乳后得游离油,合并两次得到的游离油即为脂肪酸配比均衡的调和油。 A method for preparing blended oil with a balanced ratio of fatty acids, the method comprising the following steps: (1) After cleaning soybeans, rapeseed, perilla, hempseed and evening primrose seeds, they are pulverized with a cyclone mill, and after pulverization, they are proportionally The mixed oil is obtained by mixing, and the percentage of each component by weight of the mixed oil is as follows: 1.1% soybean addition, 32.5% rapeseed addition, 2.3% perilla addition, 40.5% hemp seed addition, monthly see The amount of grass seeds added is 23.6%; (2) The mixed oil obtained in step (1) is added with water to form a mixed solution, the ratio of the mixed solution to liquid is 1:5, and the mixed solution is subjected to ultrasonic pretreatment. The ultrasonic time is 20-60min, the ultrasonic temperature is 30-70°C, and the ultrasonic intensity is 100-500W; (3) Adjust the pH of the mixture after ultrasonic pretreatment in step (2) to 5.5, and then add compound The enzyme is used to enzymatically break the wall, and the mixed enzyme is pectinase, cellulase and β-glucanase mixed in a mass ratio of 4:1:1, and the amount of the compound enzyme added is 2.6% of the mass of the mixed solution , the enzymolysis temperature is 55°C, and the enzymolysis time is 3.5h; (4) Adjust the pH of the mixed solution after the compound enzyme enzymolysis in step (3) to 8.1, and then add Alcalase 2.4L alkaline protease to the mixed solution to carry out Enzymolysis, the amount of protease added is 1.88% of the mass of the mixture, the enzymolysis temperature is 48°C, and the enzymolysis time is 3.5h. After enzymolysis, it is centrifuged at 4500r/min for 30min to obtain free oil, hydrolyzate, Emulsion and residue, the free oil is obtained after the emulsion is frozen, thawed and demulsified, and the free oil obtained by merging twice is the blended oil with a balanced fatty acid ratio.
所述的超声预处理优选参数为:超声时间49.79min,超声温度60.46℃,超声强度408.55W。 The preferred parameters of the ultrasonic pretreatment are: ultrasonic time 49.79min, ultrasonic temperature 60.46°C, ultrasonic intensity 408.55W.
the
实施例 调和油混合油料超声工艺参数的确定 Example Determination of Ultrasonic Process Parameters for Blended Oil and Mixed Oil
1. 材料与方法 1. Materials and methods
1.1 材料、试剂 1.1 Materials and reagents
1.2 主要仪器设备 1.2 Main instruments and equipment
1.3 实验方法 1.3 Experimental method
1.3.1 工艺流程(如图1) 1.3.1 Process flow (as shown in Figure 1)
原料→脱壳→粉碎→过筛→加水调节料液比→超声波处理→调节pH值→酶解反应→离心分离→萃取→调和油 Raw materials→hulling→crushing→sieving→adding water to adjust the ratio of solid to liquid→ultrasonic treatment→adjusting the pH value→enzymolysis reaction→centrifugal separation→extraction→blend oil
1.3.2 超声预处理方法 1.3.2 Ultrasonic pretreatment method
物料分别粉碎后,五种物料按照重量比1:1:1:1:1混合,总物料重50g,每种物料各10g ,物料与水1:3混合,蒸煮5min。蒸煮后的物料,室温烘干水分,再与水按照1:6的比例在烧杯中混合,之后将烧杯转移至超声波清洗机中。 After the materials are crushed separately, the five materials are mixed according to the weight ratio of 1:1:1:1:1, the total weight of the material is 50g, each material is 10g, the material is mixed with water at 1:3, and cooked for 5 minutes. The boiled material was dried at room temperature, then mixed with water in a beaker at a ratio of 1:6, and then the beaker was transferred to an ultrasonic cleaner.
1.3.3物料含油量的测定AOAC 922.06 1.3.3 Determination of oil content in materials AOAC 922.06
2.结果与讨论 2. Results and Discussion
2.1 超声工艺单因素条件对混合油料提油率的影响 2.1 Effect of single factor condition of ultrasonic process on oil extraction rate of mixed oil
2.1.1超声波预处理单因素实验 2.1.1 Ultrasonic pretreatment single factor experiment
2.1.1.1超声时间对混合物料的提油率的影响 2.1.1.1 Effect of ultrasonic time on oil extraction rate of mixed materials
在超声温度为50℃,超声功率为500W条件下,考察超声时间对混合物料提油率的影响。从图2中可以看出,当超声时间为50min 的时候,混合物料的提油率达到了最高值,为54.79%。50min之后,随着时间的延长,混合物料的提油率并没有明显的变化,提油率不随超声时间的增加而增加。因此,响应面试验设计中超声时间水平选择在46-54min Under the conditions of ultrasonic temperature of 50℃ and ultrasonic power of 500W, the effect of ultrasonic time on the oil extraction rate of the mixture was investigated. It can be seen from Figure 2 that when the ultrasonic time is 50min, the oil extraction rate of the mixed material reaches the highest value, which is 54.79%. After 50min, with the prolongation of time, the oil extraction rate of the mixture did not change significantly, and the oil extraction rate did not increase with the increase of ultrasonic time. Therefore, in the response surface test design, the ultrasonic time level is selected at 46-54min
2.1.1.2 超声温度对混合物料的提油率的影响 2.1.1.2 Effect of ultrasonic temperature on oil extraction rate of mixed materials
在超声时间为50min,超声功率为500W条件下,考察超声温度对混合物料提油率的影响。从图3中可以看出,混合物料的提油率随超声温度的升高而逐渐升高。在超声温度为60℃ 时,提油率达到了最高值。当超声温度高于60℃时,混合物料提油率不再升高。因此,响应面试验设计中超声温度水平选择在58-62℃。 Under the conditions of ultrasonic time of 50min and ultrasonic power of 500W, the effect of ultrasonic temperature on the oil extraction rate of the mixture was investigated. It can be seen from Figure 3 that the oil extraction rate of the mixed material gradually increases with the increase of ultrasonic temperature. When the ultrasonic temperature is 60°C, the oil extraction rate reaches the highest value. When the ultrasonic temperature is higher than 60°C, the oil extraction rate of the mixture will no longer increase. Therefore, the ultrasonic temperature level was selected at 58-62°C in the response surface test design.
2.1.1.3 超声强度对混合物料的提油率的影响 2.1.1.3 The influence of ultrasonic intensity on the oil extraction rate of mixed materials
在超声时间为50min,超声温度为50℃条件下,考察超声功率对混合物料提油率的影响。从图4中可以看出,混合物料的提油率在超声功率为400W时达到了最高值。继续增加超声功率,提油率略有下降。因此,响应面试验设计中超声功率水平选择在350-450W。 Under the conditions of ultrasonic time of 50min and ultrasonic temperature of 50℃, the effect of ultrasonic power on the oil extraction rate of the mixture was investigated. It can be seen from Figure 4 that the oil extraction rate of the mixed material reaches the highest value when the ultrasonic power is 400W. Continue to increase the ultrasonic power, the oil extraction rate decreased slightly. Therefore, in the design of response surface experiments, the ultrasonic power level is selected at 350-450W.
2.1.2响应面法优化超声波预处理工艺参数 2.1.2 Optimization of ultrasonic pretreatment process parameters by response surface method
响应面共设计了 19组实验优化超声波预处理工艺参数,响应面因素水平编码表见表1,实验方案及结果见表2。 A total of 19 groups of experiments were designed to optimize the process parameters of ultrasonic pretreatment by response surface methodology. The level coding table of response surface factors is shown in Table 1, and the experimental scheme and results are shown in Table 2.
表1 因素水平编码表 Table 1 Factor level coding table
表2响应面实验方案及结果 Table 2 Response surface experiment scheme and results
通过统计分析软件Design-Expert 8.0对数据进行多元回归拟合,对提油率(Y)与超声时间(X1)、超声温度(X2)、超声强度(X3)之间建立二次响应面回归模型如下: The statistical analysis software Design-Expert 8.0 was used to perform multiple regression fitting on the data, and the secondary response was established between the oil extraction rate (Y) and ultrasonic time (X 1 ), ultrasonic temperature (X 2 ), and ultrasonic intensity (X 3 ). The surface regression model is as follows:
Y = 65.33 – 0.18X1 +2.62 X2 + 3.73 X3 + 0.99 X1X2 – 0.24X1X3 – 4.84 X2X3– 3.14 X1 2– 2.47 X2 2– 4.42 X3 2 Y = 65.33 – 0.18X1 + 2.62X2 + 3.73X3 + 0.99X1X2 – 0.24X1X3 – 4.84X2X3 – 3.14X12 – 2.47X22 – 4.42X32
响应面方程方差分析见表3,交互相显著的响应面分析见图5-图6。 The variance analysis of the response surface equation is shown in Table 3, and the response surface analysis of the significant interaction phase is shown in Figures 5-6.
表3响应面方程方差分析 Table 3 Response Surface Equation Analysis of Variance
为了考察模型的拟合度,对模型进行了ANOVA方差分析。从表3 中可以看出,该模型一次项X2、X3、交互项X2X3 、二次项X1 2、X2 2、X3 2的影响极显著,交互项X1X2的影响显著,其他项不显著,表明各因素对于提油率的影响不是简单的线性关系。该模型回归显著(P<0.05),失拟误差不显著(P>0.05),并且该模型R2=99.38%,R2 Adj=98.75%,说明该模型与实验拟合良好,对实验的可预测性为99.38%,该回归方程可以较为准确地分析和预测超声参数与提油率之间的关系。由F检验可以得出因子贡献率为:X3>X2>X1,即超声强度>超声温度>超声时间。 In order to examine the fitting degree of the model, ANOVA analysis of variance was carried out on the model. It can be seen from Table 3 that the influence of the first-order items X 2 , X 3 , interaction items X 2 X 3 , quadratic items X 1 2 , X 2 2 , and X 3 2 of the model is extremely significant, and the interaction item X 1 X 2 The effect of is significant, and the other items are not significant, indicating that the influence of various factors on oil extraction rate is not a simple linear relationship. The regression of the model is significant ( P <0.05), the lack of fit error is not significant ( P >0.05), and the model R 2 =99.38%, R 2 Adj =98.75%, indicating that the model fits well with the experiment and is reliable for the experiment. The predictability is 99.38%. This regression equation can accurately analyze and predict the relationship between ultrasonic parameters and oil extraction rate. From the F test, it can be concluded that the factor contribution rate is: X 3 >X 2 >X 1 , that is, ultrasonic intensity>ultrasonic temperature>ultrasonic time.
应用Design-Expert 设计响应面实验方案,共有19组实验。由超声处理单因素试验得出超声参数水平为:超声时间46-54 min、超声温度58-62℃、超声强度350-450 W。实验得出超声参数之间的交互对提油率的的影响如图5所示。由图看出三个响应面均为开口向下的凸形曲面,同时等高线的最小椭圆都在所示的范围内,说明提油率在所选择的三个因子设计的范围内存在最大值。三个图中提油率随着超声强度和超声温度的升高而升高,且随着超声时间升高到一定程度达到最大值,所以超声温度和超声强度对提油率有着显著的影响。 Design-Expert was used to design the response surface experiment scheme, with a total of 19 groups of experiments. According to the ultrasonic treatment single factor test, the ultrasonic parameter levels were as follows: ultrasonic time 46-54 min, ultrasonic temperature 58-62 ℃, ultrasonic intensity 350-450 W. The experiment shows that the interaction between ultrasonic parameters affects the oil extraction rate, as shown in Figure 5. It can be seen from the figure that the three response surfaces are convex surfaces with the opening downward, and the minimum ellipses of the contour lines are all within the range shown, indicating that the oil extraction rate has a maximum within the range of the selected three factor designs. value. The oil extraction rate in the three figures increases with the increase of ultrasonic intensity and ultrasonic temperature, and reaches the maximum value to a certain extent with the increase of ultrasonic time, so the ultrasonic temperature and ultrasonic intensity have a significant impact on the oil extraction rate.
在此基础上,应用软件对所得到的回归方程进行分析,得到了最佳的超声参数为:超声时间49.79min、超声温度60.46℃、超声强度408.55W,此时的理论提油率为66.12%。对拟合出的超声最优参数进行了验证实验,得到的实际提油率为65.55%,略低于理论提油率66.12%。 On this basis, the software was used to analyze the obtained regression equation, and the optimal ultrasonic parameters were obtained: ultrasonic time 49.79min, ultrasonic temperature 60.46°C, ultrasonic intensity 408.55W, and the theoretical oil extraction rate at this time was 66.12%. . A verification experiment was carried out on the optimal ultrasonic parameters fitted, and the actual oil extraction rate obtained was 65.55%, which was slightly lower than the theoretical oil extraction rate of 66.12%.
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CN104745286A (en) * | 2015-03-09 | 2015-07-01 | 东北农业大学 | Method for extracting maize germ oil by adopting ultrasonic-assisted aqueous enzymatic method |
CN106922853A (en) * | 2017-04-25 | 2017-07-07 | 广州市金妮宝食用油有限公司 | The ready-mixed oil and its production method of a kind of balanced fatty acid |
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CN108913328A (en) * | 2018-08-04 | 2018-11-30 | 望江县振兴植物油厂(普通合伙) | A kind of preparation process of nutrient blend oil |
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CN110826025A (en) * | 2019-11-25 | 2020-02-21 | 佳格食品(中国)有限公司 | Method for optimizing performance of blending oil by using response surface method and matrix method |
CN113046172A (en) * | 2021-03-22 | 2021-06-29 | 安徽理工大学 | Extraction method of luffa seed oil |
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