Preparation method of ARA nano-emulsion

By using sodium casein and gum arabic composite powder as an emulsifier, ARA nanoemulsion was prepared, which solved the problem of ARA oil being prone to oxidation and deterioration, and achieved the improvement of ARA oil's stability and biological activity.

CN119769727APending Publication Date: 2025-04-08WUHAN POLYTECHNIC UNIVERSITY +1
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Patent Information

Application Number
CN202411837103.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-13
Publication Date
2025-04-08

AI Technical Summary

Technical Problem

ARA oil is susceptible to oxidation and deterioration due to factors such as light, air, metal ions, etc., resulting in a decline in its physiological activity and sensory quality, and lacks ARA products with good stability.

Method used

The composite powder composed of sodium casein and gum arabic is used as an emulsifier to prepare the composite powder through the Maillard reaction, and then mixed with deionized water to form a solution, ARA oil is added and subjected to high-speed shearing and homogenization to prepare an ARA nanoemulsion.

Benefits of technology

The conversion of ARA oil into nanoemulsion through embedding technology greatly masks the flavor of ARA oil, enhances its water solubility and fluidity, improves stability, and improves physical and chemical properties and in vitro digestive properties.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a preparation method of an ARA (arachidonic acid) nano-emulsion, which comprises the following steps: dissolving sodium casein and polysaccharide powder in ultrapure water together, stirring and mixing, and freeze-drying to obtain a freeze-dried substance; grinding and sieving the freeze-dried substance, spreading the freeze-dried substance in a culture dish, and placing the culture dish in a dryer filled with a saturated KBr solution for a Maillard reaction to obtain composite powder composed of sodium casein and Arabic gum; mixing the composite powder with water to prepare a solution, stirring, centrifuging, and taking supernate; aRA oil is added into the supernate, a coarse emulsion is obtained through high-speed shearing, the shearing rotating speed of high-speed shearing is 10000-15000 r / min, and the shearing time is 3-6 min; and carrying out homogenization treatment on the crude emulsion to prepare the ARA nano-emulsion. According to the preparation method disclosed by the invention, the ARA is embedded by the sodium casein and Arabic gum composite emulsifier to prepare the nano-emulsion, so that the original flavor of the ARA oil can be greatly covered, the water solubility and the flowability of the ARA oil are enhanced, and the stability is improved.
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Description

Technical Field

[0001] The invention relates to the technical field of food processing, and in particular to a method for preparing an ARA nanoemulsion. Background Art

[0002] ARA (cis-5,8,11,14-eicosatetraenoic acid, ARA), whose chemical name is all-cis Δ-5,8,11,14-eicosatetraenoic acid, is one of the essential polyunsaturated fatty acids for the human body. ARA is extremely important for the brain and retinal photoreceptors. ARA deficiency can lead to irreversible damage to intelligence and visual function. ARA participates in the transmission of nerve signals in the brain and has a significant effect on the function of nerve cells. At the same time, ARA can also promote growth and development, regulate endocrine, and has biological activities such as lowering blood sugar and blood lipids. It also participates in biological processes such as vasodilation and immune regulation, and is very important to human health.

[0003] ARA oil is one of the important sources of high-purity ARA. It is easily affected by factors such as light, air, and metal ions, and oxidized and deteriorated, producing metabolites that are harmful to the human body, which seriously reduces the physiological activity and sensory quality of ARA oil. Therefore, how to provide an ARA product with good stability is an urgent problem to be solved. Summary of the invention

[0004] The main purpose of the present invention is to provide a method for preparing an ARA nanoemulsion, aiming to solve the problem of how to provide an ARA product with good stability.

[0005] To achieve the above object, the present invention provides a method for preparing an ARA nanoemulsion, which comprises the following steps:

[0006] Dissolving casein sodium and polysaccharide powder in ultrapure water, stirring and mixing, and then freeze-drying to obtain a freeze-dried product;

[0007] The freeze-dried product is ground and sieved, and then spread in a culture dish, and placed in a desiccator with a saturated KBr solution at the bottom for Maillard reaction to obtain a composite powder consisting of sodium casein and gum arabic;

[0008] The composite powder is mixed with deionized water to form a solution, stirred, and centrifuged to obtain a supernatant;

[0009] ARA oil is added to the supernatant to obtain a crude emulsion through high-speed shearing, wherein the shearing speed of the high-speed shearing is 10000-15000 r / min and the shearing time is 3-6 min;

[0010] The crude emulsion is homogenized to obtain the ARA nanoemulsion.

[0011] Optionally, in the step of dissolving casein sodium and polysaccharide powder together in ultrapure water, stirring and mixing, and then freeze-drying to obtain a freeze-dried product:

[0012] The polysaccharide powder includes at least one of gum arabic, chitosan, dextran and maltodextrin.

[0013] Optionally, in the step of dissolving casein sodium and polysaccharide powder together in ultrapure water, stirring and mixing, and then freeze-drying to obtain a freeze-dried product:

[0014] The mass ratio of the casein sodium to the polysaccharide powder is 1:2.

[0015] Optionally, the freeze-dried product is ground and sieved, then spread in a culture dish, and placed in a desiccator with a saturated KBr solution at the bottom for Maillard reaction to obtain a composite powder of sodium casein and gum arabic:

[0016] The mesh number of the sieving is 100 meshes;

[0017] Optionally, the freeze-dried product is ground and sieved, then spread in a culture dish, and placed in a desiccator with a saturated KBr solution at the bottom for Maillard reaction to obtain a composite powder of sodium casein and gum arabic:

[0018] The reaction temperature of the Maillard reaction is 60° C. and the reaction time is 96 h.

[0019] Optionally, in the step of mixing the composite powder with deionized water to form a solution, stirring and centrifuging to obtain a supernatant:

[0020] The mass of the composite powder added per liter of deionized water is 2.5 to 12.5 g.

[0021] Optionally, in the step of mixing the composite powder with deionized water to form a solution, stirring and centrifuging to obtain a supernatant:

[0022] The stirring includes magnetic stirring, and the stirring speed of the magnetic stirring is 1000-3000 r / min and the stirring time is 2-2.5 h.

[0023] Optionally, in the step of adding ARA oil to the supernatant to obtain a crude emulsion by high-speed shearing:

[0024] The mass of the ARA oil added to each liter of the supernatant is 2.5 to 12.5 g.

[0025] Optionally, in the step of homogenizing the crude emulsion to obtain the ARA nanoemulsion:

[0026] The homogenization pressure of the homogenization treatment is 50 to 80 MPa, and the number of homogenization times is 3 to 7 times.

[0027] In the technical solution provided by the present invention, a composite powder composed of sodium casein and gum arabic is used as an emulsifier, deionized water is first added to form a solution, and then ARA oil is added to form a crude emulsion, and finally the ARA nanoemulsion is obtained by homogenization. ARA is embedded in the composite emulsifier of sodium casein and gum arabic to form a nanoemulsion, so that the original flavor of the ARA oil can be greatly concealed, the water solubility and fluidity of the ARA oil are enhanced, the stability is improved, and the physical and chemical properties and in vitro digestion properties of the ARA oil are improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other related drawings can be obtained based on these drawings without paying creative work.

[0029] Figure 1 The present invention provides a schematic flow chart of an embodiment of a method for preparing an ARA nanoemulsion.

[0030] The realization of the purpose, functional features and advantages of the present invention will be further explained in conjunction with embodiments and with reference to the accompanying drawings. DETAILED DESCRIPTION

[0031] To make the purpose, technical scheme and advantages of the embodiment of the present invention clearer, the technical scheme in the embodiment of the present invention will be described clearly and completely below. If the specific conditions are not specified in the embodiment, it is carried out according to the normal conditions or the conditions recommended by the manufacturer. If the reagents or instruments used do not specify the manufacturer, they are all conventional products that can be purchased commercially. In addition, the meaning of "and / or" appearing in the full text includes three parallel schemes, taking "A and / or B" as an example, including scheme A, or scheme B, or schemes that A and B meet at the same time. In addition, the technical schemes between the various embodiments can be combined with each other, but must be based on the ability of ordinary technicians in the field to achieve. When the combination of technical solutions is contradictory or cannot be achieved, it should be considered that the combination of such technical solutions does not exist, and is not within the scope of protection required by the present invention. Based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in the field without making creative work belong to the scope of protection of the present invention.

[0032] ARA oil is one of the important sources of high-purity ARA. It is easily affected by light, air, metal ions and other factors, causing oxidation and deterioration, producing metabolites that are harmful to the human body, and seriously reducing the physiological activity and sensory quality of ARA oil.

[0033] At present, in order to solve this problem, ARA oil can be protected from environmental conditions by embedding technology. Emulsion has been studied as a simple, efficient and low-cost embedding method. Making ARA oil into an emulsion by embedding technology can shield its own bad taste to a certain extent, change its morphology, enhance the water solubility and fluidity of ARA oil, improve its stability, make it easy to store, transport and use, and extend the shelf life of the product. However, there is a lack of research on the preparation process of ARA nanoemulsion in the prior art.

[0034] In order to solve the problem of how to provide an ARA nanoemulsion with good stability, the present invention provides a method for preparing an ARA nanoemulsion, wherein a composite emulsifier composed of casein sodium and gum arabic is prepared. Figure 1 FIG. 1 is an example of a method for preparing the ARA nanoemulsion provided by the present invention. Figure 1 As shown, in this embodiment, the preparation method of the ARA nanoemulsion comprises the following steps:

[0035] Step S10, dissolving casein sodium and polysaccharide powder together in ultrapure water, stirring and mixing, and then freeze-drying to obtain a freeze-dried product;

[0036] Step S20, grinding and sieving the lyophilized material, spreading it in a culture dish, and placing it in a dryer with a saturated KBr solution at the bottom to perform Maillard reaction to obtain a composite powder consisting of sodium casein and gum arabic;

[0037] Step S30, mixing the composite powder with deionized water to form a solution, stirring and centrifuging to obtain a supernatant;

[0038] Step S40, adding ARA oil to the supernatant, and obtaining a crude emulsion by high-speed shearing, wherein the shearing speed of the high-speed shearing is 10000-15000 r / min and the shearing time is 3-6 min;

[0039] Step S50, homogenizing the crude emulsion to obtain an ARA nanoemulsion.

[0040] In the technical solution provided by the present invention, a composite powder composed of sodium casein and gum arabic is used as an emulsifier, deionized water is first added to form a solution, and then ARA oil is added to form a crude emulsion, and finally the ARA nanoemulsion is obtained by homogenization. ARA is embedded in the composite emulsifier of sodium casein and gum arabic to form a nanoemulsion, so that the original flavor of the ARA oil can be greatly concealed, the water solubility and fluidity of the ARA oil are enhanced, the stability is improved, and the physical and chemical properties and in vitro digestion properties of the ARA oil are improved.

[0041] In some embodiments of the present invention, the high-speed shearing in step S30 can be achieved by means of a high-speed shearing machine, and its shearing speed can be, for example, 10000r / min, 11000r / min, 12000r / min, 13000r / min, 14000r / min, 15000r / min, etc., preferably 12000r / min; its shearing time can be, for example, 3min, 4min, 5min, 6min, etc., preferably 3min. High-speed shearing for 3min at a speed of 12000r / min can fully mix the ARA oil and the emulsifier solution to form the crude emulsion, with high efficiency and good mixing effect.

[0042] In some embodiments of the present invention, the polysaccharide powder in step S10 includes at least one of gum arabic, chitosan, dextran and maltodextrin, and can be any one of the above substances, or a mixture of any two or more thereof. By selecting the above polysaccharide powder, the emulsification effect of the composite powder composed of sodium casein and gum arabic is better. Further, in some preferred embodiments of the present invention, the polysaccharide powder includes any one of gum arabic, chitosan, dextran and maltodextrin, and is more preferably gum arabic.

[0043] In some embodiments of the present invention, in step S10, the mass ratio of the sodium casein to the polysaccharide powder is 1:2. Under this ratio, the obtained composite powder composed of sodium casein and gum arabic has better emulsification performance.

[0044] In some embodiments of the present invention, in step S20, the mesh number of the sieving is 100 meshes, so that a freeze-dried product with a smaller particle size can be obtained, so that the contact area between the freeze-dried product and the KBr solution is larger, which is conducive to the Maillard reaction.

[0045] In some embodiments of the present invention, in step S20, the reaction temperature of the Maillard reaction is 60° C. and the reaction time is 96 h. Under the above conditions, the obtained composite powder composed of sodium casein and gum arabic has the best emulsification performance.

[0046] The amount of emulsifier added affects the strength of the interfacial film formed on the surface of the dispersed phase droplet. In a preferred embodiment of the present invention, in step S30, the mass of the composite powder added per liter of deionized water is 2.5 to 12.5 g, that is, the amount of the composite powder added is 2.5 to 12.5 g / L. By controlling the amount of the composite powder added as an emulsifier within the above range, the strength of the interfacial film formed on the surface of the dispersed phase droplet is high.

[0047] In some embodiments of the present invention, in step S30, the stirring includes magnetic stirring, and the stirring speed of the magnetic stirring is 1000-3000 r / min, and the stirring time is 2-2.5 h. Under the above stirring conditions, the mixing effect is good. Specifically, the stirring speed in step S30 can be, for example, 1000 r / min, 1100 r / min, 1200 r / min, 1300 r / min, 1400 r / min, 1500 r / min, 1800 r / min, 2000 r / min, 2500 r / min, 2600 r / min, 2700 r / min, 2800 r / min, 2900 r / min or 3000 r / min; the stirring time can be, for example, 2 h, 2.1 h, 2.2 h, 2.3 h or 2.5 h.

[0048] The particle size and turbidity of the emulsion increase with the increase of the amount of oil phase added. When the amount of emulsifier added is fixed and the amount of ARA oil added is too small, part of the emulsifier cannot form an emulsion to embed the ARA oil; when the amount of emulsifier added is fixed and the ARA oil is excessive, part of the ARA oil cannot be emulsified and wrapped by the emulsifier, the volume of the emulsified oil droplets increases and the contact area with the water phase becomes smaller, and the oil droplets are prone to collision and aggregation, resulting in a decrease in the stability of the nanoemulsion. In a preferred embodiment of the present invention, in step S40, the mass of the ARA oil added to each liter of the supernatant is 2.5 to 12.5 g, that is, the amount of ARA oil added is 2.5 to 12.5 g / L. When the amount of ARA oil added is within the above range, the potential of the ARA nanoemulsion finally obtained is larger and the particle size is smaller.

[0049] In some embodiments of the present invention, the mass of the ARA oil added to each liter of the supernatant can be 2.5g, 3g, 4g, 5g, 10g, 11g or 12.5g. Preferably, the mass of the ARA oil added to each liter of the supernatant is 5g, so that the potential of the ARA nanoemulsion finally obtained has the largest absolute value and the smallest particle size.

[0050] As the number of homogenization times increases, the particle size and dispersion coefficient of the emulsion tend to decrease first and then gradually stabilize, while the potential of the emulsion tends to decrease first and then increase. Therefore, in a preferred embodiment of the present invention, in step S50, the number of homogenization times of the homogenization process is 3 to 7 times.

[0051] In some embodiments of the present invention, in step S50, the homogenization number of the homogenization treatment can be 3 times, 4 times, 5 times, 6 times or 7 times. Preferably, the homogenization number is 5 times, at which the potential of the prepared ARA nanoemulsion has the largest absolute value, and the potential gradually decreases as the homogenization number continues to increase. This may be because as the homogenization number increases, mechanical energy is converted into heat energy, which is absorbed by the emulsion to undergo a phase transition, thereby changing the emulsion stability, destroying the nanoemulsion structure in the system, and reducing the stability of the newly formed nanoparticles.

[0052] In some embodiments of the present invention, in step S50, the homogenization pressure of the homogenization treatment is 50-80 MPa, specifically, for example, it can be 50 MPa, 60 MPa, 65 MPa, 70 MPa, 75 MPa or 80 MPa, preferably 50 MPa. Under the homogenization pressure of 50 MPa, the stability of the obtained ARA nanoemulsion is better.

[0053] The technical solution of the present invention is further described in detail below in conjunction with specific embodiments and drawings. It should be understood that the following embodiments are only used to explain the present invention and are not used to limit the present invention.

[0054] In the following examples, the raw materials involved include the following:

[0055] Gum Arabic, specification: BR, >90%; manufacturer: Shanghai Yuanye;

[0056] Chitosan, specification: BR, >90%; manufacturer: McLean;

[0057] Glucan, specification: BR, >90%; manufacturer: Shanghai Yuanye;

[0058] Maltodextrin, specification: BR, >90%; manufacturer: Shanghai Yuanye;

[0059] Sodium casein, specification: BR, >90%; manufacturer: Shanghai Yuanye;

[0060] ARA oil, refined oil, produced by Hubei Fuxing Biotechnology Co., Ltd.

[0061] Example 1

[0062] S10, dissolving sodium casein and gum arabic together in ultrapure water, wherein the mass ratio of the sodium casein to the polysaccharide powder is 1:2, stirring and mixing, and then freeze-drying to obtain a freeze-dried product.

[0063] S20, grinding the lyophilized material obtained in step S10 through a 100-mesh sieve and spreading it on a culture dish, placing it in a dryer with a saturated KBr solution at the bottom for Maillard reaction to obtain a composite powder consisting of sodium casein and gum arabic, wherein the reaction temperature of the Maillard reaction is 60° C. and the reaction time is 96 h.

[0064] S30, using the sodium casein-arabic gum composite powder obtained in step S20 as an emulsifier, adding deionized water to prepare a solution, wherein the amount of the emulsifier added is 5 g / L (that is, the mass of the composite powder added per liter of deionized water is 5 g); stirring the solution with a magnetic stirrer, centrifuging and taking the supernatant, wherein the stirring speed of the magnetic stirrer is 2500 r / min, and the stirring time is 2 h.

[0065] S40, adding ARA oil to the supernatant obtained in step S30, and forming a crude emulsion by a high-speed shearing machine, wherein the amount of ARA oil added is 5 g / L (i.e., the mass of the ARA oil added per liter of the supernatant is 5 g), the speed of the high-speed shearing machine is 12000 r / min, and the shearing time is 3 min.

[0066] S50, using a high-pressure homogenizer to process the crude emulsion obtained in step S40 to obtain a finished ARA nanoemulsion, the pressure of the high-pressure homogenizer is 50 MPa, and the high-pressure homogenization times are 5 times.

[0067] Example 2

[0068] S10, dissolving sodium casein and gum arabic together in ultrapure water, wherein the mass ratio of the sodium casein to the polysaccharide powder is 1:2, stirring and mixing, and then freeze-drying to obtain a freeze-dried product.

[0069] S20, grinding the lyophilized material obtained in step S10 through a 100-mesh sieve and spreading it on a culture dish, placing it in a dryer with a saturated KBr solution at the bottom for Maillard reaction to obtain a composite powder consisting of sodium casein and gum arabic, wherein the reaction temperature of the Maillard reaction is 60° C. and the reaction time is 96 h.

[0070] S30, using the sodium casein-arabic gum complex powder obtained in step S20 as an emulsifier, adding deionized water to form a solution, wherein the amount of the emulsifier added is 5 g / L; stirring the solution with a magnetic stirrer and centrifuging to obtain a supernatant, wherein the stirring speed of the magnetic stirrer is 2000 r / min, and the stirring time is 2 h.

[0071] S40, adding ARA oil to the supernatant obtained in step S30, and forming a crude emulsion by a high-speed shearing machine, wherein the amount of ARA oil added is 5 g / L, the speed of the high-speed shearing machine is 12000 r / min, and the shearing time is 3 min.

[0072] S50, using a high-pressure homogenizer to process the crude emulsion obtained in step S40 to obtain a finished ARA nanoemulsion, the pressure of the high-pressure homogenizer is 50 MPa, and the high-pressure homogenization times are 5 times.

[0073] Example 3

[0074] S10-20, prepare sodium casein-gum arabic complex powder according to the method described in steps S10-S20 in Example 1.

[0075] S30. Using the prepared sodium casein-arabic gum complex powder as an emulsifier, adding deionized water to form a solution, wherein the amount of the emulsifier added is 2.5 g / L; stirring the solution with a magnetic stirrer and centrifuging to obtain a supernatant, wherein the stirring speed of the magnetic stirrer is 3000 r / min, and the stirring time is 2 h.

[0076] S40, adding ARA oil to the supernatant obtained in step S30, and forming a crude emulsion by a high-speed shearing machine, wherein the amount of ARA oil added is 2.5 g / L, the speed of the high-speed shearing machine is 12000 r / min, and the shearing time is 3 min.

[0077] S50, using a high-pressure homogenizer to process the crude emulsion obtained in step S40 to obtain a finished ARA nanoemulsion, the pressure of the high-pressure homogenizer is 50 MPa, and the high-pressure homogenization times are 5 times.

[0078] Example 4

[0079] S10-20, prepare sodium casein-gum arabic complex powder according to the method described in steps S10-S20 in Example 1.

[0080] S30. Using the prepared sodium casein-arabic gum complex powder as an emulsifier, adding deionized water to form a solution, wherein the amount of the emulsifier added is 7.5 g / L; stirring the solution with a magnetic stirrer and centrifuging to obtain a supernatant, wherein the stirring speed of the magnetic stirrer is 2500 r / min, and the stirring time is 2 h.

[0081] S40, adding ARA oil to the supernatant obtained in step S30, and forming a crude emulsion by a high-speed shearing machine, wherein the amount of ARA oil added is 2.5 g / L, the speed of the high-speed shearing machine is 12000 r / min, and the shearing time is 3 min.

[0082] S50, using a high-pressure homogenizer to process the crude emulsion obtained in step S40 to obtain a finished ARA nanoemulsion, the pressure of the high-pressure homogenizer is 50 MPa, and the high-pressure homogenization times are 5 times.

[0083] Example 5

[0084] S10-20, prepare sodium casein-gum arabic complex powder according to the method described in steps S10-S20 in Example 1.

[0085] S30. Using the prepared sodium casein-arabic gum complex powder as an emulsifier, adding deionized water to form a solution, wherein the amount of the emulsifier added is 2.5 g / L; stirring the solution with a magnetic stirrer and centrifuging to obtain a supernatant, wherein the stirring speed of the magnetic stirrer is 2500 r / min, and the stirring time is 2 h.

[0086] S40, adding ARA oil to the supernatant obtained in step S30, and forming a crude emulsion by a high-speed shearing machine, wherein the amount of ARA oil added is 7.5 g / L, the speed of the high-speed shearing machine is 12000 r / min, and the shearing time is 3 min.

[0087] S50, using a high-pressure homogenizer to process the crude emulsion obtained in step S40 to obtain a finished ARA nanoemulsion, the pressure of the high-pressure homogenizer is 50 MPa, and the high-pressure homogenization times are 5 times.

[0088] Example 6

[0089] S10-20, prepare sodium casein-gum arabic complex powder according to the method described in steps S10-S20 in Example 1.

[0090] S30. Using the prepared sodium casein-arabic gum complex powder as an emulsifier, adding deionized water to form a solution, wherein the amount of the emulsifier added is 7.5 g / L; stirring the solution with a magnetic stirrer and centrifuging to obtain a supernatant, wherein the stirring speed of the magnetic stirrer is 2500 r / min, and the stirring time is 2 h.

[0091] S40, adding ARA oil to the supernatant obtained in step S30, and forming a crude emulsion by a high-speed shearing machine, wherein the amount of ARA oil added is 7.5 g / L, the speed of the high-speed shearing machine is 12000 r / min, and the shearing time is 3 min.

[0092] S50, using a high-pressure homogenizer to process the crude emulsion obtained in step S40 to obtain a finished ARA nanoemulsion, the pressure of the high-pressure homogenizer is 50 MPa, and the high-pressure homogenization times are 5 times.

[0093] Example 7

[0094] S10-20, prepare sodium casein-gum arabic complex powder according to the method described in steps S10-S20 in Example 1.

[0095] S30. Using the prepared sodium casein-arabic gum complex powder as an emulsifier, adding deionized water to form a solution, wherein the amount of the emulsifier added is 2.5 g / L; stirring the solution with a magnetic stirrer and centrifuging to obtain a supernatant, wherein the stirring speed of the magnetic stirrer is 2500 r / min, and the stirring time is 2 h.

[0096] S40, adding ARA oil to the supernatant obtained in step S30, and forming a crude emulsion by a high-speed shearing machine, wherein the amount of ARA oil added is 5 g / L, the speed of the high-speed shearing machine is 12000 r / min, and the shearing time is 3 min.

[0097] S50, using a high-pressure homogenizer to process the crude emulsion obtained in step S40 to obtain a finished ARA nanoemulsion, the pressure of the high-pressure homogenizer is 50 MPa, and the high-pressure homogenization times are 4 times.

[0098] Example 8

[0099] S10-20, prepare sodium casein-gum arabic complex powder according to the method described in steps S10-S20 in Example 1.

[0100] S30. Using the prepared sodium casein-arabic gum complex powder as an emulsifier, adding deionized water to form a solution, wherein the amount of the emulsifier added is 7.5 g / L; stirring the solution with a magnetic stirrer and centrifuging to obtain a supernatant, wherein the stirring speed of the magnetic stirrer is 2500 r / min, and the stirring time is 2 h.

[0101] S40, adding ARA oil to the supernatant obtained in step S30, and forming a crude emulsion by a high-speed shearing machine, wherein the amount of ARA oil added is 5 g / L, the speed of the high-speed shearing machine is 12000 r / min, and the shearing time is 3 min.

[0102] S50, using a high-pressure homogenizer to process the crude emulsion obtained in step S40 to obtain a finished ARA nanoemulsion, the pressure of the high-pressure homogenizer is 50 MPa, and the high-pressure homogenization times are 4 times.

[0103] Example 9

[0104] S10-20, prepare sodium casein-gum arabic complex powder according to the method described in steps S10-S20 in Example 1.

[0105] S30. Using the pre-prepared sodium casein-arabic gum complex powder as an emulsifier, adding deionized water to form a solution, wherein the amount of the emulsifier added is 2.5 g / L; stirring the solution with a magnetic stirrer and centrifuging to obtain a supernatant, wherein the stirring speed of the magnetic stirrer is 2500 r / min, and the stirring time is 2 h.

[0106] S40, adding ARA oil to the supernatant obtained in step S30, and forming a crude emulsion by a high-speed shearing machine, wherein the amount of ARA oil added is 5 g / L, the speed of the high-speed shearing machine is 12000 r / min, and the shearing time is 3 min.

[0107] S50, using a high-pressure homogenizer to process the crude emulsion obtained in step S40 to obtain a finished ARA nanoemulsion, the pressure of the high-pressure homogenizer is 50 MPa, and the number of high-pressure homogenization is 6 times.

[0108] Example 10

[0109] S10-20, prepare sodium casein-gum arabic complex powder according to the method described in steps S10-S20 in Example 1.

[0110] S30. Using the prepared sodium casein-arabic gum complex powder as an emulsifier, adding deionized water to form a solution, wherein the amount of the emulsifier added is 5 g / L; stirring the solution with a magnetic stirrer and centrifuging to obtain a supernatant, wherein the stirring speed of the magnetic stirrer is 2500 r / min, and the stirring time is 2 h.

[0111] S40, adding ARA oil to the supernatant obtained in step S30, and forming a crude emulsion by a high-speed shearing machine, wherein the amount of ARA oil added is 2.5 g / L, the speed of the high-speed shearing machine is 12000 r / min, and the shearing time is 3 min.

[0112] S50, using a high-pressure homogenizer to process the crude emulsion obtained in step S40 to obtain a finished ARA nanoemulsion, the pressure of the high-pressure homogenizer is 50 MPa, and the number of high-pressure homogenization is 6 times.

[0113] Embodiment 11

[0114] S10-20, prepare sodium casein-gum arabic complex powder according to the method described in steps S10-S20 in Example 1.

[0115] S30. Using the prepared sodium casein-arabic gum complex powder as an emulsifier, adding deionized water to form a solution, wherein the amount of the emulsifier added is 5 g / L; stirring the solution with a magnetic stirrer and centrifuging to obtain a supernatant, wherein the stirring speed of the magnetic stirrer is 2500 r / min, and the stirring time is 2 h.

[0116] S40, adding ARA oil to the supernatant obtained in step S30, and forming a crude emulsion by a high-speed shearing machine, wherein the amount of ARA oil added is 7.5 g / L, the speed of the high-speed shearing machine is 12000 r / min, and the shearing time is 3 min.

[0117] S50, using a high-pressure homogenizer to process the crude emulsion obtained in step S40 to obtain a finished ARA nanoemulsion, the pressure of the high-pressure homogenizer is equal to 50 MPa, and the number of high-pressure homogenization is 4 times.

[0118] Example 12

[0119] S10-20, prepare sodium casein-gum arabic complex powder according to the method described in steps S10-S20 in Example 1.

[0120] S30. Using the pre-prepared sodium casein-arabic gum complex powder as an emulsifier, adding deionized water to form a solution, wherein the amount of the emulsifier added is 5 g / L; stirring the solution with a magnetic stirrer and centrifuging to obtain a supernatant, wherein the stirring speed of the magnetic stirrer is 2500 r / min, and the stirring time is 2 h.

[0121] S40, adding ARA oil to the supernatant obtained in step S30, and forming a crude emulsion by a high-speed shearing machine, wherein the amount of ARA oil added is 2.5 g / L, the speed of the high-speed shearing machine is 12000 r / min, and the shearing time is 3 min.

[0122] S50, using a high-pressure homogenizer to process the crude emulsion obtained in step S40 to obtain a finished ARA nanoemulsion, the pressure of the high-pressure homogenizer is 50 MPa, and the number of high-pressure homogenization is 6 times.

[0123] Embodiment 13

[0124] S10-20, prepare sodium casein-gum arabic complex powder according to the method described in steps S10-S20 in Example 1.

[0125] S30. Using the prepared sodium casein-arabic gum complex powder as an emulsifier, adding deionized water to form a solution, wherein the amount of the emulsifier added is 5 g / L; stirring the solution with a magnetic stirrer and centrifuging to obtain a supernatant, wherein the stirring speed of the magnetic stirrer is 2500 r / min, and the stirring time is 2 h.

[0126] S40, adding ARA oil to the supernatant obtained in step S30, and forming a crude emulsion by a high-speed shearing machine, wherein the amount of ARA oil added is 7.5 g / L, the speed of the high-speed shearing machine is 12000 r / min, and the shearing time is 3 min.

[0127] S50, using a high-pressure homogenizer to process the crude emulsion obtained in step S40 to obtain a finished ARA nanoemulsion, the pressure of the high-pressure homogenizer is 50 MPa, and the number of high-pressure homogenization is 6 times.

[0128] Test Case

[0129] The stability of the ARA nanoemulsion prepared in the example was analyzed.

[0130] The data were regressed and fitted to obtain the quadratic polynomial regression equation of the independent variable: potential = -42.4-1.43×A-0.53×B-0.43×C+0.52×AB-0.39×AC+0.0325×BC+2.13×A2+0.96×B2+0.48×C2. A represents the amount of emulsifier added in step S30, in g / 100ml; B represents the amount of ARA oil added in step S40, in g / 100ml; C represents the number of homogenization times. The potential unit is mV, and the test results are shown in Table 1 below.

[0131] Table 1

[0132] serial number A / g / 100ml B / g / 100ml C Potential / mV Example 1 0.5 0.5 5 -42.64 Example 2 0.5 0.5 5 -42.46 Example 3 0.25 0.25 5 -36.75 Example 4 0.75 0.25 5 -40.72 Example 5 0.25 0.75 5 -38.93 Example 6 0.75 0.75 5 -40.84 Example 7 0.25 0.5 4 -38.26 Example 8 0.75 0.5 4 -40.24 Example 9 0.25 0.5 6 -38.55 Example 10 0.5 0.25 4 -40.13 Embodiment 11 0.5 0.75 4 -41.15 Example 12 0.5 0.25 6 -40.84 Embodiment 13 0.5 0.75 6 -41.73

[0133] It can be seen from Table 1 that the ARA nanoemulsion prepared in the examples provided by the present invention has high stability.

[0134] The above are only preferred embodiments of the present invention, and do not limit the patent scope of the present invention. For those skilled in the art, the present invention may have various changes and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the patent protection scope of the present invention.

Claims

1. A method for preparing an ARA nanoemulsion, characterized in that: The preparation method of the ARA nanoemulsion comprises the following steps: Dissolving casein sodium and polysaccharide powder in ultrapure water, stirring and mixing, and then freeze-drying to obtain a freeze-dried product; The freeze-dried product is ground and sieved, and then spread in a culture dish, and placed in a desiccator with a saturated KBr solution at the bottom for Maillard reaction to obtain a composite powder consisting of sodium casein and gum arabic; The composite powder is mixed with deionized water to form a solution, stirred, and centrifuged to obtain a supernatant; ARA oil is added to the supernatant to obtain a crude emulsion through high-speed shearing, wherein the shearing speed of the high-speed shearing is 10000-15000 r / min and the shearing time is 3-6 min; The crude emulsion is homogenized to obtain the ARA nanoemulsion.

2. The method for preparing an ARA nanoemulsion according to claim 1, wherein Dissolving casein sodium and polysaccharide powder together in ultrapure water, stirring and mixing, and then freeze-drying to obtain a freeze-dried product: The polysaccharide powder includes at least one of gum arabic, chitosan, dextran and maltodextrin.

3. The preparation method of ARA nanoemulsion as claimed in claim 1, characterized in that, Dissolving casein sodium and polysaccharide powder together in ultrapure water, stirring and mixing, and then freeze-drying to obtain a freeze-dried product: The mass ratio of the casein sodium to the polysaccharide powder is 1:

2.

4. The preparation method of ARA nanoemulsion as claimed in claim 1, characterized in that, The freeze-dried product is ground and sieved, and then spread in a culture dish, and placed in a dryer with a saturated KBr solution at the bottom for Maillard reaction to obtain a composite powder composed of sodium casein and gum arabic: The mesh number of the sieving is 100 meshes.

5. The preparation method of ARA nanoemulsion as claimed in claim 1, characterized in that, The freeze-dried product is ground and sieved, and then spread in a culture dish, and placed in a dryer with a saturated KBr solution at the bottom for Maillard reaction to obtain a composite powder composed of sodium casein and gum arabic: The reaction temperature of the Maillard reaction is 60° C. and the reaction time is 96 h.

6. The method for preparing the ARA nanoemulsion according to claim 1, wherein In the step of mixing the composite powder with deionized water to form a solution, stirring and centrifuging to obtain a supernatant: The mass of the composite powder added per liter of deionized water is 2.5 to 12.5 g.

7. The method for preparing the ARA nanoemulsion according to claim 1, wherein In the step of mixing the composite powder with deionized water to form a solution, stirring and centrifuging to obtain a supernatant: The stirring includes magnetic stirring, and the stirring speed of the magnetic stirring is 1000-3000 r / min and the stirring time is 2-2.5 h.

8. The method for preparing the ARA nanoemulsion according to claim 1, wherein In the step of adding ARA oil to the supernatant to obtain a crude emulsion through high-speed shearing: The mass of the ARA oil added to each liter of the supernatant is 2.5 to 12.5 g.

9. The method for preparing the ARA nanoemulsion according to claim 1, wherein The step of homogenizing the crude emulsion to obtain the ARA nanoemulsion: The homogenization pressure of the homogenization treatment is 50 to 80 MPa, and the number of homogenization times is 3 to 7 times.