CN111848340B - A method for extracting nervonic acid and protein from Acer Truncatum Bunge seed - Google Patents
A method for extracting nervonic acid and protein from Acer Truncatum Bunge seed Download PDFInfo
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Abstract
The invention relates to a production method for extracting nervonic acid and protein by using acer truncatum seeds, the protein after alkali extraction and acid precipitation has higher purity, the protein extraction rate is more than 80 percent, and the purity is as high as more than 92 percent; can be widely applied to food additives, and promotes the comprehensive utilization of acer truncatum seed meal. The nervonic acid is extracted by adopting the processes of adsorption, saponification, urea coating, extraction, crystallization and the like, the content of the nervonic acid is improved to more than 90 percent, and the method has the advantages of simple operation, low production cost, capability of simultaneously extracting various components, comprehensive utilization, cost reduction and production benefit improvement.
Description
Technical Field
The invention belongs to the technical field of extraction of medicinal plant components, and particularly relates to a production method for extracting nervonic acid and protein by using acer truncatum seeds.
Background
Nervonic Acid (Nervoic Acid) is a long chain unsaturated fatty Acid, also known as shark Acid, since it is mainly derived from deep sea shark and shark oil. Nervonic acid is originally found in nerve tissues of mammals, has a high content in nerve tissues and brain tissues, is also present in retinas and semen, and is an important component of biological membranes. The extraction from shark oil and brain is limited by resources and cannot be mass-produced. The route of the chemical synthesis of the nervonic acid, the process is complex, the yield is low, and the industrialization can not be realized. The content of nervonic acid in the acer truncatum seeds reaches 2.0 percent, and the long-carbon-chain fatty acid of the acer truncatum seeds contains higher nervonic acid, so that the acer truncatum seeds are a new resource of nervonic acid which can be continuously utilized compared with deep sea shark oil.
The acer truncatum bunge kernel contains 25-27% of protein and no starch, and is fresh in plant seeds. After the kernel extracts the oil, the oil meal is a good edible protein. According to the determination, the protein of the Yuanbaoshu contains 9 kinds of amino acids which are necessary for human body, belongs to complete protein, and the prepared high-quality food has delicious taste and is an ideal protein resource. The functional test of the acer truncatum buge protein shows that the foaming property of the acer truncatum buge seeds is higher than that of the soybean defatted powder, and the acer truncatum buge seeds can be used as egg substitutes to be used as foaming agents for processing baked food or ice cream so as to improve the quality. The acer truncatum seed meal is solid waste generated after the acer truncatum seeds are physically squeezed to extract oil, has low utilization rate, and causes great resource waste and environmental pollution. After the acer truncatum seeds are pressed, a large amount of protein is still remained in the seed meal, which is a great resource waste, and if the acer truncatum seeds can be developed and utilized as a natural plant protein, the utilization rate of the acer truncatum seeds can be improved, and the problem of environmental pollution caused by the waste of the acer truncatum seeds can be solved.
Disclosure of Invention
The invention provides a production method for extracting nervonic acid and protein while having wide raw material sources and low extraction cost and being capable of industrial production.
The invention is realized by the following technical scheme:
a production method for extracting nervonic acid and protein from Acer Truncatum Bunge seeds comprises the following steps:
step a) pressing acer truncatum seeds by a physical squeezing method to obtain acer truncatum crude oil and oil residue, crushing the oil residue to 10-20 meshes, adding 5-15 times of 1% sodium hydroxide solution, extracting at 80-100 ℃ for 1-2 times, each time for 0.5-1.5 hours, filtering, adjusting the pH of filtrate to 7 by hydrochloric acid, standing for 2-6 hours for precipitation, centrifugally separating, and drying in vacuum to obtain a protein finished product;
step b) filtering the acer truncatum crude oil by using an adsorbent, adding alkali into 95% ethanol serving as a solvent to perform saponification reaction for 1-3 hours, filtering, and recovering ethanol to obtain mixed fatty acid salt;
step c), taking mixed fatty acid salt, adding urea ethanol solution in the same volume, stirring for 1 hour, adding 2M hydrochloric acid, reacting for 1 hour at 50-70 ℃, extracting with ethyl acetate, combining extract liquor, and concentrating to obtain a crude product of nervonic acid;
and d) adding acetone into the crude product of the nervonic acid, stirring and crystallizing, centrifugally separating, and drying in vacuum to obtain a nervonic acid product with the content of more than 90%.
Preferably, in step a), the oil residue is crushed and sieved by a sieve of 10-20 meshes, and 10 times of 1% sodium hydroxide solution is added for extraction at 85 ℃ for 1 hour.
Preferably, in the step b), the adsorbent is activated clay, and the dosage of the adsorbent is 5 times of that of the crude oil; adding 95% ethanol 4-8 times the volume of the crude oil, wherein the alkali is potassium hydroxide, the mass of the added alkali is 10% of that of the crude oil, the saponification reaction temperature is 50-80 ℃, and the saponification reaction is carried out for 1-3 hours. More preferably, in step b), 95% ethanol with 6 times volume of the base, wherein the base is potassium hydroxide, the mass of the base is 10% of that of the crude oil, the saponification reaction temperature is 65 ℃, and the saponification reaction time is 2 hours.
Preferably, in step d), the crystallization process is; adding acetone with the volume of 1-3 times of that of the mixture, and stirring and crystallizing for 2-8 hours; more preferably, 2 volumes of acetone are added and crystallization is stirred for 4 hours.
Preferably, in the step a), the oil pressing process is as follows: performing damp-heat treatment on the Acer Truncatum Bunge kernels, adjusting the water content to 8-10%, squeezing by using a shaft-cooled spiral cold squeezer, wherein the squeezing temperature is not higher than 65 ℃, the cake residual oil is not higher than 12%, and squeezing to obtain crude oil.
Preferably, step a) pulverizes the oil residue to 10-20 mesh, and adds 10 times of 1% sodium hydroxide solution to extract 1 time at 90 deg.C, each time for 1 hour.
Preferably, in the step b), the adsorbent is activated clay, and the dosage of the adsorbent is 4-8 times of the weight of the crude oil; more preferably, the adsorbent is activated clay, and the dosage is 5 times of the weight of the crude oil.
Preferably, in step c), the ratio of urea: mixed fatty acid salt: 95% ethanol at a w/w/v ratio of 1-2:1:5-15. More preferably, the ratio of urea: mixed fatty acid salt: 95% ethanol in a w/w/v ratio of 1.5:1:10.
the invention has the following beneficial technical effects:
1) According to the extraction method for simultaneously extracting the protein and the nervonic acid from the acer truncatum bunge kernel, the protein purity after alkali extraction and acid precipitation is higher, the protein extraction rate is more than 80%, and the purity is as high as more than 92%; can be widely applied to food additives, and promotes the comprehensive utilization of acer truncatum seed meal. The invention adopts the processes of adsorption, saponification, urea coating, extraction, crystallization and the like to improve the nervonic acid content to more than 90 percent, and has the advantages of simple operation, low production cost, capability of simultaneously extracting a plurality of components, comprehensive utilization, cost reduction and production benefit improvement.
2) The activated clay is used as an adsorbent, so that the activated clay has the advantages of great decolorizing capacity, strong adsorption capacity, high decolorizing rate, low oil carrying rate, high filtering speed and small addition amount; can effectively remove the total phospholipid, soap and trace metal ions of the grease; the acid value of the decolorized oil product is not increased, the decolorized oil product is not discolored, is clear and transparent, and has stable quality and long quality guarantee period.
Drawings
The invention is further described below with reference to the accompanying drawings:
FIG. 1 is a flow chart of the production process of the present invention;
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, a detailed description of the present invention will be given below in conjunction with the accompanying drawings and specific embodiments. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflict. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Example 1:
1. squeezing the acer truncatum bunge kernels: regulating the moisture content of the acer truncatum bunge kernel after the wet heat treatment to 8-10%, squeezing by using a shaft-cooling type spiral cold squeezer, wherein the squeezing temperature is not higher than 65 ℃, the cake residual oil is not higher than 12%, and filtering crude oil obtained by squeezing at the temperature of not higher than 18 ℃.
2. Weighing 10 kg of acer truncatum seeds, squeezing oil, extracting 3.5 kg of oil, 6 kg of residue, crushing the oil residue to 10-20 meshes, extracting for 1 hour at 85 ℃ by 10 times of 1% sodium hydroxide, filtering, adjusting the pH value to 7 by hydrochloric acid, standing for 4 hours for precipitation, performing centrifugal separation, and performing vacuum drying at 65 ℃ to obtain 5 kg of protein, wherein the protein extraction rate is 83%, and the purity is as high as 94%.
3. Filtering the oil with 5 times of active clay, adding 30 kg of 95% ethanol and 0.35 kg of potassium hydroxide, heating at 65 ℃ for 2 hours, filtering, recovering ethanol, adding 1 kg of urea and 10 kg of 95% ethanol, stirring for 1 hour, adding 2M hydrochloric acid, reacting at 60 ℃ for 1 hour, placing the mixture to room temperature, extracting with ethyl acetate, concentrating, adding 2 times of acetone by volume, stirring and crystallizing for 4 hours, centrifuging, and drying in vacuum at 50 ℃ to obtain 0.05 kg of nervonic acid product with the content of 90%.
Example 2:
1. squeezing the acer truncatum kernels: regulating the moisture content of the Acer Truncatum Bunge kernels to 8-10% through wet heat treatment, squeezing by using an axial cooling type spiral cold squeezer, wherein the squeezing temperature is not higher than 65 ℃, the cake residual oil is not higher than 12%, and filtering crude oil obtained through squeezing at the temperature of not higher than 18 ℃.
2. Weighing 50 kg of acer truncatum seeds, squeezing oil, extracting 18.5 kg of oil, 29 kg of residue, crushing the oil residue to 10-20 meshes, extracting for 1 hour at 90 ℃ by 10 times of 1% sodium hydroxide, filtering, adjusting the pH value to 7 by hydrochloric acid, standing for 4 hours for precipitation, performing centrifugal separation, and performing vacuum drying at 65 ℃ to obtain 23.5 kg of protein, wherein the extraction rate of the protein is 81%, and the purity is as high as 93%.
3. Filtering the oil with 6 times of active clay, adding 150 kg of 95% ethanol and 1.75 kg of potassium hydroxide, heating at 65 ℃ for 2 hours, filtering, recovering ethanol, adding 5 kg of urea and 50 kg of 95% ethanol, stirring for 1 hour, adding 2M hydrochloric acid, reacting at 60 ℃ for 1 hour, placing the mixture to room temperature, extracting with ethyl acetate, concentrating, adding 2 times of acetone by volume, stirring and crystallizing for 4 hours, centrifuging, and drying in vacuum at 50 ℃ to obtain 0.28 kg of nervonic acid product with the content of 90%.
Example 3:
1. squeezing the acer truncatum bunge kernels: regulating the moisture content of the acer truncatum bunge kernel after the wet heat treatment to 8-10%, squeezing by using a shaft-cooling type spiral cold squeezer, wherein the squeezing temperature is not higher than 65 ℃, the cake residual oil is not higher than 12%, and filtering crude oil obtained by squeezing at the temperature of not higher than 18 ℃.
2. Weighing 10 kg of acer truncatum seeds, squeezing oil, wherein 3.5 kg of oil is produced, 6 kg of residue is produced, the oil residue is crushed to 10-20 meshes, 12 times of 1% sodium hydroxide is added, extraction is carried out at 80 ℃ for 1.5 hours, hydrochloric acid is used for adjusting the pH value to 7 after filtration, the mixture is placed for 4 hours for precipitation, centrifugal separation is carried out, vacuum drying is carried out at 65 ℃,5 kg of protein is obtained, the protein extraction rate is 84%, and the purity is as high as 92%.
3. Filtering the oil with 5 times of active clay, adding 28 kg of 95% ethanol and 0.42 kg of potassium hydroxide, heating at 60 ℃ for 2 hours, filtering, recovering ethanol, adding 1 kg of urea and 10 kg of 95% ethanol, stirring for 1 hour, adding 2M hydrochloric acid, reacting at 60 ℃ for 1 hour, cooling to room temperature, extracting with ethyl acetate, concentrating, adding 2 times of acetone by volume, stirring for crystallizing for 4 hours, centrifuging, and drying at 50 ℃ in vacuum to obtain 0.05 kg of a nervonic acid product with the content of 93%.
Example 4:
1. squeezing the acer truncatum bunge kernels: regulating the moisture content of the Acer Truncatum Bunge kernels to 8-10% through wet heat treatment, squeezing by using an axial cooling type spiral cold squeezer, wherein the squeezing temperature is not higher than 65 ℃, the cake residual oil is not higher than 12%, and filtering crude oil obtained through squeezing at the temperature of not higher than 18 ℃.
2. Weighing 50 kg of acer truncatum seeds, squeezing oil, extracting 19 kg of oil, 30 kg of residue, crushing the oil residue to 10-20 meshes, adding 8 times of 1% sodium hydroxide, extracting for 2 times at 100 ℃ for 0.5 hour each time, filtering, adjusting the pH value to 7 with hydrochloric acid, standing for 4 hours for precipitation, performing centrifugal separation, and performing vacuum drying at 65 ℃ to obtain 23.5 kg of protein, wherein the protein extraction rate is 85%, and the purity is as high as 92%.
3. Filtering the oil with activated clay 8 times the mass of the oil, adding 150 kg of 95% ethanol and 1.5 kg of potassium hydroxide, heating at 80 ℃ for 3 hours, filtering, recovering ethanol, adding 5 kg of urea and 50 kg of 95% ethanol, stirring for 1 hour, adding 2M hydrochloric acid, reacting at 60 ℃ for 1 hour, placing the mixture to room temperature, extracting with ethyl acetate, concentrating, adding 2 times the volume of acetone, stirring and crystallizing for 4 hours, centrifuging, and drying in vacuum at 50 ℃ to obtain 0.3 kg of a nervonic acid product with the content of 92%.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (2)
1. A production method for extracting nervonic acid and protein from Acer Truncatum Bunge seeds is characterized by comprising the following steps:
step a), pressing acer truncatum seeds by a physical squeezing method to obtain acer truncatum crude oil and oil residue, crushing the oil residue into 10-20 meshes, adding 8-12 times of 1% sodium hydroxide solution, extracting at 80-100 ℃ for 1-2 times for 0.5-1.5 hours each time, filtering, adjusting the pH of filtrate to 7 by hydrochloric acid, standing for 2-6 hours for precipitation, carrying out centrifugal separation, and carrying out vacuum drying to obtain a protein finished product; in the step a), the squeezing oil pressing process comprises the following steps: carrying out damp-heat treatment on the acer truncatum kernels, adjusting the water content to 8-10%, squeezing by using an axial cooling type spiral cold squeezer, wherein the squeezing temperature is not higher than 65 ℃, the cake residual oil is not higher than 12%, and squeezing to obtain crude oil;
step b), filtering the acer truncatum crude oil by using an adsorbent, adding alkali into 95% ethanol serving as a solvent for saponification reaction, filtering, and recovering ethanol to obtain mixed fatty acid salt; the adsorbent is activated clay, and the dosage of the adsorbent is 4-8 times of the weight of the crude oil; adding 95% ethanol 4-8 times the volume of the crude oil, wherein the alkali is potassium hydroxide or sodium hydroxide, the mass of the added alkali is 8-12% of the mass of the crude oil, the saponification reaction temperature is 50-80 ℃, and the saponification reaction is carried out for 1-3 hours;
step c), taking mixed fatty acid salt, adding urea ethanol solution in the same volume, stirring for 1 hour, adding 2M hydrochloric acid, reacting for 1 hour at 50-70 ℃, extracting with ethyl acetate, combining extract liquor, and concentrating to obtain a crude product of nervonic acid; in step c), urea: mixed fatty acid salt: 95% ethanol at a w/w/v ratio of 1-2:1:5-15;
step d), adding acetone into the crude product of nervonic acid, stirring and crystallizing, centrifugally separating, and drying in vacuum to obtain a nervonic acid product with the content of more than 90%, wherein the crystallization process is as follows; adding acetone with the volume of 1-3 times of that of the mixture, and stirring and crystallizing for 2-8 hours.
2. The method for extracting nervonic acid and protein from Acer truncatum seeds as claimed in claim 1, wherein the method comprises the following steps:
in the step a), oil residue is crushed and sieved by a sieve with 10-20 meshes, and 10 times of 1 percent sodium hydroxide solution is added for extraction for 1 hour at 90 ℃;
in the step b), the adsorbent is activated clay, and the dosage of the adsorbent is 5 times of the weight of the crude oil; adding 95% ethanol with 6 times volume of potassium hydroxide, adding 10% alkali by mass of the crude oil, performing saponification at 65 ℃, and performing saponification for 2 hours;
in step c), urea: mixed fatty acid salt: 95% ethanol at a w/w/v ratio of 1.5:1:10;
in the step d), the crystallization process is as follows; acetone was added in 2 volumes and crystallized with stirring for 4 hours.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104928011A (en) * | 2015-05-21 | 2015-09-23 | 西安中粮工程研究设计院有限公司 | Production process for producing Acer trunctum Bunge oil and Acer trunctum Bunge protein powder by using Acer trunctum Bunge seed as raw material |
| CN108949875A (en) * | 2018-06-26 | 2018-12-07 | 浙江健智元生物科技有限公司 | A kind of preparation method of acer truncatum seed active peptide |
| CN109734577A (en) * | 2019-01-10 | 2019-05-10 | 邢永涛 | The method of acer truncatum buge oil extraction nervonic acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104928011A (en) * | 2015-05-21 | 2015-09-23 | 西安中粮工程研究设计院有限公司 | Production process for producing Acer trunctum Bunge oil and Acer trunctum Bunge protein powder by using Acer trunctum Bunge seed as raw material |
| CN108949875A (en) * | 2018-06-26 | 2018-12-07 | 浙江健智元生物科技有限公司 | A kind of preparation method of acer truncatum seed active peptide |
| CN109734577A (en) * | 2019-01-10 | 2019-05-10 | 邢永涛 | The method of acer truncatum buge oil extraction nervonic acid |
Non-Patent Citations (2)
| Title |
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| 元宝枫籽油及神经酸制取工艺;徐明辉等;《粮食与食品工业》;20171231;第24卷(第1期);41-43 * |
| 尿素包合法富集文冠果油中神经酸的研究;郭莹莹等;《中国油脂》;20181231;第43卷(第7期);119-123 * |
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