Method for separating and purifying nervonic acid in acer truncatum buge oil by combining molecular distillation with urea inclusion method
阅读说明：本技术 一种用分子蒸馏结合尿素包合法分离纯化元宝枫油中神经酸的方法 (Method for separating and purifying nervonic acid in acer truncatum buge oil by combining molecular distillation with urea inclusion method ) 是由 孙华 于功明 刘万通 秦大伟 姜磊 刘速速 于 2020-07-20 设计创作，主要内容包括：本发明涉及脂肪酸的分离纯化工艺技术领域,具体地涉及一种用分子蒸馏结合尿素包合法分离纯化元宝枫油中神经酸的方法,通过采用分子蒸馏结合尿素包合法分离纯化元宝枫油中神经酸,具体设计为先将元宝枫油、乙醇及碱性催化剂混合加热进行酯化反应,得到混合脂肪酸；再将混合脂肪酸在不同的真空条件及温度下进行分子蒸馏；得到含神经酸的重组分；分子蒸馏后的重组分与尿素在一定的包合温度、时间下进行尿素包合,得到纯度较高的神经酸。本发明提高了神经酸产量与纯度及生产效率,应用环境良好。(The invention relates to the technical field of fatty acid separation and purification processes, in particular to a method for separating and purifying nervonic acid in acer truncatum buge oil by combining molecular distillation with a urea inclusion method, wherein the nervonic acid in the acer truncatum oil is separated and purified by combining the molecular distillation with the urea inclusion method, and the method is specifically designed by mixing and heating the acer truncatum oil, ethanol and an alkaline catalyst for esterification reaction to obtain mixed fatty acid; then carrying out molecular distillation on the mixed fatty acid under different vacuum conditions and temperatures; obtaining heavy components containing nervonic acid; carrying out urea inclusion on the recombined after molecular distillation and urea at a certain inclusion temperature for a certain time to obtain nervonic acid with higher purity. The invention improves the yield, purity and production efficiency of nervonic acid and has good application environment.)
1. A method for separating and purifying nervonic acid in acer truncatum buge oil by combining molecular distillation with a urea inclusion method is characterized by comprising the following steps: the method comprises the following process steps:
(1) mixing Acer truncatum oil with 0.5-2mol/L KOH-CH3CH2Heating OH on a water bath; shaking occasionally during heating until the solution is clear and transparent;
(2) after the solution is cooled to room temperature, regulating the pH value to 2-3 by hydrochloric acid, transferring the solution into a separating funnel, extracting by petroleum ether, standing and layering, taking an upper layer organic phase, washing to be neutral, removing water by anhydrous sodium sulfate, performing rotary evaporation on the solution in a water bath, and recovering petroleum ether to obtain mixed fatty acid;
(3) carrying out molecular distillation on the mixed fatty acid under different vacuum conditions and temperatures;
(4) urea was mixed according to a 1: 4-1: dissolving 7 in 95% ethanol, heating in water bath for dissolving, stirring, adding fatty acid after urea is completely dissolved, taking out, and cooling to room temperature;
(5) performing urea inclusion, and performing suction filtration and separation on the urea inclusion compound to obtain a crystal part and a filtrate part, wherein nervonic acid exists in the crystal part;
(6) and (3) taking a urea clathrate crystallization part, washing urea with distilled water, extracting with petroleum ether, standing for layering, taking an upper layer organic phase, removing water from anhydrous sodium sulfate, performing rotary evaporation on the solution in a water bath, and recovering petroleum ether to obtain a nervonic acid sample.
2. The method for separating and purifying nervonic acid in acer truncatum buge oil by using molecular distillation combined with urea inclusion method as claimed in claim 1, wherein: in the step (1), the Acer truncatum oil is 100-; the KOH-CH3CH2OH was 150-250 ml.
3. The method for separating and purifying nervonic acid in acer truncatum buge oil by using molecular distillation combined with urea inclusion method as claimed in claim 1, wherein: the water bath temperature in the step (1) is 60-80 ℃, and the heating time is 1-2 h.
4. The method for separating and purifying nervonic acid in acer truncatum buge oil by using molecular distillation combined with urea inclusion method as claimed in claim 1, wherein: the temperature of the water bath in the step (2) is 40-60 ℃.
5. The method for separating and purifying nervonic acid in acer truncatum buge oil by using molecular distillation combined with urea inclusion method as claimed in claim 1, wherein: the temperature of the water bath in the step (4) is 50-60 ℃.
6. The method for separating and purifying nervonic acid in acer truncatum buge oil by using molecular distillation combined with urea inclusion method as claimed in claim 1, wherein: in the step (4), the ratio of urine to fat is 3: 2-1: 2, adding fatty acid.
7. The method for separating and purifying nervonic acid in acer truncatum buge oil by using molecular distillation combined with urea inclusion method as claimed in claim 1, wherein: in the step (5), urea inclusion is carried out under the conditions that the inclusion temperature is 0-10 ℃ and the inclusion time is 8-14 h.
8. The method for separating and purifying nervonic acid in acer truncatum buge oil by using molecular distillation combined with urea inclusion method as claimed in claim 1, wherein: the temperature of the water bath in the step (6) is 40-60 ℃.
Technical Field
The invention relates to the technical field of fatty acid separation and purification processes, in particular to a method for separating and purifying nervonic acid in acer truncatum buge oil by using a molecular distillation combined urea inclusion method.
Background
The acer truncatum buge oil has the function of regulating immunity, can improve the activity of immunocytes, and can improve the dual functions of cellular immunity and humoral immunity of an organism to enhance the immunity of the organism. Meanwhile, the acer truncatum buge oil also has a plurality of obvious health-care functions of resisting fatigue, resisting aging, regulating blood fat, regulating cardiovascular circulation of a human body and the like. The acer truncatum buge oil is rich in various functional substances and essential fatty acids, wherein the ratio of the unsaturated fatty acids is as high as more than 90%, and the unsaturated fatty acids are necessary for human bodies and also substances which cannot be synthesized by the bodies and can only be taken in from the outside. The nervonic acid in the acer truncatum buge oil has an important function as monounsaturated fatty acid, is a double-effect miraculous substance which is acknowledged by world scientists and can only repair and dredge nerve fibers of damaged cerebral nerve pathways and promote nerve cell regeneration, and the lack of the double-effect miraculous substance can cause cerebral diseases such as cerebral apoplexy sequelae, senile dementia, cerebral palsy, encephalatrophy, hypomnesis, insomnia, amnesia and the like. The body itself is difficult to generate nervonic acid, and can only be supplemented by in vitro intake. At present, nervonic acid at home and abroad is mainly derived from deep sea fish oil and shark brain, and the extraction of nervonic acid from the raw materials is difficult and high in cost. Therefore, the gap of nervonic acid in domestic and foreign markets is very large, the acer truncatum has become an important new resource for developing nervonic acid, and the gap of the nervonic acid market at home and foreign can be filled.
The molecular distillation technology is to separate liquid mixture by utilizing the difference of molecular motion free path, can rapidly separate light molecules and heavy molecules in the mixture under the conditions of high vacuum degree and low operation temperature, and can better protect the effective components of high boiling point and heat sensitive materials. Molecular distillation techniques are considered to be far superior to conventional heat-processing treatments because they greatly reduce the deleterious changes in the organoleptic and physical properties of the food, minimize waste and are safer.
The urea in the urea-synthesizing method is crystallized into a tetragonal body, and when the urea is dissolved in an organic solvent and meets an aliphatic compound, urea molecules are combined by hydrogen bonds to form a hexahedral structure. The diameter of the straight-chain saturated fatty acid or monounsaturated fatty acid is smaller than the free volume of the formed hexahedron, so that the saturated fatty acid or monounsaturated fatty acid can enter the unit cell in the crystallization process and be included in the unit cell, and then urea inclusion compound is formed to be separated out, so that the saturated fatty acid and monounsaturated fatty acid are separated from the polyunsaturated fatty acid. The urea inclusion method has the advantages of low production cost, simple and easy operation method and suitability for large-scale production.
In order to reduce the cost and improve the efficiency in the separation and purification process, a method combining an advanced extraction technology and a traditional technology is needed to be designed, namely a method for separating and purifying nervonic acid in acer truncatum buge oil by combining molecular distillation and a urea inclusion method is used, so that the yield and the purity of the nervonic acid can be improved, and the production efficiency of the nervonic acid can also be improved.
Disclosure of Invention
The invention aims to provide a method for separating and purifying nervonic acid in acer truncatum buge oil by combining molecular distillation with a urea inclusion method, which solves the problems of great difficulty and high cost in extracting nervonic acid in the prior art, improves the yield and purity of nervonic acid, and also improves the production efficiency of nervonic acid.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for separating and purifying nervonic acid in acer truncatum buge oil by combining molecular distillation with a urea inclusion method comprises the following process steps:
(1) mixing Acer truncatum oil with 0.5-2mol/L KOH-CH3CH2Heating OH on a water bath; shaking occasionally during heating until the solution is clear and transparent;
(2) after the solution is cooled to room temperature, regulating the pH value to 2-3 by hydrochloric acid, transferring the solution into a separating funnel, extracting by petroleum ether, standing and layering, taking an upper layer organic phase, washing to be neutral, removing water by anhydrous sodium sulfate, performing rotary evaporation on the solution in a water bath, and recovering petroleum ether to obtain mixed fatty acid;
(3) Carrying out molecular distillation on the mixed fatty acid under different vacuum conditions and temperatures;
(4) urea was mixed according to a 1: 4-1: dissolving 7 in 95% ethanol, heating in water bath for dissolving, stirring, adding fatty acid after urea is completely dissolved, taking out, and cooling to room temperature;
(5) performing urea inclusion, and performing suction filtration and separation on the urea inclusion compound to obtain a crystal part and a filtrate part, wherein nervonic acid exists in the crystal part;
(6) and (3) taking a urea clathrate crystallization part, washing urea with distilled water, extracting with petroleum ether, standing for layering, taking an upper layer organic phase, removing water from anhydrous sodium sulfate, performing rotary evaporation on the solution in a water bath, and recovering petroleum ether to obtain a nervonic acid sample.
Preferably, in the step (1), the Acer truncatum buge oil is 100-200 g; the KOH-CH3CH2OH was 150-250 ml.
Preferably, the temperature of the water bath in the step (1) is 60-80 ℃, and the heating time is 1-2 h.
Preferably, the temperature of the water bath in the step (2) is 40-60 ℃.
Preferably, the temperature of the water bath in the step (4) is 50-60 ℃.
Preferably, in the step (4), the ratio of urine to fat in the urine is 3: 2-1: 2, adding fatty acid.
Preferably, in the step (5), the urea inclusion is carried out under the conditions that the inclusion temperature is 0-10 ℃ and the inclusion time is 8-14 h.
Preferably, the temperature of the water bath in the step (6) is 40-60 ℃.
The final purity of the nervonic acid measured by the method is more than 40%.
The step (1) belongs to saponification reaction, wherein the saponification reaction is a reaction of grease and potassium hydroxide to generate higher fatty acid salt and glycerol, and the step is to completely hydrolyze glyceride to free nervonic acid; in the step (2), after sample acidification treatment, part containing nervonic acid is extracted from petroleum ether according to the principle of similarity and compatibility to prepare mixed fatty acid, and pretreatment is performed for next step of separation and purification of nervonic acid; in the step (3), the light components and the heavy components are separated according to different average free degrees of the light components and the heavy components in the fatty acid, so that the purity of the nervonic acid is improved; in the step (4), urea is crystallized into a tetragonal body, the urea is dissolved in an organic solvent, urea molecules are combined by hydrogen bonds to form a hexahedron when meeting fatty compounds, nervonic acid serving as monounsaturated fatty acid has a diameter smaller than the free volume of the formed hexahedron, and the nervonic acid can enter a crystal cell in the crystallization process to form a stable urea inclusion compound, so that the purity of the nervonic acid is improved; in the step (5), the crystallized part is separated from the filtrate part, namely, the part containing nervonic acid is separated from the polyunsaturated fatty acid, so that the purity of nervonic acid is improved; in the step (6), the fatty acid containing the nervonic acid part is dissolved in the organic solvent according to the principle of similar compatibility, and then the nervonic acid part is separated from the solvent through reduced pressure evaporation to obtain the nervonic acid sample.
The invention has the technical effects that:
compared with the prior art, the method for separating and purifying nervonic acid in acer truncatum buge oil by using the molecular distillation combined with the urea inclusion method, disclosed by the invention, separates and purifies nervonic acid in acer truncatum buge oil by using the molecular distillation combined with the urea inclusion method, and is specifically designed as follows: firstly, mixing and heating acer truncatum buge oil, ethanol and an alkaline catalyst to perform esterification reaction to obtain mixed fatty acid; then carrying out molecular distillation on the mixed fatty acid under different vacuum conditions and temperatures; obtaining heavy components containing nervonic acid; carrying out urea inclusion on the recombined after molecular distillation and urea at a certain inclusion temperature for a certain time to obtain nervonic acid with higher purity. The design of the steps and the cooperative matching of the steps improve the yield and the purity of the nervonic acid, simultaneously improve the production efficiency and have good application environment.
Detailed Description
The invention is further illustrated by the following specific examples.