Polyunsaturated fatty acid oil microcapsule, preparation method therefor, and use thereof

Abstract

The present application relates to the technical field of microcapsules, and in particular to a polyunsaturated fatty acid oil microcapsule, a preparation method therefor, and a use thereof. The present application provides a polyunsaturated fatty acid oil microcapsule, the raw material of which comprises polyunsaturated fatty acid oil, wherein an anisidine value of the polyunsaturated fatty acid oil is not greater than 10. It is found in the present application that the anisidine value of the polyunsaturated fatty acid oil will affect the solubility of the microcapsule containing the polyunsaturated fatty acid oil, and the solubility of the polyunsaturated fatty acid oil microcapsule can be effectively improved by controlling the anisidine value of the polyunsaturated fatty acid oil within a range of not higher than 10, thereby solving the problems that a product containing the polyunsaturated fatty acid oil microcapsule has poor solubility and is prone to generation of insoluble particles, and improving the quality of the product containing the polyunsaturated fatty acid oil microcapsule.

Description

A polyunsaturated fatty acid oil microcapsule, its preparation method and application

[0001] Related applications

[0002] This application claims priority to Chinese Patent Application No. 202410485526.7, filed on April 22, 2024, entitled "A Polyunsaturated Fatty Acid Oil Microcapsule and Its Preparation Method and Application", the entire contents of which are incorporated herein by reference. Technical Field

[0003] This application relates to the field of microcapsule technology, and in particular to a polyunsaturated fatty acid oil microcapsule, its preparation method, and its application. Background Technology

[0004] Polyunsaturated fatty acid oils, such as arachidonic acid (AFA) oils and docosahexaenoic acid (DHA) oils, have a wide range of biological functions in biological systems. They can regulate lipid metabolism and the immune system, and possess functions such as anti-cancer activity, prevention and treatment of cardiovascular diseases, promotion of growth and development, and regulation of gene expression. Based on the numerous functional characteristics of polyunsaturated fatty acids, their applications in the food, pharmaceutical, and feed industries have attracted widespread attention. Because AFA oils and DHA oils are easily oxidized and produce unpleasant odors, which also affect their functionality, microencapsulation technology is commonly used to protect them with encapsulating materials, thereby improving their stability and flavor.

[0005] Infant formula is one of the main application areas for polyunsaturated fatty acid oil microcapsules. When preparing infant formula, the ratio of formula to water is generally around 1:8. Users often observe whether there are insoluble particles clinging to the sides of the container, and if this occurs, they question the quality of the formula. Several factors contribute to this phenomenon, with poor solubility of the polyunsaturated fatty acid oil microcapsules being a key factor. Therefore, improving the solubility of polyunsaturated fatty acid oil microcapsules is crucial for addressing the solubility and quality issues of products using these microcapsules. Summary of the Invention

[0006] This application provides a polyunsaturated fatty acid oil microcapsule, its preparation method, and its application.

[0007] The purpose of preparing polyunsaturated fatty acid oils into microcapsules is to protect their quality and maintain their stability. Current research on microcapsule formulations mainly focuses on component selection and optimization of preparation methods (e.g., selection of wall materials, curing methods, wall material concentration, core-to-wall ratio, pH value, drying process, etc.) to improve the properties of microcapsule products. The component composition, process procedures, and product indicators of microcapsules are all quite complex.

[0008] Currently, the conventional approach to solving the solubility problem of microcapsules usually lies in adjusting the ingredients or improving the particle size of the product. For example, patent applications 2023107758584 and 202310773295.5 both address the solubility problem from the perspective of optimizing the component composition and improving the product's moisture content. There are currently no reports on the impact of the quality of the raw polyunsaturated fatty acid oils themselves on the microcapsule system or its solubility. However, in subsequent research, the applicant found that improving moisture content cannot completely solve the solubility problem of other polyunsaturated fatty acid oil microcapsule products not based on the Maillard reaction. In attempting to solve the solubility problem of polyunsaturated fatty acid oil microcapsule products not based on the Maillard reaction, this application unexpectedly discovered that the anisidine value of polyunsaturated fatty acid oils significantly affects the solubility of their microcapsules. By controlling and reducing the anisidine value of polyunsaturated fatty acid oils, the water solubility of the microcapsule powder can be effectively improved.

[0009] Specifically, this application provides the following technical solutions:

[0010] This application provides a polyunsaturated fatty acid oil microcapsule, the raw material of which includes polyunsaturated fatty acid oil, wherein the anisidine value of the polyunsaturated fatty acid oil is not greater than 10.

[0011] The anisidine value reflects the content of secondary products such as aldehydes (mainly α,β-unsaturated aldehydes) in oils. In actual production, the anisidine value of freshly produced refined oil is usually strictly controlled. However, because polyunsaturated fatty acid oils are easily oxidized, the anisidine value can increase uncontrollably when storage or environmental conditions are unsuitable or changed. This leads to the α,β-unsaturated aldehydes in the oil raw materials easily reacting with amino groups in proteins to form Schiff bases during the microcapsule storage or preparation process (especially in processes with long drying sections). The dehydration condensation of the hydrogen on the α-amino group of an amino acid with the oxygen on the carbonyl group of an aldehyde or ketone produces an imine containing a carbon-nitrogen double bond (-C=N-), called a Schiff base (as shown in Figure 1). This reaction causes the microcapsule product to exhibit poor solubility (i.e., white spots) during dissolution applications. However, since the oil is encapsulated in the microcapsule at this time, and the main aldehydes have already reacted, the relevant indicators of the produced microcapsules are often qualified. Therefore, it is difficult to realize that the indicators of polyunsaturated fatty acid oil raw materials (especially the anisidine value) will affect the solubility of their microcapsules.

[0012] This application discovers that the quality of polyunsaturated fatty acid oils themselves (anisidine value) affects the solubility of polyunsaturated fatty acid oil microcapsules, and this discovery can be applied to water-soluble microcapsules with different polyunsaturated fatty acid oil contents and formulations, and can be used to improve the quality of polyunsaturated fatty acid oil microcapsule products.

[0013] For polyunsaturated fatty acid oils with an anisamine value of no more than 10, those skilled in the art can obtain them using conventional extraction and refining methods. For polyunsaturated fatty acid oils with an anisamine value greater than 10, the anisamine value can be reduced by improving the oil refining process. For example, the anisamine value can be reduced to the range described in this application through processes such as resin adsorption, degumming, alkali refining, decolorization, and re-deodorization before being used to prepare microcapsules. In this case, the effect of improving solubility described in this application can still be achieved.

[0014] The anisidine value of the polyunsaturated fatty acid oils used in this application can be any value not exceeding 10. Through multiple degumming and high-intensity deodorization techniques, the anisidine value of the polyunsaturated fatty acid oils can be controlled to an extremely low level.

[0015] As an example, the method for reducing the anisidine value can refer to the method described in 202111582374.5, which involves sequentially treating the oil raw materials with the following steps: two degumming treatments, alkaline reaction (this step can be omitted when the acid value is less than 1 mg / g based on KOH), decolorization treatment, solvent removal treatment (this step can be omitted if no solvent is used in the preceding process), and mild deodorization treatment.

[0016] In this application, the microcapsules are water-soluble microcapsules.

[0017] In this application, the solubility refers to water solubility.

[0018] In this application, the microcapsules are not polyunsaturated fatty acid oil microcapsules based on Maillard reaction.

[0019] The content of polyunsaturated fatty acid oils in polyunsaturated fatty acid oil microcapsules is usually 15%-60%, which is suitable for most of the preparation processes in the existing technology. The content of polyunsaturated fatty acids in polyunsaturated fatty acid oils is usually 30%-60% (a few specially treated polyunsaturated fatty acid oils can have a polyunsaturated fatty acid content of 80%-90%, but the proportion of oil in the microcapsules will be reduced accordingly). Therefore, the content of polyunsaturated fatty acids in polyunsaturated fatty acid oil microcapsules is usually 5%-30%.

[0020] In this application, the mass percentage of polyunsaturated fatty acids contained in the microcapsules is 5%-30%.

[0021] In some embodiments, the microcapsules contain 7%-30% by mass of polyunsaturated fatty acids, a range more suitable for meeting the application requirements of polyunsaturated fatty acid supplementation.

[0022] For example, the mass percentage of polyunsaturated fatty acids contained in the microcapsules is 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, or 30%, or any value in between.

[0023] The aforementioned polyunsaturated fatty acids are fatty acids with a carbon chain length of 18 or more carbons and a number of double bonds of 3 or more.

[0024] The polyunsaturated fatty acids mentioned include, but are not limited to, one or more of γ-linoleic acid, DHA (docosahexaenoic acid), DPA (docosapentaenoic acid), EPA (eicosapentaenoic acid), ARA (arachidonic acid, also known as AA), and DPA (docosapentaenoic acid). These fatty acids, due to their high double bond content, are easily oxidized and readily produce unpleasant rancid or fishy odors.

[0025] In some specific embodiments of this application, the polyunsaturated fatty acid oil is AA oil, DHA oil, or EPA oil (fish oil). Generally, polyunsaturated fatty acid oils in the art often contain multiple fatty acids with a carbon chain length of 18 or more carbons and more than 3 double bonds. For example, the so-called DHA oil contains docosahexaenoic acid, eicosapentaenoic acid, and docosahexaenoic acid. The oils used in this application are not limited to those listed above. As mentioned earlier, the content of polyunsaturated fatty acids in polyunsaturated fatty acid oils is usually 30%-60%. A few specially treated oils can reach a polyunsaturated fatty acid content of 80%-90%, but for product stability considerations, the corresponding proportion of oil in the microcapsules will be reduced. None of these situations will affect the implementation of this application.

[0026] The raw materials for the microcapsules described above also include emulsifiers, which include one or more of plant gums, modified starch, and proteins.

[0027] In some embodiments, the emulsifier comprises 4%-20% by mass in the raw materials. In some embodiments, it comprises 4%-15%.

[0028] For example, the mass percentage of emulsifier can be 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, or 20%, or any value in between.

[0029] The plant gums include, but are not limited to, any one or a combination of at least two of gellan gum, gum arabic, xanthan gum, vegan gum, gelatin, dextran, pullulan, agar, pectin, carrageenan, alginate, and gelatin.

[0030] The protein is a water-soluble protein, which can be plant-based or animal-based. Animal-based proteins include one or more of sodium caseinate, whey protein, and gelatin. Plant-based proteins include one or more of pea protein, soy protein isolate, hemp seed protein, perilla seed protein, flaxseed protein, rice protein, or chickpea protein. The modified starch includes, but is not limited to, sodium octenyl succinate starch.

[0031] In some embodiments, the emulsifier is a water-soluble protein.

[0032] The water-soluble protein is a plant protein or an animal protein, wherein the animal protein preferably includes one or more of sodium caseinate, whey protein, and gelatin, and the plant protein includes one or more of pea protein, soy protein isolate, hemp seed protein, perilla seed protein, flaxseed protein, rice protein, and chickpea protein.

[0033] It should be made clear that although the emulsifying properties of various proteins differ, those skilled in the art should have the ability to adjust the compounding to achieve suitable emulsifying properties of water-soluble proteins for preparing stable microcapsule emulsions.

[0034] Furthermore, in some embodiments, the water-soluble protein includes one or more of sodium caseinate, whey protein, soy protein, and pea protein.

[0035] In some embodiments of this application, the emulsifier is sodium caseinate, or sodium caseinate and whey protein in a mass ratio of (0.5-3.5):1, or soy protein and sodium caseinate in a mass ratio of (0.5-3.5):1.

[0036] For example, the mass ratio of sodium caseinate to whey protein is (0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2.0, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9, 3.0, 3.1, 3.2, 3.3, 3.4, 3.5):1.

[0037] The raw materials for the microcapsules described above may also include one or more of the following: water-soluble filler wall materials, pH adjusters, and antioxidants.

[0038] In some embodiments, the water-soluble filler wall material includes one or more of lactose, starch, cellulose, syrup, and dextrin.

[0039] In some embodiments, the pH adjuster includes one or more of sodium citrate, potassium hydroxide, sodium hydroxide, sodium bicarbonate, potassium bicarbonate, and sodium carbonate.

[0040] The main function of pH adjusters is to maintain the feed solution at a neutral level. They can be added selectively depending on the raw materials. When adding pH adjusters, the dosage should be such that the feed solution is adjusted to a pH of 6.5-7.5.

[0041] In some embodiments, the antioxidant includes one or more of sodium ascorbate, ascorbic acid, ascorbyl palmitate, vitamin E, phospholipids, and tea polyphenols.

[0042] In some embodiments, the water-soluble filler wall material accounts for no less than 30% of the raw materials of the microcapsules described above.

[0043] The raw materials for the microcapsules described above may also include anti-caking agents.

[0044] In some embodiments, the anti-caking agent includes one or more of tricalcium phosphate, silica, microcrystalline cellulose, and magnesium stearate.

[0045] In some embodiments of this application, the raw material comprises the following components in parts by weight: 20-50 parts of polyunsaturated fatty acid oil, 4-20 parts of emulsifier, 30-60 parts of water-soluble filler wall material, 0-0.1 parts of pH adjuster, 1-10 parts of antioxidant, and 0-2 parts of anti-caking agent.

[0046] In some embodiments of this application, the raw materials comprise the following components in parts by weight: 20-50 parts of polyunsaturated fatty acid oil, 4-20 parts of emulsifier, 30-60 parts of water-soluble filler wall material, 0.005-0.1 parts of pH adjuster, 1-10 parts of antioxidant, and 0.1-1 parts of anti-caking agent.

[0047] For example, polyunsaturated fatty acid oils can be 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, or 50 parts, or any value in between.

[0048] For example, the emulsifier can be 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, or 20 parts, or any value in between.

[0049] For example, water-soluble filler wall materials can be 30 parts, 31 parts, 32 parts, 33 parts, 34 parts, 35 parts, 36 parts, 37 parts, 38 parts, 39 parts, 40 parts, 41 parts, 42 parts, 43 parts, 44 parts, 45 parts, 46 parts, 47 parts, 48 ​​parts, 49 parts, 50 parts, 51 parts, 52 parts, 53 parts, 54 parts, 55 parts, 56 parts, 57 parts, 58 parts, 59 parts, or 60 parts, as well as any value in between.

[0050] For example, the pH adjuster can be 0.005 parts, 0.015 parts, 0.025 parts, 0.035 parts, 0.045 parts, 0.055 parts, 0.065 parts, 0.075 parts, 0.085 parts, or 0.095 parts, or any value in between.

[0051] For example, the antioxidant can be 1 part, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, or 10 parts, or any value in between. For example, the anti-caking agent can be 0 parts, 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, 1.0 parts, 1.1 parts, 1.2 parts, 1.3 parts, 1.4 parts, 1.5 parts, 1.6 parts, 1.7 parts, 1.8 parts, 1.9 parts, or 2.0 parts, or any value in between.

[0052] This application also provides a method for preparing the polyunsaturated fatty acid oil microcapsules described above, the method comprising: preparing the raw materials into an emulsion, and then drying the emulsion. In some embodiments, an exemplary preparation method is provided, which includes the following steps:

[0053] (1) Mix polyunsaturated fatty acid oil, emulsifier, water-soluble wall material, antioxidant, pH adjuster and water to obtain a mixture, wherein the mixing includes stirring and shearing;

[0054] (2) Homogenize the mixture obtained in step (1) to obtain an emulsion;

[0055] (3) Dry the emulsion obtained in step (2).

[0056] In some embodiments, the shearing rate is 8000-12000 r / min.

[0057] For example, the shearing rate is 8000 r / min, 9000 r / min, 10000 r / min, 11000 r / min, or 12000 r / min, or any value in between. In some embodiments, the shearing time is 10-30 min.

[0058] For example, the cutting time can be 10 min, 11 min, 12 min, 13 min, 14 min, 15 min, 16 min, 17 min, 18 min, 19 min, 20 min, 21 min, 22 min, 23 min, 24 min, 25 min, 26 min, 27 min, 28 min, 29 min, or 30 min, or any value in between.

[0059] In some embodiments, the homogenization pressure is 600-1000 bar. For example, the pressure is 600 bar, 700 bar, 800 bar, 900 bar, or 1000 bar, and any value in between.

[0060] In some embodiments, the homogenization is performed 2-3 times.

[0061] In some embodiments, the drying method includes, but is not limited to, boiling drying, spray drying, freeze drying, fluidized bed drying, etc., with the aim of removing moisture from the liquid material to form solid particles, and is not limited thereto.

[0062] For example, the spray drying process conditions include: an inlet air temperature of 160-180°C, an outlet air temperature of 60-80°C, and a pressure of 100-200 bar.

[0063] For example, the inlet air temperature can be 160℃, 161℃, 162℃, 163℃, 164℃, 165℃, 166℃, 167℃, 168℃, 169℃, 170℃, 171℃, 172℃, 173℃, 174℃, 175℃, 176℃, 177℃, 178℃, 179℃, or 180℃, or any value in between.

[0064] For example, the air outlet temperature can be 60℃, 61℃, 62℃, 63℃, 64℃, 65℃, 66℃, 67℃, 68℃, 69℃, 70℃, 71℃, 72℃, 73℃, 74℃, 75℃, 76℃, 77℃, 78℃, 79℃, or 80℃, or any value in between.

[0065] For example, pressures of 100 bar, 110 bar, 120 bar, 130 bar, 140 bar, 150 bar, 160 bar, 170 bar, 180 bar, 190 bar, or 200 bar, or any value in between.

[0066] In some embodiments, the boiling drying temperature is between 30°C and 90°C. For example, the boiling drying temperature is 30°C, 35°C, 40°C, 45°C, 50°C, 55°C, 60°C, 65°C, 70°C, 75°C, 80°C, 85°C, or 90°C, or any value in between.

[0067] After step (3), the process also includes mixing the dried material with an anti-caking agent and then sieving it.

[0068] This application also provides the use of the above-described polyunsaturated fatty acid oil microcapsules in the preparation of food, pharmaceuticals or feed.

[0069] This application provides a product comprising the polyunsaturated fatty acid oil microcapsules described above.

[0070] In some embodiments, the product is a water-soluble powder.

[0071] In some embodiments, the product may be a dairy product, including but not limited to milk powder.

[0072] This application also provides a method for improving the solubility of polyunsaturated fatty acid oil microcapsules, the method comprising: controlling the anisidine value of the polyunsaturated fatty acid oil used in the preparation of the microcapsules to be no greater than 10.

[0073] In some embodiments, the microcapsules contain 5%-30% by mass of polyunsaturated fatty acids. In some embodiments, the content is 7%-30%. For example, the microcapsules contain 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, or 30% by mass, or any value in between.

[0074] In some embodiments, the polyunsaturated fatty acid is a fatty acid with a carbon chain length of 18 or more carbons and a number of double bonds of 3 or more.

[0075] The beneficial effects of this application include at least the following: This application has discovered that the anisidine value of polyunsaturated fatty acid oils affects the solubility of polyunsaturated fatty acid oil microcapsules. By controlling the anisidine value of polyunsaturated fatty acid oils to a range not exceeding 10, the solubility of polyunsaturated fatty acid oil microcapsules can be effectively improved. This helps to solve problems such as poor solubility and easy formation of insoluble particles adhering to the wall in products containing polyunsaturated fatty acid oil microcapsules, thereby improving the quality of polyunsaturated fatty acid oil microcapsule products. Attached Figure Description

[0076] To more clearly illustrate the technical solutions in this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0077] Figure 1 is a reaction formula in the invention content section of this application, in which α,β-unsaturated aldehydes react with amino groups in proteins to form Schiff bases. Detailed Implementation

[0078] To make the objectives, technical solutions, and advantages of this application clearer, the technical solutions of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application.

[0079] The present application will be further described in detail below with reference to the embodiments and examples. It should be understood that these embodiments and examples are for illustrative purposes only and are not intended to limit the scope of the present application. The purpose of providing these embodiments and examples is to enable a more thorough and comprehensive understanding of the disclosure of the present application. It should also be understood that the present application can be implemented in many different forms and is not limited to the embodiments and examples described herein. Those skilled in the art can make various modifications or alterations without departing from the spirit of the present application, and the equivalent forms obtained also fall within the protection scope of the present application. Furthermore, numerous specific details are set forth in the following description to provide a more complete understanding of the present application. It should be understood that the present application can be implemented without one or more of these details.

[0080] Unless otherwise defined, all technical and scientific terms used in this application have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains.

[0081] In this application, the technical features described in an open-ended manner include both closed technical solutions consisting of the listed features and open technical solutions that include the listed features.

[0082] In this application, numerical intervals (i.e., numerical ranges) are involved. Unless otherwise specified, the selected numerical distributions within the aforementioned numerical intervals are considered continuous and include the two endpoints (i.e., the minimum and maximum values) of the numerical range, as well as every value between these two endpoints. Unless otherwise specified, when a numerical interval refers only to integers within that interval, it includes the two endpoint integers of the numerical range, as well as every integer between the two endpoints. In this document, this is equivalent to directly listing every integer. For example, if t is an integer selected from 1 to 10, it means that t is any integer selected from the group of integers consisting of 1, 2, 3, 4, 5, 6, 7, 8, 9, and 10. Furthermore, when multiple ranges are provided to describe features or characteristics, these ranges can be merged. In other words, unless otherwise specified, the ranges disclosed herein should be understood to include any and all subranges to which they are included.

[0083] Unless otherwise specified, the temperature parameters in this application are permitted to be either constant-temperature treatment or variations within a certain temperature range. It should be understood that the constant-temperature treatment allows temperature fluctuations within the precision range of the instrument control, such as ±5℃, ±4℃, ±3℃, ±2℃, or ±1℃.

[0084] In this application, % (w / w) and wt% both represent weight percentage, % (v / v) refers to volume percentage, and % (w / v) refers to mass-volume percentage.

[0085] All references to documents mentioned in this application are incorporated herein by reference as if each document were individually incorporated herein by reference. Unless they conflict with the inventive purpose and / or technical solution of this application, all cited documents are incorporated herein by reference in their entirety and for all purposes. When citing documents in this application, the definitions of relevant technical features, terms, nouns, phrases, etc., are also incorporated herein by reference. When citing documents in this application, examples and preferred embodiments of the cited technical features may also be incorporated herein by reference, but only to the extent that they enable the implementation of this application. It should be understood that when the cited content conflicts with the description in this application, this application shall prevail or modifications shall be made adaptably to the description in this application.

[0086] The DHA oil used in the following examples contains 50% docosahexaenoic acid (DHA) and 11% other polyunsaturated fatty acids as defined above. The AA oil contains 45% eicosapentaenoic acid (EPA) and 6% other polyunsaturated fatty acids as defined above. The fish oil contains 70% eicosapentaenoic acid (EPA) and 2% other polyunsaturated fatty acids as defined above. Due to variations in processing batches, time, and storage conditions, the anisidine values ​​of the above oils may differ.

[0087] The embodiments of this application will be described in detail below with reference to examples. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of this application. For experimental methods in the following embodiments where specific conditions are not specified, please refer to the guidelines given in this application, or follow experimental manuals or conventional conditions in the art, or follow the conditions recommended by the manufacturer, or refer to experimental methods known in the art.

[0088] In the specific embodiments described below, the measurement parameters involving raw material components may have slight deviations within the weighing accuracy range unless otherwise specified. Temperature and time parameters are subject to acceptable deviations due to instrument testing accuracy or operational precision.

[0089] It should be understood that in the various embodiments of this application, the order of the above-mentioned processes does not imply the order of execution. The execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the embodiments of this application.

[0090] Example 1

[0091] This embodiment provides a polyunsaturated fatty acid oil microcapsule, the raw materials of which include the following components (mass percentage): sodium caseinate 4%, DHA oil 26%, sodium ascorbate 4.5%, tricalcium phosphate 0.6%, sodium citrate 0.01%, solid corn syrup 14.89%, and the remainder being lactose, wherein the anisidine value of the DHA oil is 6.9.

[0092] This embodiment also provides a method for preparing the above-mentioned polyunsaturated fatty acid oil microcapsules, the method comprising the following steps:

[0093] (1) Mix DHA oil, sodium caseinate, lactose, sodium ascorbate, sodium citrate, solid corn syrup and water to obtain a mixture. The mixing process includes stirring and shearing, wherein the shearing is shearing at 10000r / min speed for 10min.

[0094] (2) Homogenize the mixture obtained in step (1) at 800 bar for 2-3 times to obtain an emulsion;

[0095] (3) The emulsion obtained in step (2) is atomized into droplets and sprayed into a preheated boiling dryer. The temperature inside the boiling dryer is 60℃-80℃. Powder-encapsulated lactose is placed at the bottom of the boiling dryer. At the same time, the boiling dryer is dried by blowing air to maintain the temperature inside the boiling dryer at 60℃-80℃.

[0096] (4) Then dry it further, mix it with tricalcium phosphate, and sieve it to obtain polyunsaturated fatty acid oil microcapsule products.

[0097] Example 2

[0098] This embodiment provides a polyunsaturated fatty acid oil microcapsule, the only difference between its raw materials and those in Example 1 is that the anisidine value of the DHA oil is 3.12.

[0099] This embodiment also provides a method for preparing the above-mentioned polyunsaturated fatty acid oil microcapsules, which is the same as the preparation method in Example 1.

[0100] Example 3

[0101] This embodiment provides a polyunsaturated fatty acid oil microcapsule, the only difference between its raw materials and those in Example 1 is that the anisidine value of the DHA oil is 1.87.

[0102] This embodiment also provides a method for preparing the above-mentioned polyunsaturated fatty acid oil microcapsules, which is the same as the preparation method in Example 1.

[0103] Example 4

[0104] This embodiment provides a polyunsaturated fatty acid oil microcapsule, the only difference between its raw materials and those of Example 1 is that the anisidine value of the DHA oil is 2.37.

[0105] This embodiment also provides a method for preparing the above-mentioned polyunsaturated fatty acid oil microcapsules, which is the same as the preparation method in Example 1.

[0106] Example 5

[0107] This embodiment provides a polyunsaturated fatty acid oil microcapsule, the raw materials of which include the following components (mass percentage): sodium caseinate 10%, whey protein powder 5%, AA oil 46%, sodium ascorbate 5.5%, tricalcium phosphate 0.6%, sodium citrate 0.01%, maltodextrin 32.89%, wherein the anisidine value of the AA oil is 1.87.

[0108] This embodiment also provides a method for preparing the above-mentioned polyunsaturated fatty acid oil microcapsules, the method comprising the following steps:

[0109] (1) Mix AA oil, sodium caseinate, whey protein powder, solid corn syrup, sodium ascorbate, sodium citrate and water to obtain a mixture. The mixing process includes stirring and shearing, wherein the shearing is shearing at 10000r / min speed for 10min.

[0110] (2) Homogenize the mixture obtained in step (1) at 800 bar for 2-3 times to obtain an emulsion;

[0111] (3) The emulsion obtained in step (2) is directly spray-dried under the following conditions: inlet air temperature 170±5℃, outlet air temperature 70±5℃, and spray pressure 180 bar.

[0112] (4) Mix the dried material from step (3) with tricalcium phosphate and sieve to obtain polyunsaturated fatty acid oil microcapsule product.

[0113] Example 6

[0114] This embodiment provides a polyunsaturated fatty acid oil microcapsule, the raw materials of which include the following components (mass percentage): 8% soybean protein, 8% sodium caseinate, 33% fish oil, 4.0% sodium ascorbate, 0.5% tricalcium phosphate, 0.01% sodium citrate, and the remainder being solid corn syrup, wherein the fish oil has anisidine value of 7.15.

[0115] This embodiment also provides a method for preparing the above-mentioned polyunsaturated fatty acid oil microcapsules, the method comprising the following steps:

[0116] (1) Fish oil, sodium caseinate, soy protein, solid corn syrup, sodium ascorbate, sodium citrate and water are mixed to obtain a mixture. The mixing process includes stirring and shearing, wherein the shearing is shearing at 10000r / min speed for 10min.

[0117] (2) Homogenize the mixture obtained in step (1) at 800 bar for 2-3 times to obtain an emulsion;

[0118] (3) The emulsion obtained in step (2) is directly spray-dried under the following conditions: inlet air temperature 160±5℃, outlet air temperature 80±5℃, and spray pressure 185 bar.

[0119] (4) Mix the dried material from step (3) with tricalcium phosphate and sieve to obtain polyunsaturated fatty acid oil microcapsule product.

[0120] Comparative Example 1

[0121] This comparative example provides a polyunsaturated fatty acid oil microcapsule, the only difference between its raw materials and those of Example 1 is that the DHA oil has anisidine value of 25.7.

[0122] The preparation method of the above-mentioned polyunsaturated fatty acid oil microcapsules is the same as that of Example 1.

[0123] Comparative Example 2

[0124] This comparative example provides a polyunsaturated fatty acid oil microcapsule, the only difference between its raw materials and those of Example 1 is that the anisidine value of the DHA oil is 31.09.

[0125] The preparation method of the above-mentioned polyunsaturated fatty acid oil microcapsules is the same as that of Example 1.

[0126] Comparative Example 3

[0127] This comparative example provides a polyunsaturated fatty acid oil microcapsule, the only difference between its raw materials and those of Example 1 is that the anisidine value of the DHA oil is 29.65.

[0128] The preparation method of the above-mentioned polyunsaturated fatty acid oil microcapsules is the same as that of Example 1.

[0129] Comparative Example 4

[0130] This comparative example provides a polyunsaturated fatty acid oil microcapsule, the only difference between its raw materials and those of Example 1 is that the DHA oil has anisidine value of 15.

[0131] The preparation method of the above-mentioned polyunsaturated fatty acid oil microcapsules is the same as that of Example 1.

[0132] Comparative Example 5

[0133] This comparative example provides a polyunsaturated fatty acid oil microcapsule, the only difference between its raw material and that of Example 5 is that the anisidine value of the AA oil is 31.09.

[0134] The preparation method of the above-mentioned polyunsaturated fatty acid oil microcapsules is the same as that of Example 5.

[0135] Comparative Example 6

[0136] This comparative example provides a polyunsaturated fatty acid oil microcapsule, the only difference between its raw material and that of Example 5 is that the anisidine value of the AA oil is 18.46.

[0137] The preparation method of the above-mentioned polyunsaturated fatty acid oil microcapsules is the same as that of Example 5.

[0138] Comparative Example 7

[0139] This comparative example provides a polyunsaturated fatty acid oil microcapsule, the only difference between its raw material and that of Example 6 is that the fish oil has anisidine value of 40.58.

[0140] The preparation method of the above-mentioned polyunsaturated fatty acid oil microcapsules is the same as that in Example 6.

[0141] Experimental Example: Solubility Detection of Polyunsaturated Fatty Acid Oil Microcapsules

[0142] The solubility of the polyunsaturated fatty acid oil microcapsules in each example and comparative example was tested using the following method: At a water temperature of 40-50℃, 0.5g of polyunsaturated fatty acid oil microcapsule powder was added to 200mL of pure water. After stirring for 30 seconds (15 rotations to the left and 15 rotations to the right), the mixture was poured onto a ceramic plate. The presence or absence of white spots on the ceramic plate was observed, and the number of white spots was recorded. If the number of white spots was greater than 10, it was considered negligible. The results are shown in Table 1. When the anisidine value of the polyunsaturated fatty acid oil was not higher than 10 (Examples 1-6), the number of insoluble particles formed when the microcapsules dissolved in water was significantly less than when using polyunsaturated fatty acid oils with anisidine values ​​greater than 10 (Comparative Examples 1-7). Therefore, this application achieves a significant improvement in the solubility of polyunsaturated fatty acid oil microcapsules by controlling the anisidine value of the polyunsaturated fatty acid oil.

[0143] Table 1

[0144] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of this application.

Claims

1. A polyunsaturated fatty acid oil microcapsule, characterized in that, Its raw materials include polyunsaturated fatty acid oils, wherein the anisidine value of the polyunsaturated fatty acid oils is not greater than 10.

2. The polyunsaturated fatty acid oil microcapsules according to claim 1, characterized in that, The microcapsules are water-soluble microcapsules.

3. The polyunsaturated fatty acid oil microcapsules according to claim 1 or 2, characterized in that, The microcapsules contain 5%-30% polyunsaturated fatty acids by mass.

4. The polyunsaturated fatty acid oil microcapsules according to claim 1 or 2, characterized in that, The microcapsules contain 7%-30% polyunsaturated fatty acids by mass.

5. The polyunsaturated fatty acid oil microcapsules according to any one of claims 1 to 4, characterized in that, The polyunsaturated fatty acids are fatty acids with a carbon chain length of 18 or more carbons and a number of double bonds of 3 or more.

6. The polyunsaturated fatty acid oil microcapsules according to any one of claims 1 to 5, characterized in that, The raw materials also include emulsifiers.

7. The polyunsaturated fatty acid oil microcapsules according to claim 6, characterized in that, The emulsifier includes one or more of plant gums, modified starch, and protein.

8. The polyunsaturated fatty acid oil microcapsules according to claim 6 or 7, characterized in that, The emulsifier in the raw materials has a mass percentage content of 4%-20%.

9. The polyunsaturated fatty acid oil microcapsules according to any one of claims 6 to 8, characterized in that, The emulsifier is a water-soluble protein.

10. The polyunsaturated fatty acid oil microcapsules according to claim 9, characterized in that, The water-soluble protein is either plant protein or animal protein.

11. The polyunsaturated fatty acid oil microcapsules according to claim 10, characterized in that, The animal protein includes one or more of sodium caseinate, whey protein, and gelatin.

12. The polyunsaturated fatty acid oil microcapsules according to claim 10, characterized in that, The plant protein includes one or more of the following: pea protein, soy protein, hemp seed protein, perilla seed protein, flaxseed protein, rice protein, and chickpea protein.

13. The polyunsaturated fatty acid oil microcapsules according to claim 9 or 10, characterized in that, The water-soluble protein includes one or more of sodium caseinate, whey protein, soy protein, and pea protein.

14. The polyunsaturated fatty acid oil microcapsules according to any one of claims 1 to 13, characterized in that, The raw materials also include one or more of water-soluble filler wall materials, pH adjusters, and antioxidants.

15. The polyunsaturated fatty acid oil microcapsules according to claim 14, characterized in that, The water-soluble filler wall material includes one or more of lactose, starch, cellulose, syrup, and dextrin.

16. The polyunsaturated fatty acid oil microcapsules according to claim 14, characterized in that, The pH adjuster includes one or more of sodium citrate, potassium hydroxide, sodium hydroxide, sodium bicarbonate, potassium bicarbonate, and sodium carbonate.

17. The polyunsaturated fatty acid oil microcapsules according to claim 14, characterized in that, The antioxidants include one or more of sodium ascorbate, ascorbic acid, ascorbyl palmitate, vitamin E, phospholipids, and tea polyphenols.

18. The polyunsaturated fatty acid oil microcapsules according to claim 14, characterized in that, The water-soluble filler wall material in the raw materials shall have a mass percentage of not less than 30%.

19. The method for preparing polyunsaturated fatty acid oil microcapsules according to any one of claims 1 to 18, characterized in that, The method includes: preparing the raw materials into an emulsion, and then drying the emulsion.

20. A product characterized in that, The product comprises polyunsaturated fatty acid oil microcapsules as described in any one of claims 1 to 18.

21. The product according to claim 20, characterized in that, The product is a water-soluble powder.

22. A method for improving the solubility of polyunsaturated fatty acid oil microcapsules, characterized in that, The method includes: The anisidine value of the polyunsaturated fatty acid oil used in the preparation of the microcapsules is controlled to be no greater than 10.

23. The method for improving the solubility of polyunsaturated fatty acid oil microcapsules according to claim 22, characterized in that, The polyunsaturated fatty acid oil is defined as any one of claims 1-18.

24. The method for improving the solubility of polyunsaturated fatty acid oil microcapsules according to claim 22, characterized in that, The microcapsule preparation also includes the use of emulsifiers; The emulsifier is defined as an emulsifier as described in any one of claims 6 to 13.

25. The method for improving the solubility of polyunsaturated fatty acid oil microcapsules according to claim 22, characterized in that, The microcapsule preparation also includes the use of one or more of water-soluble filler wall materials, pH adjusters, and antioxidants; The water-soluble filler wall material, the pH adjuster, and the antioxidant are defined as described in any one of 14 to 18.

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