CN115011642A - Method for preparing structured lipid rich in EPA and DHA by using tuna - Google Patents
Method for preparing structured lipid rich in EPA and DHA by using tuna Download PDFInfo
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Abstract
The invention discloses a method for preparing structural lipid rich in EPA and DHA by using tuna, which comprises the following steps: s1, pretreating raw materials, and sequentially cleaning, drying, freeze-drying and wall breaking viscera of tuna to obtain tuna powder; s2, extracting and separating lipid, processing tuna powder by an ultrasonic-assisted solvent extraction method to obtain crude lipid, purifying and removing impurities from the crude lipid by a Folch method, adding cold acetone into the crude lipid after the impurities are removed, carrying out low-temperature sedimentation, separating supernatant liquid, carrying out rotary evaporation to obtain triglyceride type fish oil, and blowing off acetone residues from insoluble nitrogen to obtain phospholipid type fish oil; s3, preparing the triglyceride type fish oil rich in EPA and DHA by using the triglyceride type fish oil and the fatty acid ethyl ester rich in EPA and DHA for ester exchange. It can be used for preparing structural lipid rich in EPA and DHA, and has high EPA and DHA content and good absorption effect.
Description
Technical Field
The invention relates to a method for preparing a structural lipid rich in EPA and DHA, in particular to a method for preparing a structural lipid rich in EPA and DHA by using tuna.
Background
EPA and DHA are useful in inhibiting inflammation, promoting development of visual system, preventing cardiovascular disease, and improving memory. The intake of a suitable amount of DHA during childhood is particularly important because DHA is a major component of brain, eye and nerve tissue, and is also associated with gestation time and incidence of preterm labor. The ALA, EPA and DHA derived lipin, lytic molecule, protective agent, etc. can not only inhibit inflammation, but also enhance healing, enhance phagocytosis of macrophage and other immune cells, reduce microbial load, and even have the possibility of antivirus. DHA is essential for brain tissue and contributes more than 40% of PUFAs in neuronal membranes.
EPA and DHA belong to the family of omega-3 polyunsaturated fatty acids, as essential fatty acids for the human body, mainly from two sources: one is to metabolise linolenic acid taken from plants to synthesis by in vivo dehydrogenases and elongases, but this pathway has a very limited amount of DHA that can be synthesized. Another way is by direct dietary supplementation, EPA and DHA are common in foods of marine origin, and EPA and DHA are also present in eggs and freshwater fish, in addition to which synthetic dietary supplements can achieve higher purity of EPA and DHA, mainly enriched from algal and fish oils. The edible synthetic supplement has the advantage of high safety because the marine products have methyl mercury and organochlorine (polychlorinated biphenyl, dioxin) pollution, edible fishes and marine mammals are the only way for human beings to contact methyl mercury, tuna viscera are rich in various lipids, phospholipid and glyceride contents are high, and EPA and DHA are rich, and the edible fishes and the marine mammals are important resources for comprehensive utilization of marine biological processing wastes in recent years, but fish oil directly prepared from the tuna has low EPA and DHA contents, namely the lipid with EPA and DHA chains accounts for a small proportion of the total lipid. The natural delivery forms of EPA and DHA are triglyceride, phospholipid, and a small amount of other acylglycerol and free fatty acid, and as a supplement, the three forms of triglyceride, phospholipid and ethyl ester are mainly used, the first commercialized form is the ethyl ester form, and most studies show that triglyceride type EPA and DHA and phospholipid type EPA and DHA can be digested more effectively than ethyl ester type EPA and DHA, but concentrated EPA and DHA in the current market are usually produced in the form of fatty acid ethyl ester, and ethyl ester type EPA and DHA are poor in utilization effect, cannot be well absorbed and utilized by human bodies, and are poor in use effect.
Disclosure of Invention
The invention aims to provide a method for preparing a structural lipid rich in EPA and DHA by using tuna. It can be used for preparing structural lipid rich in EPA and DHA, and has high EPA and DHA content and good absorption effect.
The technical scheme of the invention is as follows: a method for preparing EPA and DHA enriched structural lipid by using tuna comprises the following steps:
s1, pretreating raw materials, and sequentially cleaning, drying, freeze-drying and wall breaking viscera of tuna to obtain tuna powder;
s2, extracting and separating lipid, processing tuna powder by an ultrasonic-assisted solvent extraction method to obtain crude lipid, purifying and removing impurities from the crude lipid by a Folch method, adding cold acetone into the crude lipid after the impurities are removed, carrying out low-temperature sedimentation, separating supernatant liquid, carrying out rotary evaporation to obtain triglyceride type fish oil, and blowing off acetone residues from insoluble nitrogen to obtain phospholipid type fish oil;
s3, carrying out ester exchange on triglyceride type fish oil and fatty acid ethyl ester rich in EPA and DHA to prepare triglyceride type fish oil rich in EPA and DHA;
and S4, performing ester exchange on the phospholipid fish oil and the fatty acid ethyl ester rich in EPA and DHA to prepare the phospholipid fish oil rich in EPA and DHA.
In the aforementioned method for preparing structural lipid rich in EPA and DHA from tuna, the transesterification process in S3 comprises:
taking 1-5 parts by mass of fatty acid ethyl ester rich in EPA and DHA in a reaction container, and adding 0.5-2.5% of pure water by mass of the total mass of reaction substrates;
adding 5-25% of lipase based on the total mass of the reaction substrate, placing the mixture in a magnetic stirrer for stirring and heating in water bath, and setting the rotating speed at 400 rpm. In order to avoid fat oxidation and degradation in the process, the reaction vessel is connected with a vacuum pump by a leather hose so that the system is in a vacuum state of 5 Pa;
thirdly, 1 part of triglyceride type fish oil in mass ratio is added into a mixture of fatty acid ethyl ester rich in EPA and DHA and lipase while stirring in a dropwise adding mode within two minutes after the mixture is heated to 60 ℃;
fourthly, the reaction lasts for 24 hours in a dark state, then the mixture is centrifuged to stop the reaction, and oil phase products are separated to prepare the triglyceride type fish oil rich in EPA and DHA.
In the method for preparing the structured lipid rich in EPA and DHA by using tuna, the lipase is LRI, the amount of the lipase is 20% by mass of the total mass of the reaction substrate, the part of the fatty acid ethyl ester rich in EPA and DHA is 3 parts, and the pure water amount is 0.75% by mass of the total mass of the reaction substrate.
In the method for preparing the EPA and DHA-rich structural lipid by using the tuna, the EPA and DHA-rich fatty acid ethyl ester is converted into the EPA and DHA-rich fatty acid ethyl ester through an enrichment process by using commercially available EPA and DHA-containing fatty acid ethyl ester.
In the method for preparing EPA and DHA-rich structural lipid by using tuna, the enrichment process comprises the following steps: stirring 3 parts of urea and 6 parts of ethanol according to the mass ratio for 30 minutes at 65 ℃ and the rotating speed of 800 revolutions per minute, adding 2 parts of commercially available fatty acid ethyl ester containing EPA and DHA, continuously stirring for 30 minutes, crystallizing at the temperature of-5 ℃ for 10 hours, then obtaining a solid phase and filtrate through first vacuum filtration, cleaning the solid phase for 2-3 times through ethanol, carrying out second vacuum filtration, mixing the obtained filtrate with the first vacuum filtration filtrate, then carrying out rotation at 45 ℃ to remove ethanol, washing and separating liquid, collecting an oil phase to obtain a separated product, and carrying out liquid-liquid extraction on the solid phase to obtain the fatty acid ethyl ester rich in EPA and DHA.
In the aforementioned method for preparing structural lipid rich in EPA and DHA from tuna, the transesterification process in S4 comprises: firstly, acidifying the fatty acid ethyl ester rich in EPA and DHA to prepare free fatty acid rich in EPA and DHA, and then carrying out ester exchange on the free fatty acid rich in EPA and DHA and the phospholipid fish oil to prepare the phospholipid fish oil rich in EPA and DHA.
In the method for preparing EPA and DHA-rich structural lipid by using tuna, the process for preparing EPA and DHA-rich phospholipid fish oil by transesterification comprises the following steps:
weighing 1 part of phospholipid fish oil in a mass ratio, putting the phospholipid fish oil into a reaction container, adding 1-5 parts of free fatty acid rich in EPA and DHA and 0.25-1.25% of pure water in terms of the total mass of a reaction substrate, and adding an extracting agent n-hexane;
secondly, continuously adding 5-25% of lipase by the total mass of the reaction substrate into the reaction container, then filling a nitrogen cover and sealing with a sealing film, and placing the mixture in a constant-temperature gas bath shaking table, wherein the set temperature is 60 ℃ and the rotating speed is 200 r/min;
thirdly, the reaction lasts for 24 hours in a dark state, then the mixture is centrifuged to stop the reaction, and oil phase products are separated to obtain the phospholipid type fish oil rich in EPA and DHA.
The method for preparing EPA and DHA-rich structural lipid by using tuna is characterized in that the acidification process of EPA and DHA-rich fatty acid ethyl ester comprises the following steps: adding 1 part of fatty acid ethyl ester rich in EPA and DHA in mass ratio into a reaction container, and adding 4 parts of NaOH-CH 3 Uniformly mixing OH solution, heating in water bath at 80 ℃, condensing, refluxing and continuously saponifying for 2 hours, stopping heating, cooling the mixture to room temperature, adding 2 parts of normal hexane, continuously adding 2 parts of pure water, and uniformly mixingStanding and layering, collecting a lower layer, continuously adding n-hexane for repeated extraction twice, dripping concentrated sulfuric acid into the collected water phase of the lower layer to adjust the pH value to 1-2, moving out an upper layer after layering, adding a saturated NaCl solution into the upper layer for washing until clarification, adding anhydrous sodium sulfate into the separated upper layer solution to remove residual moisture, and then removing the residual n-hexane by nitrogen blowing, thus obtaining the free fatty acid rich in EPA and DHA.
The method for preparing the EPA and DHA-rich structural lipid by using the tuna is characterized in that the part of the EPA and DHA-rich free fatty acid is 4 parts, and the pure water accounts for 0.75 percent of the total mass of the reaction substrate.
The method for preparing the structural lipid rich in EPA and DHA by using tuna is characterized in that the lipase is PLA1, and the amount of the lipase is 15% of the total mass of a reaction substrate.
Compared with the prior art, the invention has the following advantages:
1. the phospholipid type fish oil and the triglyceride type fish oil are prepared from the viscera of the tuna, so that the phospholipid type fish oil and the triglyceride type fish oil are more beneficial to human body absorption and have lower cost.
2. According to the invention, commercially available fatty acid ethyl ester containing EPA and DHA is used for enrichment and is subjected to ester exchange with phospholipid type fish oil and triglyceride type fish oil to prepare triglyceride type fish oil rich in EPA and DHA and phospholipid type fish oil rich in EPA and DHA, the content of triglyceride type EPA and DHA in the triglyceride type fish oil rich in EPA and DHA can reach more than 70%, the total content of phospholipid type EPA and DHA in the phospholipid type fish oil rich in EPA and DHA reaches 186.39mg/g, and the nutritional value is high.
Drawings
FIG. 1 is a line graph of an experiment for optimizing the amount of a solvent in an enrichment process in example 1 of the present invention;
FIG. 2 is a line graph of the experimental optimization of the urea-to-ester ratio in the enrichment process in example 1 of the present invention;
FIG. 3 is a line graph of an optimization experiment of crystallization temperature in the enrichment process in example 1 of the present invention;
FIG. 4 is a bar graph showing the effect of water content on the transesterification of triglyceride-type fish oil and EPA-and DHA-rich fatty acid ethyl esters in Experimental example 2 of the present invention;
FIG. 5 is a bar graph of substrate mass ratio versus triglyceride-type fish oil and EPA and DHA-rich fatty acid ethyl ester transesterification effect experiment in Experimental example 2 of the present invention;
FIG. 6 is a bar graph showing the effect of the addition of lipase in Experimental example 2 on the transesterification of triglyceride-type fish oil and fatty acid ethyl esters rich in EPA and DHA;
FIG. 7 is a bar graph showing the effect of water content on the transesterification of phospholipid-type fish oil and EPA-and DHA-rich fatty acid ethyl esters in Experimental example 3;
FIG. 8 is a bar graph showing the effect of substrate mass ratio on the transesterification of phospholipid-type fish oil and EPA-and DHA-rich fatty acid ethyl esters in Experimental example 3;
FIG. 9 is a bar graph showing the effect of the addition of lipase on the transesterification of phospholipid fish oil with fatty acid ethyl esters rich in EPA and DHA in Experimental example 3 of the present invention.
The applicant carries out a series of experiments, and can confirm that the method provided by the invention is effective and controllable, and can prepare the structural lipid rich in EPA and DHA.
In the experimental example 1, the following examples were conducted,
and (3) optimizing factor experiments on the enrichment conditions of the commercially available EPA and DHA-containing fatty acid ethyl ester.
The experimental method comprises the following steps:
(1) solvent quantity optimization experiment
Fixing the amount of urea 10g, adding ethanol and urea at the weight ratio of 1:1, 2:1, 3:1, 4:1 and 5:1, adding fatty acid ethyl ester containing EPA and DHA at the urea-ester ratio of 1:1, and crystallizing at 0 deg.C for 10h after inclusion. Other operations follow the enrichment process. And finally, weighing the collected EPA and DHA-rich fatty acid ethyl ester, performing gas phase detection and analysis, wherein the result is shown in figure 1, and the experimental data show that the enrichment effect is best when the proportion of ethanol to fatty acid ethyl ester is 3:1 under the condition of considering the factors of resource saving and recovery rate.
(2) Optimization experiment of urine-to-ester ratio
Fixing 10g of EPA and DHA-containing fatty acid ethyl ester, adding 20g of solvent ethanol, respectively adding 5g, 10g, 15g, 20g and 25g of urea according to the mass ratio of 0.5:1, 1:1, 1.5:1, 2:1 and 2.5:1 of urea to EPA and DHA-containing fatty acid ethyl ester, and crystallizing at 0 ℃ for 10 hours after inclusion. Other operations follow the enrichment process. And finally, weighing the collected EPA and DHA-rich fatty acid ethyl ester, detecting and analyzing the fatty acid ethyl ester in a gas phase, wherein the result is shown in figure 2, and the experimental data show that the urine-ester ratio of 1.5:1 is good in enrichment effect under the condition of considering the factors of resource saving and recovery rate.
(3) Crystallization temperature optimization experiment
Weighing 10g of urea, dissolving the urea in 20g of ethanol, adding 10g of fatty acid ethyl ester containing EPA and DHA, crystallizing the included mixture at the temperature of-10 ℃, minus 5 ℃, 0 ℃, 5 ℃ and 10 ℃ for 10 hours according to the operation steps of the enrichment process, and finally weighing the fatty acid ethyl ester rich in EPA and DHA and carrying out gas phase analysis on the product, wherein the result is shown in figure 3, and the experimental data show that the enrichment effect is good when the crystallization temperature is-5 ℃ from the aspects of recovery rate and efficiency.
In the experimental example 2, the following experiments were carried out,
and (3) carrying out factor optimization experiments on triglyceride type fish oil and fatty acid ethyl ester rich in EPA and DHA.
The experimental method comprises the following steps:
(1) water content
The substrate mass ratio of 1:3, the substrate ratio of triglyceride type fish oil to EPA and DHA rich fatty acid ethyl ester, the enzyme addition amount of 10% (based on the total mass of the reaction substrate), and the pure water of 0.5%, 1.0%, 1.5%, 2.0%, 2.5% (based on the total mass of the reaction substrate) were added, respectively, and other operations were performed according to the experimental procedures of the transesterification process in claim 2, and the results are shown in FIG. 4, and the above experimental data show that the optimum water content of N435 is 0.5%, the optimum water content of LRI is 1.5%, and the optimum water content of LTI is 2%.
(2) Mass ratio of substrate
Experiments were carried out with a substrate mass ratio of 1:1, 1:2, 1:3, 1:4, 1:5, respectively, of triglyceride type fish oil to EPA and DHA-rich fatty acid ethyl ester, an added amount of immobilized enzyme of 10%, and a water content of 1.0%, and other operations were carried out according to the experimental procedures of the transesterification process of claim 2, and the results are shown in fig. 5, and the above experimental data show that the optimum substrate mass ratio of N435 is 1:2, and the optimum substrate mass ratio of LRI and LTI is 1: 4.
(3) Adding amount of lipase
The substrate mass ratio of 1:3, the substrate ratio of triglyceride type fish oil to EPA and DHA rich fatty acid ethyl ester, the water content of 1.0%, were fixed, 5%, 10%, 15%, 20%, 25% (based on the total mass of the reaction substrate) of the enzyme was added, and the other operations were performed according to the experimental procedure of the transesterification process in claim 2, and the results are shown in fig. 6, and the above experimental data show that the optimal enzyme addition amounts of N435, LRI and LTI in this experiment were 25%, 20% and 25%, respectively.
In general, the optimal catalysis conditions of the lipase N435 are that the water content is 0.5%, the substrate mass ratio is 1:2, and the enzyme addition amount is 20%, at the moment, the relative content of triglyceride type EPA and DHA in triglyceride type fish oil rich in EPA and DHA in a catalysis product reaches 68.74%; the optimal catalysis condition of the LRI is that the water content is 1.5 percent, the mass ratio of the substrate is 1:4, and the enzyme addition amount is 20 percent, at the moment, the relative content of triglyceride type EPA and DHA in the triglyceride type fish oil rich in EPA and DHA in the product reaches 73.26 percent; the optimal catalysis condition of LTI is that the water content is 2%, the substrate mass ratio is 1:4 and 25% of enzyme addition amount, and the relative content of triglyceride type EPA and DHA in the triglyceride type fish oil rich in EPA and DHA in the product reaches 56.13%, so in the transesterification condition of triglyceride type fish oil and fatty acid ethyl ester rich in EPA and DHA, the optimal catalysis condition of LRI is 1.5% of water content, and the substrate mass ratio is 1:4 and 20% of enzyme addition amount, the transesterification effect is best.
In the experimental example 3, the following experiments were carried out,
and (3) performing factor optimization experiments on phospholipid fish oil and fatty acid ethyl ester rich in EPA and DHA in transesterification conditions.
The experimental method comprises the following steps:
(1) water content
The substrate mass ratio of 1:3, the substrate ratio being the ratio of phospholipid fish oil to free fatty acid rich in EPA and DHA, the enzyme addition amount of 10% (by total mass of reaction substrate), 0.25%, 0.5%, 0.75%, 1.0%, 1.25% pure water (by total mass of reaction substrate) were added, and other operations were performed according to the experimental procedures of the transesterification process in claim 7, and the results are shown in fig. 7, where the above experimental data indicate that the optimum moisture content of N435 is 0.25%, the optimum moisture content of LRI is 1%, and the optimum moisture content of PLA1 is 0.75%.
(2) Mass ratio of substrate
Experiments were carried out with a substrate mass ratio of 1:1, 1:2, 1:3, 1:4, 1:5, respectively, of phospholipid-type fish oil to free fatty acid rich in EPA and DHA, an amount of immobilized enzyme added of 10%, and a water content of 1.0%, and other operations were carried out according to the experimental procedure of the transesterification process of claim 7, and the results are shown in fig. 8, where the above experimental data indicate that the mass ratio of N435 to LRI is 1:5, the mass ratio of LRI to optimal substrate is 1:4, and the mass ratio of PLA1 to optimal substrate is 1: 3.
(3) Adding amount of lipase
The substrate mass ratio of 1:3, the substrate ratio being the ratio of phospholipid fish oil to free fatty acid rich in EPA and DHA, the water content being 1.0%, and 5%, 10%, 15%, 20%, 25% (based on the total mass of the reaction substrate) of the enzymes were added, respectively, and the other operations were performed according to the experimental procedure of the transesterification process in claim 7, and the results are shown in fig. 9, and the above experimental data indicate that the optimal enzyme addition amounts of N435, LRI and PLA1 in this experiment were 20%, 20% and 15%, respectively.
In general, the optimal catalysis conditions of the lipase PLA1 are that the water content is 0.75%, the substrate mass ratio is 1:3, and the enzyme addition amount is 15%, and the total content of phospholipid EPA and DHA in the phospholipid fish oil rich in EPA and DHA in the catalysis product reaches 186.39 mg/g; the optimal catalysis condition of the LRI is that the water content is 1 percent, the substrate mass ratio is 1:4, and the enzyme addition amount is 20 percent, and the total content of phospholipid EPA and DHA in the phospholipid fish oil rich in EPA and DHA in the catalysis product reaches 168.10 mg/g; the optimal catalytic conditions of N435 are water content of 0.25%, substrate mass ratio of 1:5 and enzyme addition amount of 20%, and the total content of phospholipid EPA and DHA in the phospholipid fish oil rich in EPA and DHA in the catalytic product reaches 114.13mg/g, so the optimal reaction conditions are water content of 0.75%, substrate mass ratio of 1:3 and enzyme addition amount of 15%.
Detailed Description
The invention is further illustrated by the following figures and examples, which are not to be construed as limiting the invention.
Example 1. A method for preparing lipid with structure rich in EPA and DHA from tuna comprises sequentially cleaning viscera of tuna, drying, lyophilizing, breaking cell wall to obtain tuna powder, processing the tuna powder by ultrasonic-assisted solvent extraction to obtain crude lipid, purifying the crude lipid by Folch method to remove impurities, adding cold acetone into the crude lipid after impurities removal, precipitating at low temperature, separating supernatant, performing rotary evaporation to obtain triglyceride type fish oil, and blowing off acetone residue for insoluble nitrogen to obtain phospholipid type fish oil.
Taking 4 parts of EPA and DHA-rich fatty acid ethyl ester in mass ratio into a reaction vessel, adding 1.5% of pure water in terms of the total mass of a reaction substrate, adding 20% of LRI lipase in terms of the total mass of the reaction substrate, placing the mixture into a magnetic stirrer for stirring and heating in water bath, setting the rotating speed at 400 r/m, connecting the reaction vessel and a vacuum pump by a leather hose to enable the system to be in a vacuum state of 5Pa, adding 1 part of triglyceride type fish oil in terms of mass ratio dropwise within two minutes after heating to 60 ℃ while stirring, continuing the reaction for 24 hours in a dark state, centrifuging the mixture to terminate the reaction, and separating an oil phase product to obtain the triglyceride type fish oil rich in EPA and DHA.
Weighing 1 part of phospholipid fish oil in mass ratio, putting the phospholipid fish oil into a reaction vessel, adding 3 parts of free fatty acid rich in EPA and DHA and pure water accounting for 0.75% of the total mass of a reaction substrate, adding an extracting agent n-hexane, continuously adding 15% of PLA1 lipase accounting for the total mass of the reaction substrate into the reaction vessel, then filling a nitrogen cover cap, sealing the reaction vessel by using a sealing film, placing the mixture into a constant-temperature gas bath shaking table, setting the temperature to be 60 ℃, setting the rotating speed to be 200 r/min, keeping the reaction for 24h in a light-proof state, then centrifuging the mixture to stop the reaction, and separating an oil phase product to obtain the phospholipid fish oil rich in EPA and DHA.
Claims (10)
1. A method for preparing structural lipid rich in EPA and DHA by using tuna is characterized by comprising the following steps: the method comprises the following steps:
s1, pretreating raw materials, namely sequentially cleaning, drying, freeze-drying and breaking walls of viscera of tuna to obtain tuna powder;
s2, extracting and separating lipid, processing tuna powder by an ultrasonic-assisted solvent extraction method to obtain crude lipid, purifying and removing impurities from the crude lipid by a Folch method, adding cold acetone into the crude lipid after the impurities are removed, carrying out low-temperature sedimentation, separating supernatant liquid, carrying out rotary evaporation to obtain triglyceride type fish oil, and blowing off acetone residues from insoluble nitrogen to obtain phospholipid type fish oil;
s3, carrying out ester exchange on triglyceride type fish oil and fatty acid ethyl ester rich in EPA and DHA to prepare triglyceride type fish oil rich in EPA and DHA;
and S4, performing ester exchange on the phospholipid fish oil and the fatty acid ethyl ester rich in EPA and DHA to prepare the phospholipid fish oil rich in EPA and DHA.
2. The method for preparing structural lipid rich in EPA and DHA from tuna according to claim 1, wherein the transesterification process in S3 includes:
taking 1-5 parts by mass of fatty acid ethyl ester rich in EPA and DHA in a reaction container, and adding 0.5-2.5% of pure water by mass of the total mass of reaction substrates;
adding 5-25% of lipase based on the total mass of the reaction substrate, placing the mixture in a magnetic stirrer for stirring and heating in water bath, setting the rotating speed at 400 r/m, and connecting the reaction container and a vacuum pump by a leather hose to ensure that the system is in a vacuum state of 5Pa in order to avoid fat oxidation degradation in the process;
thirdly, 1 part of triglyceride type fish oil in mass ratio is added into a mixture of fatty acid ethyl ester rich in EPA and DHA and lipase while stirring in a dropwise adding mode within two minutes after the mixture is heated to 60 ℃;
fourthly, the reaction lasts for 24 hours in a dark state, then the mixture is centrifuged to stop the reaction, and oil phase products are separated to obtain the triglyceride type fish oil rich in EPA and DHA.
3. The method for preparing EPA and DHA-rich structural lipid from tuna according to claim 2, wherein the lipase is LRI, the amount of the lipase is 20% by mass of the total reaction substrate, the part of the EPA and DHA-rich fatty acid ethyl ester is 3 parts, and the pure water amount is 0.75% by mass of the total reaction substrate.
4. The method for preparing EPA and DHA-rich structural lipids according to claim 1, wherein the EPA and DHA-rich fatty acid ethyl ester is obtained by converting commercially available EPA and DHA-containing fatty acid ethyl ester into EPA and DHA-rich fatty acid ethyl ester through an enrichment process.
5. The method for preparing structural lipids rich in EPA and DHA according to claim 4, wherein the enrichment process comprises the following steps: stirring 3 parts of urea and 6 parts of ethanol in a mass ratio for 30 minutes at 65 ℃ and at the rotating speed of 800 rpm, adding 2 parts of commercially available EPA and DHA-containing fatty acid ethyl ester, continuously stirring for 30 minutes, crystallizing at the temperature of-5 ℃ for 10 hours at low temperature, then obtaining a solid phase and a filtrate through first vacuum filtration, cleaning the solid phase for 2-3 times through ethanol, carrying out second vacuum filtration, mixing the obtained filtrate with the first vacuum filtration filtrate, then carrying out rotation at 45 ℃ to remove ethanol, washing the liquid, collecting an oil phase to obtain a separated product, and carrying out liquid-liquid extraction on the solid phase to obtain the fatty acid ethyl ester rich in EPA and DHA.
6. The method for preparing structural lipid rich in EPA and DHA from tuna according to claim 1, wherein the transesterification process in S4 includes: firstly, acidifying the fatty acid ethyl ester rich in EPA and DHA to prepare free fatty acid rich in EPA and DHA, and then carrying out ester exchange on the free fatty acid rich in EPA and DHA and the phospholipid fish oil to prepare the phospholipid fish oil rich in EPA and DHA.
7. The method for preparing EPA and DHA-enriched structural lipids by tuna according to claim 6, wherein the transesterification process for preparing EPA and DHA-enriched phospholipid-type fish oil comprises:
weighing 1 part of phospholipid fish oil in a mass ratio, putting the phospholipid fish oil into a reaction container, adding 1-5 parts of free fatty acid rich in EPA and DHA and 0.25-1.25% of pure water in terms of the total mass of a reaction substrate, and adding an extracting agent n-hexane;
secondly, continuously adding 5-25% of lipase by the total mass of the reaction substrate into the reaction container, then filling a nitrogen cover and sealing with a sealing film, and placing the mixture in a constant-temperature gas bath shaking table, wherein the set temperature is 60 ℃ and the rotating speed is 200 r/min;
thirdly, the reaction lasts for 24 hours in a dark state, then the mixture is centrifuged to stop the reaction, and oil phase products are separated to obtain the phospholipid type fish oil rich in EPA and DHA.
8. The method for preparing EPA and DHA enriched structural lipids according to claim 6, wherein the structural lipids are extracted from tuna: the acidification process of the EPA and DHA-rich fatty acid ethyl ester comprises the following steps: adding 1 part of fatty acid ethyl ester rich in EPA and DHA in mass ratio into a reaction container, and adding 4 parts of NaOH-CH 3 And (2) uniformly mixing the OH solution, heating in a water bath at 80 ℃ and continuously saponifying by condensation reflux for 2 hours, stopping heating, cooling the mixture to room temperature, adding 2 parts of n-hexane, continuously adding 2 parts of pure water, standing for layering after uniform mixing, collecting the lower layer, continuously adding n-hexane for repeated extraction twice, dropwise adding concentrated sulfuric acid into the collected water phase of the lower layer to adjust the pH value to 1-2, removing the upper layer after layering, adding a saturated NaCl solution into the upper layer for washing until clarification, adding anhydrous sodium sulfate into the separated upper layer solution to remove residual moisture, and blowing off the residual n-hexane by nitrogen to obtain the free fatty acid rich in EPA and DHA.
9. The method for preparing EPA and DHA enriched structural lipids from tuna according to claim 7, wherein: the parts of the free fatty acid rich in EPA and DHA are 4 parts, and the pure water amount is 0.75 percent based on the total mass of the reaction substrate.
10. The method for preparing EPA and DHA enriched structural lipids according to claim 6, wherein the structural lipids are extracted from tuna: the lipase is PLA1, and the amount of the lipase is 15% of the total mass of the reaction substrate.
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