A perilla seed oil microcapsule emulsion and a preparation process thereof
By using sodium caseinate and chitosan hydrochloride as wall materials and combining them with high-pressure homogenization technology, a perilla seed oil microcapsule emulsion with small particle size and high stability was prepared, which solved the stability and particle size problems in the existing technology and achieved good emulsification effect and storage performance.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- BEIJING TECH & BUSINESS UNIV
- Filing Date
- 2026-04-29
- Publication Date
- 2026-06-23
AI Technical Summary
Existing perilla seed oil microemulsions have low stability, with an absolute zeta potential value of less than 30mV, and varying particle sizes with a relatively large particle size of around 1-10μm.
Sodium caseinate and chitosan hydrochloride were used as wall materials to prepare perilla seed oil microcapsule emulsions by high-pressure homogenization technology. The mass ratio of core material to wall material was controlled at 15:1-3. Multiple high-pressure homogenizations were performed, and the pH value was adjusted to 7±0.1.
The microcapsule emulsion of perilla seed oil exhibits good centrifugal stability, small and uniform particle size, an absolute Zeta potential value above 40mV, strong emulsification ability, and good storage stability.
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Figure CN122250665A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of health food processing technology, specifically to a perilla seed oil microcapsule emulsion and its preparation process. Background Technology
[0002] For understanding the technical content of this invention: Perilla seed oil is a plant oil extracted from perilla seeds. It contains 54%-64% alpha-linolenic acid and is rich in vitamin E, exhibiting good anti-inflammatory, antioxidant, and cardiovascular disease prevention effects. However, the high content of polyunsaturated fatty acids in perilla seed oil makes it extremely sensitive to light, heat, and oxygen. It is easily oxidized under light and high temperatures and is unstable, limiting its application scenarios. Therefore, how to protect its biological activity and improve its oxidative stability has become an urgent problem to be solved.
[0003] Microcapsules are miniature containers with polymer walls, essentially encapsulating a core material within the wall material to form tiny sacs with semi-permeable or sealed membranes. This technology reduces the impact of external environmental factors, such as light and temperature, on the chemical properties of the core material and masks unpleasant odors and colors, facilitating transportation, storage, and better application. With technological advancements, the preparation of perilla seed oil using microencapsulation technology has become a popular research area.
[0004] Relevant patent documents retrieved: This document, published in China (CN114698843B) on May 12, 2023, discloses a perilla seed oil microemulsion-hydrogel system, its preparation method, and its application. The method includes the following steps: 1) mixing casein with water to obtain an aqueous phase, mixing EGCG with perilla seed oil to obtain an oil phase, and mixing and homogenizing the aqueous and oil phases to obtain a perilla seed oil microemulsion; 2) adding gellan gum solution dropwise to a chitosan-MgCl2 solution, and repeatedly freezing and thawing 3-5 times to obtain a hydrogel; 3) freeze-drying the hydrogel and mixing it with the perilla seed oil microemulsion for 10-14 hours to obtain the perilla seed oil microemulsion-hydrogel system. This invention prepares an oil-in-water EGCG perilla seed oil microemulsion and then prepares it into a hydrogel system, further improving the stability and physiological activity of perilla seed oil. However, the absolute value of the Zeta potential of the perilla seed oil microemulsion is only 20.77±0.68mV, indicating low stability.
[0005] This document, published in China (CN111436500A) on July 24, 2020, discloses a method for preparing perilla seed oil microcapsules by adding corn oligopeptides. The perilla seed oil microcapsules comprise a core material and a wall material. The core material is perilla seed oil, and the wall material is a mixture of one or more of the following: gum arabic, soluble soybean polysaccharide, modified starch, sodium caseinate, and soy protein isolate, along with corn oligopeptides. This invention reduces the oil content on the surface of the perilla seed oil microcapsules by adding corn oligopeptides to the wall material for reinforcement and to enhance the emulsifying effect of the core material, thereby improving the encapsulation of perilla seed oil in the wall material and preventing oxidation of the perilla seed oil. However, the resulting perilla seed oil microcapsules have inconsistent particle sizes and are relatively large, around 10 μm.
[0006] Relevant non-patent literature retrieved: The document, titled "Preparation of Soybean Polysaccharide-Chitosan Complex and Its Effect on the Physicochemical Stability of Perilla Seed Oil," is a master's thesis published by Hebei University of Science and Technology in May 2019. It discloses a single-layer and double-layer emulsion of perilla seed oil, using perilla seed oil as the core material and soybean polysaccharide and chitosan as the wall material. The chitosan concentration is greater than 0.4%, resulting in a Zeta potential of 43 mV, but its maximum particle size is 1.185 μm.
[0007] The prior art represented by the aforementioned documents has at least the following unresolved technical problems or defects: (1) Perilla seed oil microemulsion has low stability, with an absolute value of Zeta potential below 30mV; (2) The particle size is not uniform and the particle diameter is relatively large, around 1-10 μm. Summary of the Invention
[0008] The purpose of this invention is to provide: A perilla seed oil microcapsule emulsion and its preparation process, as well as related technologies, are disclosed to solve technical problems such as centrifugal stability, small particle size, polydispersity index of less than 0.3, zeta potential of greater than 40mV and good emulsification ability, or combinations thereof.
[0009] Terminology Explanation: Unless otherwise defined, all technical terms in this document have the same meanings as commonly understood by one of ordinary skill in the art to which the subject matter of the claims pertains. Unless otherwise stated, all patents, patent inventions, and publications cited in this document are incorporated herein by reference in their entirety. If multiple definitions exist for terms in this document, the definitions in this chapter shall prevail.
[0010] It should be understood that the above brief description and the following detailed description are exemplary and for illustrative purposes only, and do not limit the subject matter of the invention in any way. In this invention, the singular is used in conjunction with the plural unless otherwise specifically stated. It should also be noted that, unless otherwise stated, the use of “or” or “or” means “and / or”. Furthermore, the use of the term “comprising” and other forms such as “including,” “containing,” and “contains” are not limiting.
[0011] Definitions of standard chemical terms can be found in the references "Food Microencapsulation Technology" and "Encyclopedia of Food Engineering".
[0012] Unless otherwise stated, conventional methods within the scope of the art shall be used.
[0013] Unless specifically defined herein, the use of all commercially available products herein employs standard techniques. For example, it may be carried out using the manufacturer's instructions for use with the kit, or in accordance with methods known in the art or the description of this invention. The techniques and methods described herein can generally be implemented according to conventional methods well known in the art, based on the descriptions in the various summary and more specific documents cited and discussed in this specification.
[0014] As used herein, "perilla seed oil" refers to an oil extracted from the seeds of *Perilla frutescens* L. (family Lamiaceae), characterized by its high content of α-linolenic acid (ALA, an ω-3 polyunsaturated fatty acid), typically exceeding 50%. In this invention, it serves as the core material (active load) of microcapsules.
[0015] As used in this article, the term "microcapsule" refers to a miniature container or package with a polymer wall shell.
[0016] The term "sodium caseinate" used in this article refers to the sodium salt form of casein (the main protein in milk) obtained after alkali treatment. It is a food-grade emulsifier and film-forming protein with good emulsifying, thickening and film-forming abilities, and is often used to construct microcapsule wall materials.
[0017] The term "homogenization" as used in this article refers to a mechanical process that reduces the particle size and homogenizes the distribution of particles in an emulsion or suspension.
[0018] The term "chitosan hydrochloride" as used in this article refers to the hydrochloride form of chitosan (a deacetylated product of chitin), a cationic polysaccharide with good water solubility, film-forming properties and biocompatibility, and capable of forming polyelectrolyte complexes with anionic wall materials.
[0019] The term "emulsion" as used in this article refers to an "oil / water" (O / W) emulsion system formed by dispersing perilla seed oil in an aqueous phase containing wall material during the microcapsule preparation process.
[0020] The term "high-pressure homogenization" as used in this article refers to the key process of obtaining nano- or micron-scale stable emulsions by using a high-pressure homogenizer to pass fluid through a narrow homogenizing valve at high pressures of tens to hundreds of megapascals (MPa).
[0021] The term "PE9010" used in this article refers to a preservative composed of phenoxyethanol and ethylhexylglycerin.
[0022] In a first aspect, the present invention provides: a perilla seed oil microcapsule emulsion, comprising a core material and a wall material.
[0023] This includes technical features: core material and wall material.
[0024] The core material is perilla seed oil; the wall material is sodium caseinate and chitosan salts. Preferably, the chitosan salts include one of chitosan hydrochloride, chitosan quaternary ammonium salt, chitosan lactate, and chitosan glutamate. More preferably, the chitosan salt is chitosan hydrochloride.
[0025] Preferably, the mass ratio of the core material to the wall material is 15:1-3; More preferably, the mass ratio of the core material to the wall material is 15:1-2; More preferably, the mass ratio of the core material to the wall material is 15:1; Preferably, the mass ratio of sodium caseinate to chitosan hydrochloride is 1:1.
[0026] Secondly, the present invention provides a preparation process for the above-mentioned perilla seed oil microcapsule emulsion, comprising the following steps: (1) Add sodium caseinate to a solvent and stir until it is completely dissolved to obtain solution A. Add chitosan hydrochloride to a solvent and stir until it is completely dissolved to obtain solution B. (2) Homogenize solution A once, add perilla seed oil and homogenize a second time, and finally add solution B and homogenize a third time to obtain an emulsion. (3) The emulsion is homogenized under high pressure, preservatives are added, and the mixture is stirred evenly to obtain the perilla seed oil microcapsule emulsion.
[0027] The technical features include: solvent, stirring, homogenization, high-pressure homogenization, and preservative.
[0028] The solvent is water and / or glycerin; Preferably, the amount of glycerol added is 0-13% of the mass of the solvent; Preferably, the mass ratio of sodium caseinate to solvent is 0.5-1.5:40-42, and the mass ratio of chitosan hydrochloride to solvent is 0.5-1.5:40-42. The stirring temperature in step (1) is 50-60℃, and the stirring time is 30-60 min; Preferably, the stirring temperature is any point or range between 50-60℃, and can be selected from 50℃, 52℃, 55℃, 57℃, 59℃, and 60℃. As a further preferred embodiment, the stirring temperature is any point or range between 50-60℃, and can be selected from 50℃, 55℃, 59℃, and 60℃. Most preferably, the stirring temperature is any point or range between 50-60°C, and can be selected from 60°C.
[0029] Preferably, the stirring time is any value or range between 30 and 60 minutes, and can be selected from 30 minutes, 40 minutes, 50 minutes, and 60 minutes. As a further preferred embodiment, the stirring time is any value or range between 30 and 60 min, and can be selected from 40 min, 50 min, or 60 min. Most preferably, the stirring time is any value or range between 30 and 60 minutes, and can be selected from 40 minutes.
[0030] The rotation speed for the first, second, and third homogenizations in step (2) is 8000-10000 rpm, and the time is 5-10 min. Preferably, the rotational speed is any point or range value between 8000-10000 rpm, and can be selected from 8000 rpm, 8500 rpm, 9000 rpm, 9500 rpm, and 10000 rpm. As a further preferred embodiment, the rotational speed is any point or range value between 8000-10000 rpm, and can be selected from 8000 rpm, 9000 rpm, or 10000 rpm. Most preferably, the rotational speed is any point or range between 8000-10000 rpm, and can be selected from 10000 rpm.
[0031] Preferably, the time is any point or range value between 5 and 10 minutes, and can be selected from 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes, and 10 minutes. As a further preferred embodiment, the time is any point or range value between 5 and 10 minutes, and can be selected from 5 minutes, 7 minutes, 9 minutes, and 10 minutes; Most preferably, the time is any point or range between 5 and 10 minutes, and can be selected from 5 minutes.
[0032] The pH value of the emulsion described in step (2) is 7±0.1.
[0033] The pressure of high-pressure homogenization in step (3) is 600-800 bar, and the number of homogenization cycles is 4-6. Preferably, the pressure is any point or range between 600-800 bar, and can be selected from 600 bar, 650 bar, 700 bar, 750 bar, or 800 bar. As a further preferred embodiment, the pressure is any point or range value between 600-800 bar, and can be selected from 600 bar, 700 bar, or 800 bar; Most preferably, the pressure is any point or range between 600-800 bar, and can be selected from 800 bar.
[0034] Preferably, the number of homogenization cycles is any point or range between 4 and 6, and can be selected from 4, 5, or 6 times. As a further preferred embodiment, the number of homogenization cycles is any value or range between 4 and 6, and can be selected from 4 or 5 times. Most preferably, the number of homogenization cycles is any value or range between 4 and 6, and can be selected from 5 cycles.
[0035] The preservative mentioned is PE9010.
[0036] Based on further solutions to the technical problems of the present invention, or simultaneous solutions to multiple technical problems, the preferred solution in the technical solution provided in the first aspect of the present invention includes: The first preferred solution is as follows: the stirring temperature in step (1) is 50-60℃, the stirring time is 30-60 min, the rotation speed of the first, second, and third homogenizations in step (2) is 8000-10000 rpm, and the time is 5-10 min, and the pressure of the high-pressure homogenization in step (3) is 600-800 bar, and the number of homogenizations is 4-6. This technical solution solves the technical problem of "centrifugal stability" and further solves the technical problem of "reducing particle size".
[0037] The second preferred solution is as follows: the stirring temperature in step (1) is 60℃, the stirring time is 40 min, the rotation speed of the first homogenization, second homogenization and third homogenization in step (2) is 10000 rpm, and the time is 5 min, and the pressure of the high-pressure homogenization in step (3) is 800 bar, and the number of homogenizations is 5. This technical solution solves the technical problem of "centrifugal stability" and further solves the technical problem of "reducing particle size".
[0038] Examples 1-6 of this invention at least support the protection scope of the claims regarding the mass ratio of core material to wall material, the mass ratio of glycerol, sodium caseinate or chitosan hydrochloride to the solvent, homogenization, and high-pressure homogenization.
[0039] The mass ratio of the core material to the wall material is 15:1-3, which is summarized by the corresponding technical features "15:1, 15:3" in the foregoing explanation and / or embodiments 1-6. Therefore, those skilled in the art can reasonably infer that the technical feature "the mass ratio of the core material to the wall material is 15:1-3", its subordinate concepts, its substantially equivalent technical means, and technical means that can replace it within the scope of conventional technical means and common knowledge based on the existing level of technology should all fall within the protection scope of the mass ratio of the core material to the wall material.
[0040] The amount of glycerol added is 0-13% of the mass of the solvent, which is summarized by the corresponding technical features "0, 6%, 12%, 6.1%, 12.3%" in the foregoing explanation and / or Examples 1-6. Therefore, those skilled in the art can reasonably presume that the technical feature "the amount of glycerol added is 0-13% of the mass of the solvent", its subordinate concept, its substantially equivalent technical means, and technical means that can replace it within the scope of conventional technical means and common knowledge based on the existing level of technology should all fall within the protection scope of glycerol.
[0041] The mass ratio of sodium caseinate to solvent is 0.5-1.5:40-42, which is summarized by the corresponding technical features "0.5:41.7, 1.5:40.7" in the foregoing explanation and / or Examples 1-6. Therefore, those skilled in the art can reasonably infer that the technical feature "the mass ratio of sodium caseinate to solvent is 0.5-1.5:40-42", its subordinate concepts, its substantially equivalent technical means, and technical means that can replace it within the scope of conventional technical means and common knowledge based on the existing technical level should all fall within the protection scope of the mass ratio of sodium caseinate to solvent.
[0042] The mass ratio of chitosan hydrochloride to the solvent is 0.5-1.5:40-42, which is summarized by the corresponding technical features "0.5:41.7, 1.5:40.7" in the foregoing explanation and / or Examples 1-6. Therefore, those skilled in the art can reasonably infer that the technical feature "the mass ratio of chitosan hydrochloride to the solvent is 0.5-1.5:40-42", its subordinate concepts, its substantially equivalent technical means, and technical means that can replace it within the scope of conventional technical means and common knowledge based on the existing technical level should all fall within the protection scope of the mass ratio of chitosan hydrochloride to the solvent.
[0043] The conditions for the first, second, and third homogenizations described in step (2) are all selected from a rotation speed of 8000-10000 rpm and a time of 5-10 min, which are summarized by the corresponding technical features "10000 rpm" and "5 min" in the foregoing explanation and / or Examples 1-6. Therefore, those skilled in the art can reasonably infer that the technical feature "the conditions for the first, second, and third homogenizations described in step (2) are all selected from a rotation speed of 8000-10000 rpm and a time of 5-10 min", its subordinate concepts, its basically equivalent technical means, and technical means that can replace it within the scope of conventional technical means and common knowledge based on the existing technical level should all fall within the protection scope of homogenization.
[0044] The high-pressure homogenization conditions described in step (3) are selected from homogenization pressure of 600-800 bar and homogenization times of 4-6 times, which are summarized by the corresponding technical features "800 bar" and "5 times" in the foregoing explanation and / or Examples 1-6. Therefore, those skilled in the art can reasonably infer that the technical feature "the high-pressure homogenization conditions described in step (3) are selected from homogenization pressure of 600-800 bar and homogenization times of 4-6 times", its subordinate concepts, its basically equivalent technical means, and technical means that can replace it within the scope of conventional technical means and common knowledge based on the existing technical level should all fall within the protection scope of high-pressure homogenization.
[0045] The beneficial effects of this invention are as follows: The present invention has at least the following beneficial effects: 1. Compared with the prior art, the present invention has better technical effect in terms of particle size.
[0046] According to experimental tests, the present invention reduces the particle size from 1-10 μm in the prior art to below 900 nm.
[0047] 2. Compared with the prior art, the present invention provides a technical solution with a different technical concept, and its technical effect is equivalent to or slightly improved with the prior art. The difference between the technical concept of the present invention and the prior art includes, but is not limited to, the present invention using a higher core material to wall material mass ratio (15:1-3), and using a 1:1 mixture of sodium caseinate and chitosan hydrochloride as the wall material to encapsulate perilla seed oil.
[0048] 3. The perilla seed oil microcapsule emulsion preparation process provided by this invention is simple to operate, cost-effective, and has broad market application prospects. 4. The perilla seed oil microcapsule emulsion of the present invention has small and uniform particle size, high stability and good emulsification ability, which is beneficial to better storage and application of perilla seed oil.
[0049] Furthermore, based on the present invention: Based on the comparison of Examples 1-6 and Comparative Examples 1-8, the present invention employs a core-to-wall material mass ratio of 15:1-3, and a 1:1 mixture of sodium caseinate and chitosan hydrochloride as the wall material to encapsulate perilla seed oil. The resulting emulsion is adjusted to pH 7±0.1 and subjected to 4-6 high-pressure homogenization cycles. The perilla seed oil microcapsule emulsions prepared in Examples 1-6 exhibit good centrifugal stability, small and uniform particle size, and good emulsifying ability. Furthermore, they demonstrate good stability at room temperature and 4°C, with absolute Zeta potential values all above 40mV. The combined technical effect is superior to the sum of the effects of each individual technique. Attached Figure Description
[0050] Figure 1 This is a comparison chart of the centrifugation results of perilla seed oil microcapsule emulsions in Examples 1-6.
[0051] Figure 2 This is a comparative graph showing the centrifugation results of perilla seed oil microcapsule emulsions from Examples 1-7.
[0052] Figure 3 This is a comparison chart of the particle size of perilla seed oil microcapsule emulsions in Examples 1-6 and Comparative Examples 1-7.
[0053] Figure 4 This is a comparison chart of the polydispersity index (PI) of perilla seed oil microcapsule emulsions in Examples 1-6 and Comparative Examples 1-7.
[0054] Figure 5 This is a comparison graph of the zeta potentials of the perilla seed oil microcapsule emulsions of Examples 1-6 and Comparative Examples 1-7.
[0055] Figure 6 This is a comparison chart of the emulsification index (EAI) of perilla seed oil microcapsule emulsions in Examples 1-6 and Comparative Examples 1-7.
[0056] Figure 7 The diagram shows a comparison of the emulsification stability (ESI) of the perilla seed oil microcapsule emulsions in Examples 1-6 and Comparative Examples 1-7.
[0057] Figure 8 The diagram shows the state of the perilla seed oil microcapsule emulsion of Example 1 on days 1, 7, 14, and 28 under the conditions of room temperature, light, 4°C, -20°C, alternating hot and cold, and 50°C.
[0058] Figure 9 The diagram shows the state of the perilla seed oil microcapsule emulsion of Example 2 on days 1, 7, 14, and 28 under the conditions of room temperature, light, 4°C, -20°C, alternating hot and cold, and 50°C.
[0059] Figure 10 The diagram shows the state of the perilla seed oil microcapsule emulsion of Example 3 on days 1, 7, 14, and 28 under the conditions of room temperature, light, 4°C, -20°C, alternating hot and cold, and 50°C.
[0060] Figure 11 The diagram shows the state of the perilla seed oil microcapsule emulsion of Example 4 on days 1, 7, 14, and 28 under the conditions of room temperature, light, 4°C, -20°C, alternating hot and cold, and 50°C.
[0061] Figure 12 The diagram shows the state of the perilla seed oil microcapsule emulsion of Example 5 on days 1, 7, 14, and 28 under the conditions of room temperature, light, 4°C, -20°C, alternating hot and cold, and 50°C.
[0062] Figure 13 The diagram shows the state of the perilla seed oil microcapsule emulsion of Example 6 on days 1, 7, 14, and 28 under the conditions of room temperature, light, 4°C, -20°C, alternating hot and cold, and 50°C.
[0063] Figure 14 The diagram shows the state of the perilla seed oil microcapsule emulsion of Comparative Example 1 on days 1, 7, 14, and 28 under the conditions of room temperature, light, 4℃, -20℃, alternating hot and cold, and 50℃.
[0064] Figure 15 The diagram shows the state of the perilla seed oil microcapsule emulsion of Comparative Example 2 on days 1, 7, 14, and 28 under the conditions of room temperature, light, 4℃, -20℃, alternating hot and cold, and 50℃.
[0065] Figure 16 The diagram shows the state of the perilla seed oil microcapsule emulsion of Comparative Example 3 on days 1, 7, 14, and 28 under the conditions of room temperature, light, 4℃, -20℃, alternating hot and cold, and 50℃.
[0066] Figure 17The diagram shows the state of the perilla seed oil microcapsule emulsion of Comparative Example 4 on days 1, 7, 14, and 28 under the conditions of room temperature, light, 4℃, -20℃, alternating hot and cold, and 50℃.
[0067] Figure 18 The diagram shows the state of the perilla seed oil microcapsule emulsion of Comparative Example 5 on days 1, 7, 14, and 28 under the conditions of room temperature, light, 4℃, -20℃, alternating hot and cold, and 50℃.
[0068] Figure 19 The diagram shows the state of the perilla seed oil microcapsule emulsion of Comparative Example 6 on days 1, 7, 14, and 28 under the conditions of room temperature, light, 4℃, -20℃, alternating hot and cold, and 50℃.
[0069] Figure 20 The diagram shows the state of the perilla seed oil microcapsule emulsion of Comparative Example 7 on days 1, 7, 14, and 28 under the conditions of room temperature, light, 4℃, -20℃, alternating hot and cold, and 50℃.
[0070] Figure 21 This is a diagram showing the state of the perilla seed oil microcapsule emulsion of Comparative Example 8 at room temperature. Detailed Implementation
[0071] The following non-limiting embodiments are intended to enable those skilled in the art to gain a more comprehensive understanding of the present invention, but do not limit the invention in any way. The following content is merely an exemplary description of the scope of protection claimed by the present invention, and those skilled in the art can make various changes and modifications to the present invention based on the disclosed content, and such changes should also fall within the scope of protection claimed by the present invention.
[0072] The present invention will be further described below by way of specific embodiments. Unless otherwise specified, all instruments, devices, equipment, reagents, products, etc., used in the embodiments of the present invention are obtained through conventional commercial means.
[0073] Specific raw material information is shown in Table 1: Table 1. Raw Material Information
[0074] Example 1: A perilla seed oil microcapsule emulsion and its preparation process Includes the following steps: (1) Weigh 0.5g of sodium caseinate and 0.5g of chitosan hydrochloride into clean beakers, and add 41.7g of deionized water to dissolve them, to obtain solution A (protein) and solution B (polysaccharide). Seal the above solutions with plastic wrap and place them at 60℃ for 40min until completely dissolved; (2) Homogenize solution A at 10,000 rpm for 5 min using a homogenizer. Add 15 g of perilla seed oil to solution A and homogenize for 5 min. Then add solution B and continue homogenizing at 10,000 rpm for 5 min to obtain an emulsion. The homogenization process is uninterrupted. (3) Adjust the pH of the obtained emulsion to 7±0.1, and homogenize it 5 times at 800 bar using a high-pressure homogenizer. Finally, add 0.6g of PE9010 and stir evenly to obtain the perilla seed oil microcapsule emulsion.
[0075] Example 2: A perilla seed oil microcapsule emulsion and its preparation process Includes the following steps: (1) Weigh 0.5g of sodium caseinate and 0.5g of chitosan hydrochloride into clean beakers, add 39.2g of deionized water and 2.5g of glycerol respectively to dissolve them, to obtain solution A (protein) and solution B (polysaccharide). Seal the above solutions with plastic wrap and place them at 60℃ for 40min until completely dissolved; (2) Homogenize solution A at 10,000 rpm for 5 min using a homogenizer. Add 15 g of perilla seed oil to solution A and homogenize for 5 min. Then add solution B and continue homogenizing at 10,000 rpm for 5 min to obtain an emulsion. The homogenization process is uninterrupted. (3) Adjust the pH of the obtained emulsion to 7±0.1, and homogenize it 5 times at 800 bar using a high-pressure homogenizer. Finally, add 0.6g of PE9010 and stir evenly to obtain the perilla seed oil microcapsule emulsion.
[0076] Example 3: A perilla seed oil microcapsule emulsion and its preparation process Includes the following steps: (1) Weigh 0.5g of sodium caseinate and 0.5g of chitosan hydrochloride into clean beakers, add 36.7g of deionized water and 5g of glycerol respectively to dissolve them, to obtain solution A (protein) and solution B (polysaccharide). Seal the above solutions with plastic wrap and place them at 60℃ for 40min until completely dissolved.
[0077] (2) Homogenize solution A at 10,000 rpm for 5 min using a homogenizer. Add 15 g of perilla seed oil to solution A and homogenize for 5 min. Then add solution B and continue homogenizing at 10,000 rpm for 5 min to obtain an emulsion. The homogenization process is uninterrupted.
[0078] (3) Adjust the pH of the obtained emulsion to 7±0.1, and homogenize it 5 times at 800 bar using a high-pressure homogenizer. Finally, add 0.6g of PE9010 and stir evenly to obtain the perilla seed oil microcapsule emulsion.
[0079] Example 4: A perilla seed oil microcapsule emulsion and its preparation process Includes the following steps: (1) Weigh 1.5g of sodium caseinate and 1.5g of chitosan hydrochloride into clean beakers, and add 40.7g of deionized water to dissolve them to obtain solution A (protein) and solution B (polysaccharide). Seal the above solutions with plastic wrap and place them at 60℃ for 40min until completely dissolved.
[0080] (2) Homogenize solution A at 10,000 rpm for 5 min using a homogenizer. Add 15 g of perilla seed oil to solution A and homogenize for 5 min. Then add solution B and continue homogenizing at 10,000 rpm for 5 min to obtain an emulsion. The homogenization process is uninterrupted.
[0081] (3) Adjust the pH of the obtained emulsion to 7±0.1, and homogenize it 5 times at 800 bar using a high-pressure homogenizer. Finally, add 0.6g of PE9010 and stir evenly to obtain the perilla seed oil microcapsule emulsion.
[0082] Example 5: A perilla seed oil microcapsule emulsion and its preparation process Includes the following steps: (1) Weigh 1.5g of sodium caseinate and 1.5g of chitosan hydrochloride into a clean beaker, add 38.2g of deionized water and 2.5g of glycerol respectively to dissolve them, to obtain solution A (protein) and solution B (polysaccharide). Seal the above solutions with plastic wrap and place them at 60℃ for 40min until completely dissolved.
[0083] (2) Homogenize solution A at 10,000 rpm for 5 min using a homogenizer. Add 15 g of perilla seed oil to solution A and homogenize for 5 min. Then add solution B and continue homogenizing at 10,000 rpm for 5 min to obtain an emulsion. The homogenization process is uninterrupted.
[0084] (3) Adjust the pH of the obtained emulsion to 7±0.1, and homogenize it 5 times at 800 bar using a high-pressure homogenizer. Finally, add 0.6g of PE9010 and stir evenly to obtain the perilla seed oil microcapsule emulsion.
[0085] Example 6: A perilla seed oil microcapsule emulsion and its preparation process Includes the following steps: (1) Weigh 1.5g of sodium caseinate and 1.5g of chitosan hydrochloride into a clean beaker, add 35.7g of deionized water and 5g of glycerol respectively to dissolve them, to obtain solution A (protein) and solution B (polysaccharide). Seal the above solutions with plastic wrap and place them at 60℃ for 40min until completely dissolved.
[0086] (2) Homogenize solution A at 10,000 rpm for 5 min using a homogenizer. Add 15 g of perilla seed oil to solution A and homogenize for 5 min. Then add solution B and continue homogenizing at 10,000 rpm for 5 min to obtain an emulsion. The homogenization process is uninterrupted.
[0087] (3) Adjust the pH of the obtained emulsion to 7±0.1, and homogenize it 5 times at 800 bar using a high-pressure homogenizer. Finally, add 0.6g of PE9010 and stir evenly to obtain the perilla seed oil microcapsule emulsion.
[0088] Comparative Example 1: A perilla seed oil microcapsule emulsion and its preparation process The difference from Example 4 is that the amount of perilla seed oil added is replaced from 15g to 10g, and the insufficient part is made up with deionized water so that the total mass of core material, wall material and solvent is 99.4g. The pH value of the emulsion in step (3) is adjusted from 7±0.1 to 9±0.1, and the rest are the same.
[0089] Includes the following steps: (1) Weigh 1.5g each of sodium caseinate and chitosan hydrochloride into a clean beaker, and add 43.2g of deionized water to dissolve them to obtain solution A (protein) and solution B (polysaccharide). Seal the above solutions with plastic wrap and place them at 60℃ for 40min until completely dissolved.
[0090] (2) Homogenize solution A at 10,000 rpm for 5 min using a homogenizer. Add 10 g of perilla seed oil to solution A and homogenize for 5 min. Then add solution B and continue homogenizing at 10,000 rpm for 5 min to obtain an emulsion. The homogenization process is uninterrupted.
[0091] (3) Adjust the pH of the obtained emulsion to 9±0.1, and homogenize it 5 times at 800 bar using a high-pressure homogenizer. Finally, add 0.6g of PE9010 and stir evenly to obtain the perilla seed oil microcapsule emulsion.
[0092] Comparative Example 2: A perilla seed oil microcapsule emulsion and its preparation process The difference from Example 4 is that the amount of perilla seed oil added is replaced from 15g to 10g, and the insufficient part is made up with deionized water so that the total mass of core material, wall material and solvent is 99.4g. The emulsion described in step (3) is not subjected to high pressure homogenization, and the rest are the same.
[0093] Includes the following steps: (1) Weigh 1.5g each of sodium caseinate and chitosan hydrochloride into a clean beaker, and add 43.2g of deionized water to dissolve them to obtain solution A (protein) and solution B (polysaccharide). Seal the above solutions with plastic wrap and place them at 60℃ for 40min until completely dissolved.
[0094] (2) Homogenize solution A at 10,000 rpm for 5 min using a homogenizer. Add 10 g of perilla seed oil to solution A and homogenize for 5 min. Then add solution B and continue homogenizing at 10,000 rpm for 5 min to obtain an emulsion. The homogenization process is uninterrupted.
[0095] (3) Adjust the pH of the obtained emulsion to 7±0.1 without high-pressure homogenization. Finally, add 0.6g of PE9010 and stir evenly to obtain the perilla seed oil microcapsule emulsion.
[0096] Comparative Example 3: A perilla seed oil microcapsule emulsion and its preparation process The difference from Example 4 is that the amount of perilla seed oil added is replaced from 15g to 10g, and the insufficient part is made up with deionized water so that the total mass of core material, wall material and solvent is 99.4g. The number of high pressure homogenization times is replaced from 5 times to 3 times, and the rest are the same.
[0097] Includes the following steps: (1) Weigh 1.5g each of sodium caseinate and chitosan hydrochloride into a clean beaker, and add 43.2g of deionized water to dissolve them to obtain solution A (protein) and solution B (polysaccharide). Seal the above solutions with plastic wrap and place them at 60℃ for 40min until completely dissolved.
[0098] (2) Homogenize solution A at 10,000 rpm for 5 min using a homogenizer. Add 10 g of perilla seed oil to solution A and homogenize for 5 min. Then add solution B and continue homogenizing at 10,000 rpm for 5 min to obtain an emulsion. The homogenization process is uninterrupted.
[0099] (3) Adjust the pH of the obtained emulsion to 7±0.1, and homogenize it three times under high pressure at 800 bar using a high-pressure homogenizer. Finally, add 0.6g of PE9010 and stir evenly to obtain the perilla seed oil microcapsule emulsion.
[0100] Comparative Example 4: A perilla seed oil microcapsule emulsion and its preparation process The difference from Example 4 is that the amount of perilla seed oil added is replaced from 15g to 10g, and the insufficient part is made up with deionized water so that the total mass of core material, wall material and solvent is 99.4g. The number of high pressure homogenization times is replaced from 5 times to 7 times, and the rest are the same.
[0101] Includes the following steps: (1) Weigh 1.5g each of sodium caseinate and chitosan hydrochloride into a clean beaker, and add 43.2g of deionized water to dissolve them to obtain solution A (protein) and solution B (polysaccharide). Seal the above solutions with plastic wrap and place them at 60℃ for 40min until completely dissolved.
[0102] (2) Homogenize solution A at 10,000 rpm for 5 min using a homogenizer. Add 10 g of perilla seed oil to solution A and homogenize for 5 min. Then add solution B and continue homogenizing at 10,000 rpm for 5 min to obtain an emulsion. The homogenization process is uninterrupted.
[0103] (3) Adjust the pH of the obtained emulsion to 7±0.1, and homogenize it 7 times at 800 bar using a high-pressure homogenizer. Finally, add 0.6g of PE9010 and stir evenly to obtain the perilla seed oil microcapsule emulsion.
[0104] Comparative Example 5: A perilla seed oil microcapsule emulsion and its preparation process The difference from Example 4 is that the amount of sodium caseinate added is replaced from 1.5g to 2.5g, the amount of chitosan hydrochloride added is replaced from 1.5g to 2.5g, the amount of perilla seed oil added is replaced from 15g to 10g, and the amount of deionized water added is replaced from 40.7g to 42.2g. All other aspects are the same.
[0105] Includes the following steps: (1) Weigh 2.5g each of sodium caseinate and chitosan hydrochloride into a clean beaker, add 42.2g of deionized water to dissolve them, and obtain solution A (protein) and solution B (polysaccharide). Seal the above solutions with plastic wrap and place them at 60℃ for 40min until completely dissolved.
[0106] (2) Homogenize solution A at 10,000 rpm for 5 min using a homogenizer. Add 10 g of perilla seed oil to solution A and homogenize for 5 min. Then add solution B and continue homogenizing at 10,000 rpm for 5 min to obtain an emulsion. The homogenization process is uninterrupted.
[0107] (3) Adjust the pH of the obtained emulsion to 7±0.1, and homogenize it 5 times at 800 bar using a high-pressure homogenizer. Finally, add 0.6g of PE9010 and stir evenly to obtain the perilla seed oil microcapsule emulsion.
[0108] Comparative Example 6: A perilla seed oil microcapsule emulsion and its preparation process The difference from Example 4 is that the amount of sodium caseinate added is replaced by 3.5g instead of 1.5g, the amount of chitosan hydrochloride added is replaced by 3.5g instead of 1.5g, the amount of deionized water added is replaced by 41.2g instead of 40.7g, and the amount of perilla seed oil added is replaced by 10g instead of 15g. All other aspects are the same.
[0109] Includes the following steps: (1) Weigh 3.5g each of sodium caseinate and chitosan hydrochloride into a clean beaker, add 41.2g of deionized water to dissolve them, and obtain solution A (protein) and solution B (polysaccharide). Seal the above solutions with plastic wrap and place them at 60℃ for 40min until completely dissolved.
[0110] (2) Homogenize solution A at 10,000 rpm for 5 min using a homogenizer. Add 10 g of perilla seed oil to solution A and homogenize for 5 min. Then add solution B and continue homogenizing at 10,000 rpm for 5 min to obtain an emulsion. The homogenization process is uninterrupted.
[0111] (3) Adjust the pH of the obtained emulsion to 7±0.1, and homogenize it 5 times at 800 bar using a high-pressure homogenizer. Finally, add 0.6g of PE9010 and stir evenly to obtain the perilla seed oil microcapsule emulsion.
[0112] Comparative Example 7: A perilla seed oil microcapsule emulsion and its preparation process The difference from Example 4 is that the amount of sodium caseinate added is replaced by 1g instead of 1.5g, the amount of chitosan hydrochloride added is replaced by 2.0g instead of 1.5g, the amount of deionized water added is replaced by 43.2g instead of 40.7g, and the amount of perilla seed oil added is replaced by 10g instead of 15g. All other aspects are the same.
[0113] Includes the following steps: (1) Weigh 1.0 g of sodium caseinate and 2.0 g of chitosan hydrochloride into clean beakers, and add 43.2 g of deionized water to dissolve them to obtain solution A (protein) and solution B (polysaccharide). Seal the above solutions with plastic wrap and place them at 60°C for 40 min and stir until completely dissolved.
[0114] (2) Homogenize solution A at 10,000 rpm for 5 min using a homogenizer. Add 10 g of perilla seed oil to solution A and homogenize for 5 min. Then add solution B and continue homogenizing at 10,000 rpm for 5 min to obtain an emulsion. The homogenization process is uninterrupted.
[0115] (3) Adjust the pH of the obtained emulsion to 7±0.1, and homogenize it 5 times at 800 bar using a high-pressure homogenizer. Finally, add 0.6g of PE9010 and stir evenly to obtain the perilla seed oil microcapsule emulsion.
[0116] Comparative Example 8: A perilla seed oil microcapsule emulsion and its preparation process The difference from Example 4 is that the amount of sodium caseinate added is replaced from 1.5g to 2g, the amount of chitosan hydrochloride added is replaced from 1.5g to 1g, the amount of deionized water added is replaced from 40.7g to 43.2g, and the amount of perilla seed oil added is replaced from 15g to 10g. All other aspects are the same.
[0117] Includes the following steps: (1) Weigh 2.0g of sodium caseinate and 1.0g of chitosan hydrochloride into clean beakers, and add 43.2g of deionized water to dissolve them to obtain solution A (protein) and solution B (polysaccharide). Seal the above solutions with plastic wrap and stir at 60℃ for 40min until completely dissolved.
[0118] (2) Homogenize solution A at 10,000 rpm for 5 min using a homogenizer. Add 10 g of perilla seed oil to solution A and homogenize for 5 min. Then add solution B and continue homogenizing at 10,000 rpm for 5 min to obtain an emulsion. The homogenization process is uninterrupted.
[0119] (3) Adjust the pH of the obtained emulsion to 7±0.1, and homogenize it 5 times at 800 bar using a high-pressure homogenizer. Finally, add 0.6g of PE9010 and stir evenly to obtain the perilla seed oil microcapsule emulsion.
[0120] Example 1: Centrifugal stability of perilla seed oil microcapsule emulsion. Take 2 mL of the perilla seed oil microcapsule emulsions prepared in Examples 1-6 and Comparative Examples 1-7 respectively into 5 mL centrifuge tubes, and centrifuge at 25℃ and 4500 rpm for 20 min. Observe whether the emulsions in the tubes show stratification. The centrifugation results are shown in the figure. Figure 1-2 .
[0121] from Figure 1 As can be seen, the perilla seed oil microcapsule emulsions prepared in Examples 1-6 did not separate into layers after centrifugation, indicating good centrifugal stability; from Figure 1As can be seen, the perilla seed oil microcapsule emulsion of Comparative Example 2 separated into layers after centrifugation, while the emulsions of Comparative Examples 5 and 6 were viscous but did not separate into layers. This indicates that the lack of high-pressure homogenization of the emulsion in step (2) significantly affects the centrifugal stability of the perilla seed oil microcapsule emulsion, and a core-to-wall material mass ratio exceeding 15:1-3 also affects the state of the perilla seed oil microcapsule emulsion after centrifugation. Furthermore, the perilla seed oil microcapsule emulsion of Comparative Example 8 separated into layers without undergoing centrifugal stability testing after being placed at room temperature. Figure 21 As shown, the stability is poor.
[0122] Example 2: Determination of particle size, polydispersity index, and zeta potential of perilla seed oil microcapsule emulsion. The particle size, polydispersity index, and zeta potential of the perilla seed oil microcapsule emulsions of Examples 1-6 and Comparative Examples 1-7 were tested using a particle size analyzer, following the manufacturer's instructions for use. 1. Particle size and polydispersity index test: Clean the "DTS0012" sample cell, add 1 cm of sample, place the sample cell into the instrument's sample chamber, close the instrument cover, and perform the test. Results are shown below. Figure 3 .
[0123] 2. Zeta potential test: Clean the "DTS1070" sample cell, add sample to near the MAX / FULL line, shake left and right to mix the solution, place the sample cell into the instrument's sample holder, close the instrument cover, and perform the test. Results are shown in [link to test]. Figure 4 .
[0124] from Figure 3 As can be seen, the particle size of the perilla seed oil microcapsule emulsions in Examples 1-6 is smaller than that in Comparative Examples 1-7, with the particle size in Examples 1 and 3 being below 600 nm. This indicates that the pH value of the emulsion, the number of high-pressure homogenization cycles, and the mass ratio of core material to wall material all affect the particle size of the emulsion, thus increasing it.
[0125] from Figure 4 As can be seen, the polydispersity index (PDI) of the perilla seed oil microcapsule emulsions in Examples 1-6 is lower than that in Comparative Examples 1-7. The PDI of Examples 1-6 is less than 0.3, indicating relatively uniform particle size. The PDI of Comparative Examples 1 and 3-7 is less than 0.5, indicating relatively uniform particle size, but the PDI of Comparative Example 2 is above 0.7. This shows that the absence of high-pressure homogenization significantly affects the particle size and PDI of the emulsion. Furthermore, too few or too many high-pressure homogenization cycles will not achieve the optimal particle size and PDI. Additionally, a core-to-wall material mass ratio exceeding 15:1-3 will also affect the particle size and PDI of the emulsion.
[0126] from Figure 5As can be seen, the absolute values of the Zeta potential of the perilla seed oil microcapsule emulsions in Examples 1-6 and Comparative Examples 1-7 are all above 40 mV, indicating high stability. However, the Zeta potentials of Comparative Examples 3 and 4 are significantly higher than those of other groups. This may be because under these conditions, chitosan hydrochloride cations form a high-charge-density adsorption layer on the surface of the oil droplets, resulting in insufficient neutralization of positive and negative charges. This avoids the optimal ratio for protein-polysaccharide electrostatic aggregation. Considering both particle size and PI results, this condition is indeed not the preferred process.
[0127] Example 3: Determination of emulsification index and emulsification stability of perilla seed oil microcapsule emulsion. The perilla seed oil microcapsule emulsion samples from Examples 1-6 and Comparative Examples 1-7 were poured into beakers. 6 mL of the microcapsule emulsion sample was pipetted from 0.5 cm below the bottom of the beaker and mixed with 1 mL of 0.1% SDS solution. The absorbance of the sample was measured using a microplate reader at 500 nm. After 10 min, the absorbance of the emulsion was measured again after standing for 10 min using the same method. A 0.1% SDS solution was used as the blank control. The emulsification index (EAI) and emulsification stability (ESI) were calculated according to the following formulas, and the results are shown in [Figure number missing]. Figure 6-7 .
[0128]
[0129]
[0130] In the formula: The absorbance value at 0 min is... The absorbance value is given after 10 minutes, N is the dilution factor, and c is the sample concentration (g / mL). For oil phase volume, This is the optical path length.
[0131] from Figure 6 As can be seen, the emulsification index of the perilla seed oil microcapsule emulsions in Examples 1-3 is above 24 m² / g, which is superior to that of the other examples and comparative examples. The emulsification index of Examples 4-6 is relatively low, possibly because the amount of perilla seed oil added is high, and the preparation process and formulation are insufficient to fully emulsify and stabilize the system. In Comparative Example 7, reducing the amount of perilla seed oil added and increasing the proportion of wall material can improve the emulsification performance of the system accordingly. However, an excessively high proportion of wall material will lead to increased particle size and uneven dispersion, resulting in poor overall stability.
[0132] from Figure 7 As can be seen from the data, the emulsification stability of the perilla seed oil microcapsule emulsions in Examples 1-6 and Comparative Examples 1-7 is not significantly different, all being above 97%, indicating good emulsification stability.
[0133] Example 4: Stability of perilla seed oil microcapsule emulsion was tested after 28 days under the following conditions: room temperature, light exposure, 4°C, -20°C, alternating hot and cold temperatures, and 50°C. Two to three mL samples of the perilla seed oil microcapsule emulsion from Examples 1-6 and Comparative Examples 1-7 were taken and placed in six test tubes. The six test tubes were then placed in environments of room temperature, light, 4°C, -20°C, alternating hot and cold temperatures (i.e., alternating between -20°C and 50°C), and 50°C, respectively. The sample conditions were observed and recorded on days 1, 7, 14, and 28. The results are shown in the table below. Figure 8-21 .
[0134] from Figure 8-13 As can be seen, the perilla seed oil microcapsule emulsions of Examples 1-6 did not undergo significant changes at room temperature and 4℃. Under light conditions, the perilla seed oil microcapsule emulsions of Examples 1-3 did not undergo significant changes, while small water droplets appeared on the tube walls of the emulsions of Examples 4-6. Under -20℃ and alternating hot and cold conditions, the emulsion of Example 3 did not undergo significant changes, while the emulsions of Examples 1, 2, and 4-6 all separated into layers and showed clumping over time. At 50℃, the perilla seed oil microcapsule emulsions of Examples 1-6 all darkened in color over time, with the emulsions of Examples 4-6 also showing clumping over time.
[0135] from Figure 14-20 As can be seen, at room temperature and 4℃, the perilla seed oil microcapsule emulsions of Comparative Examples 1-7 did not undergo significant changes; under light conditions, the perilla seed oil microcapsule emulsions of Comparative Examples 3, 4, and 7 did not undergo significant changes, the emulsions of Comparative Examples 1 and 2 showed small lumps, while the emulsions of Comparative Examples 5 and 6 gradually solidified over time; under -20℃, alternating hot and cold conditions, and 50℃ conditions, the perilla seed oil microcapsule emulsions of Comparative Examples 1-7 all darkened in color and separated into layers over time, and lumps appeared.
[0136] Therefore, the perilla seed oil microcapsule emulsions of Examples 1-6 and Comparative Examples 1-7 were stable at room temperature and 4°C, but the stability of the emulsion of Examples 1-6 was better than that of Comparative Examples 1-7 under light conditions. The emulsion of Example 3 had the best stability, showing no significant changes under room temperature, light, 4°C, -20°C, and alternating hot and cold conditions; the emulsion at 50°C only darkened in color over time. This indicates that adding a certain proportion of glycerol as a solution can increase the stability of the emulsion.
[0137] Verification of technical effectiveness and / or analysis of solutions to technical problems: from Figure 1-7It can be seen that by using a core material to wall material mass ratio of 15:1-3, and a 1:1 mixture of sodium caseinate and chitosan hydrochloride as the wall material to encapsulate perilla seed oil, the pH of the resulting emulsion was adjusted to 7±0.1 and subjected to 4-6 high-pressure homogenization cycles. The perilla seed oil microcapsule emulsions prepared in Examples 1-6 have good centrifugal stability, small and uniform particle size, and good emulsification ability. Furthermore, they exhibit good stability at room temperature and 4℃, with absolute Zeta potential values all above 40mV, which is beneficial for better storage and application of perilla seed oil.
[0138] Finally, it should be noted that the above content is only used to illustrate the technical solution of the present invention, and is not intended to limit the scope of protection of the present invention. Simple modifications or equivalent substitutions made by those skilled in the art to the technical solution of the present invention do not depart from the essence and scope of the technical solution of the present invention.
Claims
1. A perilla seed oil microcapsule emulsion, characterized in that, It includes a core material and a wall material; the core material is perilla seed oil, and the wall material is sodium caseinate and chitosan salts; the mass ratio of the core material to the wall material is 15:1-3.
2. The perilla seed oil microcapsule emulsion according to claim 1, characterized in that, The chitosan salts mentioned include one of chitosan hydrochloride, chitosan quaternary ammonium salt, chitosan lactate, and chitosan glutamate.
3. The perilla seed oil microcapsule emulsion according to claim 2, characterized in that, The chitosan salt is chitosan hydrochloride, and the mass ratio of sodium caseinate to chitosan hydrochloride is 1:
1.
4. The perilla seed oil microcapsule emulsion according to claim 1, characterized in that, The mass ratio of the core material to the wall material is 15:1-2.
5. The preparation process of the perilla seed oil microcapsule emulsion according to any one of claims 1-4, characterized in that, Includes the following steps: (1) Add sodium caseinate to a solvent and stir until it is completely dissolved to obtain solution A. Add chitosan hydrochloride to a solvent and stir until it is completely dissolved to obtain solution B. (2) Homogenize solution A once, add perilla seed oil and homogenize a second time, and finally add solution B and homogenize a third time to obtain an emulsion. (3) The emulsion is homogenized under high pressure, preservatives are added, and the mixture is stirred evenly to obtain the perilla seed oil microcapsule emulsion.
6. The preparation process according to claim 5, characterized in that, The solvent is water and / or glycerol, and the amount of glycerol added is 0-13% of the mass of the solvent.
7. The preparation process according to claim 5, characterized in that, The mass ratio of sodium caseinate to solvent is 0.5-1.5:40-42, and the mass ratio of chitosan hydrochloride to solvent is 0.5-1.5:40-42.
8. The preparation process according to claim 5, characterized in that, In step (2), the rotation speed for the first homogenization, the second homogenization and the third homogenization are all 8000-10000 rpm and the time is 5-10 min.
9. The preparation process according to claim 5, characterized in that, The pH value of the emulsion described in step (2) is 7±0.
1.
10. The preparation process according to claim 5, characterized in that, The pressure of high-pressure homogenization in step (3) is 600-800 bar, and the number of homogenization cycles is 4-6.
Citation Information
Patent Citations
CN111436500A