Manufacturing method of double matrix capsule
The double matrix capsule method stabilizes high concentrations of active ingredients and enhances skin absorption by encapsulating them in a liquid crystal and polymer matrix, addressing the limitations of existing cosmetic encapsulation methods.
Patent Information
- Authority / Receiving Office
- KR · KR
- Patent Type
- Patents
- Current Assignee / Owner
- SUANN HANGJANG
- Filing Date
- 2022-07-28
- Publication Date
- 2026-07-27
AI Technical Summary
Existing methods for stabilizing active ingredients in cosmetics face challenges in maintaining high concentrations over time and facilitating skin absorption, as they often fail to encapsulate large amounts effectively and are prone to instability.
A method for manufacturing a double matrix capsule involving an oil-in-water type liquid crystal emulsion with a multilayer lamellar structure, encapsulating active ingredients within liquid crystal nanoparticles, followed by a secondary encapsulation in a polymer matrix to form a double matrix capsule.
The double matrix capsule provides enhanced stability and effective transdermal absorption of active ingredients, maintaining their efficacy over a long period while ensuring aesthetically pleasing appearances.
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Figure 112022079081700-PAT00001_ABST
Abstract
Description
Technology Field
[0001] The present invention relates to a method for manufacturing a double matrix capsule that facilitates transdermal absorption while increasing stability. Background Technology
[0002] Generally, unlike food, cosmetics require long-term use, making it of paramount importance to ensure stability. Recently, the cosmetics industry has seen numerous applications incorporating capsules or beads into containers or contents to express beauty and enhance quality.
[0003] In addition, for cosmetics, unstable active ingredients that are difficult to maintain stability for a long period of time are stabilized by simply adding a stabilizer, encapsulating them in multiple emulsions, developing special containers, or simply encapsulating them in vesicles such as liposomes.
[0004] However, these methods do not encapsulate a large amount of active ingredients and have limitations in ensuring excellent stability. Recently, methods have been developed to stabilize active ingredients by forming them into bead-shaped granules or to differentiate their appearance by using them in combination with pigments, which are being commercialized. Additionally, encapsulation methods utilizing simple monomer forms with a polymer matrix are also being introduced.
[0005] However, these methods are used merely for cosmetic purposes, and they face difficulties in stabilizing high concentrations of active ingredients and have limitations in absorbing the drug into the skin due to changes over time. Prior art literature
[0006] Patent Document 1: Republic of Korea Registered Patent 10-0115074 Patent Document 2: Republic of Korea Registered Patent 10-0837558 Patent Document 3: Republic of Korea Registered Patent 10-0173445 Patent Document 4: Republic of Korea Registered Patent 10-0799407 Patent Document 5: Republic of Korea Registered Patent 10-0825834 Patent Document 6: Republic of Korea Registered Patent 10-0544443 Patent Document 7: Republic of Korea Registered Patent 10-1032623 Patent Document 8: Republic of Korea Registered Patent 10-1192161 Patent Document 9: Republic of Korea Registered Patent 10-1281527 Patent Document 10: Republic of Korea Registered Patent 10-1484836 The problem to be solved
[0007] In order to solve the problems of the prior art as described above, the present invention provides a method for manufacturing a double matrix capsule capable of stabilizing a high concentration of active ingredients and absorbing the drug into the skin over time.
[0008] By providing a stable spherical capsule through a material and optimal composition that forms a double matrix capsule, it is possible to stably encapsulate an effective drug. means of solving the problem
[0009] The method for manufacturing a double matrix capsule according to the present invention is,
[0010] A step for providing an oil component to prepare an oil component;
[0011] A water component provision step for preparing water components;
[0012] A first mixing step of mixing the above oil phase component and the above water phase component;
[0013] A step of providing an active ingredient to prepare a first mixed solution by mixing an active ingredient into the mixture after the first mixing step;
[0014] A first encapsulation step of passing the above-mentioned first mixed solution through a nanomixer at a high pressure of 100 to 1000 bar to form an oil-in-water type liquid crystal emulsion comprising nanoparticles having a multilayer lamellar liquid crystal structure in which the active ingredient is trapped inside;
[0015] A second mixing step of preparing a second mixed solution by mixing the liquid crystal emulsion and an aqueous polymer solution in which a polymer is dissolved; and
[0016] The method is characterized by including a secondary encapsulation step of passing the second mixed solution through a nozzle and dropping it to obtain a double matrix capsule particle having a polymer matrix containing nanoparticles of the liquid crystal structure inside.
[0017] At this time, it is preferable that the size of the double matrix capsule particles be 0.1㎛ to 5mm.
[0018] In addition, it is preferable that the above oil component includes a surfactant for forming a primary capsule, a polyalcohol, and an oil component.
[0019] In addition, it is desirable that the above aqueous components include purified water, a thickening agent, a skin irritation-relieving ingredient, a skin moisturizing ingredient, a preservative ingredient, etc.
[0020] In addition, the active ingredient may be one or more substances selected from the group consisting of GHK-Cu, AHK-Cu, fisetin, quercetin, idebenone, vitamins, resveratrol, caffeine, adenosine, cordycepin, niacinamide, and genistein.
[0021] In addition, it is preferable that the polymer is PEG-240 / HDI copolymer bis-decyltetradeceth-20 ether. Effects of the invention
[0023] A cosmetic composition having a double matrix capsule according to the present invention can significantly increase the long-term preservation stability of active ingredients and can have an aesthetically pleasing appearance, and active ingredients, such as GHK-Cu, AHK-Cu, fisetin, quercetin, idebenone, vitamins, resveratrol, caffeine, adenosine, cordycepin, niacinamide, and genistein, can be stably encapsulated in the center of liquid crystal nanoparticles in an oil-in-water structure so that the stabilization can be maintained for a long period.
[0024] In addition, liquid crystal nanoparticles are encapsulated in a polymer matrix to provide double-encapsulation and stabilization, and this is used to maximize efficacy and ensure an aesthetically pleasing appearance. Brief explanation of the drawing
[0025] FIG. 1 is a flowchart illustrating a method for manufacturing a double matrix capsule according to one embodiment of the present invention. FIG. 2 is a structural diagram of a double matrix capsule according to one embodiment of the present invention. FIG. 3 is a structural diagram showing the state in which an active ingredient is encapsulated in a nanoparticle of a multilayer lamellar structure according to one embodiment of the present invention. Figure 4 is a photograph of Example 3 of the present invention observed with a polarizing microscope. Figure 5 is a photograph of a double matrix capsule after manufacturing according to one embodiment of the present invention. Figure 6 is a graph showing the results of skin moisturizing power for a cosmetic composition capable of double matrix encapsulation according to one embodiment of the present invention. Figure 7 is a schematic diagram of transdermal absorption of a double matrix encapsulated sample according to the examples. FIG. 8 is a graph showing the transdermal absorption effect of a cosmetic composition capable of double matrix encapsulation according to one embodiment of the present invention. FIG. 9 is a graph showing the stability results for a cosmetic composition capable of double matrix encapsulation according to one embodiment of the present invention. Specific details for implementing the invention
[0026] The present invention is capable of various modifications and may have various embodiments. Specific embodiments are illustrated in the drawings and described in detail. However, this is not intended to limit the present invention to specific embodiments, but should be understood to include all modifications, equivalents, and substitutions that fall within the technical spirit and scope of the present invention. The invention may be modified in various other forms, and the scope of the present invention is not limited to the following embodiments. Hereinafter, embodiments according to the present invention will be described in detail with reference to the attached drawings. Identical or corresponding components are assigned the same reference numerals regardless of the drawing symbols, and redundant descriptions thereof will be omitted.
[0027] The present invention is susceptible to various modifications and may have various embodiments; therefore, specific embodiments are illustrated in the drawings and described in detail. However, this is not intended to limit the present invention to specific embodiments, but should be understood to include all modifications, equivalents, and substitutions that fall within the technical spirit and scope of the present invention, and may be modified in various other forms. Furthermore, the scope of the present invention is not limited to the following embodiments. Additionally, the definitions of major loanwords used in the present invention are expressed as follows to clarify understanding.
[0028] A method for manufacturing a double matrix capsule according to one aspect of the present invention comprises: a step of providing an oil phase component; a step of providing an aqueous phase component; a first mixing step; a step of providing an active ingredient; a first encapsulation step; a second mixing step; a second encapsulation step; and a washing step. FIG. 1 is a flowchart illustrating a double matrix encapsulation method according to an embodiment of the present invention.
[0029] The oil phase provision step is a step of preparing the oil phase components used in the manufacture of the double-matrix capsule. In this embodiment, the oil phase components include a surfactant, a polyhydric alcohol, and an oil component for forming the primary capsule. The oil phase components are heated and melted to 75 to 90°C and well dispersed by stirring with a disperser at 500 to 1500 rpm for 10 to 20 minutes.
[0030] The oil phase components are, for example, sucrose polycotton seed date, polyglyceryl-10 behenate / eicosadioate, cetearyl alcohol, and lotus flower wax.
[0031] The aqueous component provision step is a step of preparing an aqueous component for forming an oil-in-water type emulsion, wherein the aqueous component includes purified water, a thickening agent, a skin irritation-reducing ingredient, a skin moisturizing ingredient, a preservative ingredient, etc. The aqueous component is heated and dissolved at 75 to 85 ℃ for 5 to 10 minutes while stirring at 800 to 1200 rpm. Examples of the aqueous components are glycerol, purified water, 1,2-hexanediol, and ethylhexylglycerin.
[0032] The first mixing step is a step of mixing the oil phase component and the water phase component. The oil phase component can be slowly added to the water phase component and mixed using a homomixer. The oil phase component and the water phase component are mixed in a ratio of 1:7 or 1:5, and stirred with a homomixer at 1000 to 4600 rpm for 2 to 10 minutes at 75 to 85 ℃.
[0033] The active ingredient provision step is a step of preparing a first mixed solution by mixing the active ingredient into the mixture of the oil phase component and the water phase component of the aforementioned mixing step. The active ingredient is cooled to 45 to 60°C, the active ingredient is added, and the mixture is stirred at 2,000 to 4,000 rpm for 2 to 5 minutes.
[0034] The active ingredient can be either water-soluble or oil-soluble. For example, the active ingredient may be one or more substances selected from the group consisting of GHK-Cu, AHK-Cu, fisetin, quercetin, idebenone, vitamins, resveratrol, caffeine, adenosine, cordycepin, niacinamide, and genistein.
[0035] Here, GHK-Cu, also referred to as copper peptide-1, refers to a compound in which copper ions are bound to a structure composed of the amino acids glycine, histidine, and lysine to form a complex, and AHK-Cu, also referred to as copper peptide-3, refers to a compound in which copper ions are bound to a structure composed of the amino acids alanine, histidine, and lysine to form a complex. These are commonly known as drugs effective in preventing hair loss and are active ingredients known as anti-aging components in hair care and skincare cosmetics.
[0036] The first encapsulation step is a step of nano-forming by passing the first mixed solution containing the active ingredient through a high-pressure nanomixer at 100 to 1000 bar. The liquid crystal nanoparticles generated at this time are of the oil-in-water type (O / W type) and have a lamellar liquid crystal structure, in which the active ingredient is trapped inside, and the average particle size is 10 to 500 nm.
[0037] FIG. 3 is a structural diagram showing the state in which an active ingredient is encapsulated in a nanoparticle with a multilayer lamellar structure according to one embodiment of the present invention, illustrating that a hydrophilic active ingredient and a lipophilic active ingredient are encapsulated in the hydrophilic region and the lipophilic region within the multilayer lamellar structure. In addition, the nanoparticle with a multilayer lamellar structure forms an aqueous-water type liquid crystal emulsion, so that the outer layer is formed as an aqueous phase, and an aqueous-water type particle is dispersed therein.
[0038] The resulting oil-in-water (O / W) liquid crystal emulsion can be formed, for example, by mixing 0.1 to 10 weight% of sucrose polycotton citrate, 0.5 to 8 weight% of polyglyceryl-10 behenate / eicosadioate, 0.1 to 12 weight% of cetearyl alcohol, 0.01 to 3 weight% of lotus flower wax, 0.1 to 45 weight% of glycerin, and 1 to 70 weight% of purified water, based on the total weight of the liquid crystal emulsion.
[0039] At this time, for example, based on the total weight of the liquid crystal emulsion, one or more of the following may be encapsulated as active ingredients in the single O / W liquid crystal emulsion: 0.001 to 3 weight% GHK-Cu, 0.001 to 1 weight% AHK-Cu, 3 weight% fisetin, 2 weight% quercetin, 2 weight% idebenone, 0.001 to 5 weight% vitamins (retinol, ascorbic acid, tocopherol), 1 weight% resveratrol, 1 weight% caffeine, 1 weight% adenosine, 1 weight% cordycepin, 3 weight% niacinamide, and 2 weight% genistein.
[0040] The second mixing step is a step of mixing the liquid crystal emulsion prepared in the aforementioned step with the aqueous polymer solution in which the polymer is dissolved. A polymer undergoing aqueous gelation is weighed, added to purified water, heated to 50 to 60°C, and stirred well with a disperser mixer at 1,000 to 2,000 rpm for 7 to 12 minutes to make a polymer solution. Next, this is cooled to 60°C to 40°C, added to the liquid crystal emulsion, and stirred at 1,000 to 2,000 rpm with a homomixer at a pH of 4.5 to 7.5 to stably disperse it to prepare the second mixed solution.
[0041] The polymer used at this time may be, for example, PEG-240 / HDI copolymer bis-decyltetradeceth-20 ether, as a polymer that undergoes aqueous gelation. It is preferable that the polymer be included in an amount of 0.05 to 1 weight% of the secondary encapsulated emulsion solution.
[0042] In addition, the second mixed solution contains a surfactant. There are no limitations on the surfactant, but it is preferable to use a mixture of polyglyceryl-10 stearate and polyglyceryl-10 oleate. It is preferable that the surfactant be included in an amount of 0.1 to 7 weight%, preferably 0.5 to 5 weight%, of the secondary encapsulated emulsion solution.
[0043] In addition, the second mixed solution may further include fragrance, glycerin, butylene glycol, PEG-240 / HDI copolymer bis-decyltetradeceth-20 ether, hydrolyzed collagen or agar, etc., and the collagen may be hydrolyzed collagen, etc., and purified water is included in an amount of 30% to 80% by weight.
[0044] More specifically, a composition is provided in which the final material is composed of 0.05 to 0.3 weight% of PEG-240 / HDI copolymer bis-decyltetradeceth-20 ether, 0.05 to 0.2 weight% of hydrolyzed collagen, or 0.1 to 3 weight% of agar, either as a single or mixed component, and is characterized in that the final material forms a spherical matrix capsule like a granule.
[0045] The second encapsulation step is a step of obtaining granule-type double matrix capsule particles by passing the second mixed solution through a nozzle and dropping it. In addition, natural pigments can be added to the double matrix capsule particles to make the appearance have various colors.
[0046] When the second mixed solution is passed through a nozzle with an inner diameter of 0.1 to 15 mm and the solution passing through the nozzle is dropped downward through an oil layer, the mixed solution solidifies and double matrix capsule particles are formed.
[0047] At this time, particles of various sizes can be produced depending on the size of the nozzle. When passing through an oil layer, a process to clean off the adhering oil may be included.
[0048] That is, in the second encapsulation step, the liquid crystal nanoparticles that were first encapsulated are secondarily encapsulated in a polymer matrix to form a double matrix capsule structure. Figure 2 illustrates double matrix capsule particles after the second encapsulation step, in which a single liquid crystal emulsion is enclosed within a polymer matrix. At this time, the size of the double matrix capsule particles is in the form of granules ranging from 0.1 µm to 5 mm.
[0049] The double matrix capsule functions to stably preserve the single capsule inside, and when applied to the skin, it has the advantage of spreading smoothly and being quickly absorbed.
[0050] Therefore, the double matrix capsule can be absorbed into the skin by gently breaking when rubbed by hand or discharged through a pump. It may be characterized by a nozzle with an inner diameter of 0.1 to 15 mm and the contents passing through the nozzle settling into the lower layer through an oil layer and solidifying.
[0051] In the second encapsulation step, a cleaning step may be further included to clean the oil adhering to the double matrix capsule particles when they pass through the oil layer during dropping.
[0052] The product obtained in this way has excellent long-term stability and allows for more effective transdermal absorption. Furthermore, through expanded application, it can be used in basic cosmetics, color cosmetics, and hair care products to create various formulations that provide a luxurious feel by producing beautiful and diverse colors in appearance, and offer a soft and moisturizing sensation in terms of user experience.
[0053] <Example>
[0054] <Example 1> Preparation of a monolithic O / W nano liquid crystal emulsion
[0055] The oil phase component is weighed, heated and dissolved, and thoroughly dispersed using a disperser mixer while stirring for at least 10 minutes (500–1500 rpm). Next, the aqueous phase component is weighed, heated and dissolved, and dispersed while stirring (800–1200 rpm). Then, the oil phase component is slowly added to the aqueous phase component and stirred using a homomixer at 1000–4000 rpm for 5 minutes. Next, the mixture is cooled to 50°C, the active ingredient is added, and the mixture is stirred at 2000–4000 rpm for 3 minutes. Finally, the mixture is passed through a high-pressure nanocell to form nano liquid crystal particles. The manufacturing process is completed after vacuum degassing. The content of each component used is summarized in Table 1.
[0056] <Examples 2 to 10>
[0057] Except for the difference in content between Table 1 and Table 2, it was prepared in the same manner as Example 1. Examples 6 to 10 contained only one substance as the active ingredient.
[0058] division Ingredients (Weight%) Example 1 Example 2 Example 3 Example 4 Example 5 Yoo Sang-bu Sucrose polycotton seedate polyglyceryl-10 behenate / eicosadioate cetearyl alcohol lotus wax 1253 21.553 3153 40.553 50.153 Awards Division Glycerol purified water 1,2-hexanediol ethylhexylglycerin 4033.8120.1 3043.9020.1 2051.9020.1 1053.9020.1 541.7720.1 Active ingredient GHK-CuAHK-Cu Pisetin Quercetin Idebenone Vitamins Resveratrol Caffeine Adenosine Cordycepin Niacinamide Genistein 0.010.015530.010.010.010.010.010.010.01 0.50.53320.50.50.50.50.50.50.5 112211111111 551112110.5121 10100.010.010.013221253 subtotal 100 100 100 100 100 result Underwater type Underwater type Underwater type Underwater type Underwater type
[0059] division Ingredients (Weight%) Example 6 Example 7 Example 8 Example 9 Example 10 Yoo Sang-bu Sucrose Polycotton Seedate Polyglyceryl-10 Behenate / Eicosadioate Cetearyl Alcohol Lotus Wax Scarpylic / Capric Triglyceride 32535 32535 32535 32535 32535 Awards Division Glycerol purified water 1,2-hexanediol ethylhexylglycerin 3048.920.1 3048.920.1 3048.920.1 3048.920.1 3048.920.1 Active ingredient GHK-CuAHK-CuPisetinQuercetinIdebenone 1---- -1--- --1-- ---1- ----1 subtotal 100 100 100 100 100 result Underwater type Underwater type Underwater type Underwater type Underwater type
[0060] <Examples 11 to 15>
[0061] First, a polymer solution was prepared by thoroughly dissolving fragrance, glycerin, butylene glycol, PEG-240 / HDI copolymer bis-decyltetradeceth-20 ether, hydrolyzed collagen, and agar in purified water with the composition as shown in Table 3. Double matrix encapsulation was carried out by mixing Example 3 of Table 1 into the prepared polymer solution and stirring thoroughly.
[0062] division Ingredients (Weight%) Example 11 Example 12 Example 13 Example 14 Example 15 premier Solubil ORG-1300 Flavoring Glycerin Butylene Glycol PEG-240 / HDI Copolymer Bis-Decyltetradeces-20 Ether Hydrolyzed Collagen Aga Jeongsan Water 0.50.1380.10.20.267.9 10.1280.10.20.558.1 1.50.1380.10.20.846.3 30.1480.10.2133.6 50.1580.10.2378.6 adding Example 3 of Table 1 20 30 50 60 - subtotal 100 100 100 100 100 result underwater type capsule underwater type capsule underwater type capsule underwater type capsule underwater type capsule * Solubil ORG-1300: Polygleceryl-10 Stearate & Polygleceryl-10 Oleate 50:50 mixture.
[0063] Meanwhile, FIG. 5 is a photograph of the aforementioned embodiments manufactured into granule-type capsules with sizes of 1 mm and 3 mm. As such, it exists in the form of double-encapsulated granules and is the final finished product intended to be achieved in the present invention. This can be applied to various formulations such as skin toners, lotions, essences, creams, foundations, and sunblock creams, and can also be applied to hair products such as shampoos, conditioners, ampoules, and hair dyes.
[0064] Prescription Example
[0065] <Prescription Examples 1~3> Essence
[0066] Weigh the aqueous solution and heat it to 50~60℃ to dissolve it. Cool this to 40℃ or below, and mix and stir Addition 1 into it. Add a neutralizing agent to this and mix. Add Addition 2 to this and mix.
[0067] division Ingredients (Weight%) Prescription Example 1 Prescription Example 2 Prescription Example 3 premier Solubil ORG-1300 Glycerin Butylene Glycol Dipropylene Glycol EDTA-2Na Allantoin Carbomer-941 (2% solution) Purified Water 15530.020.11075.08 15530.020.11075.08 15530.020.11065.08 Addition 1 Purslane extract Centella asiatica extract 5- -5 55 Chinese Arginine 10% Solution Purified Water 12 12 12 Addition 2 Example 12 Example 18 0.20.3 0.20.3 0.20.3 subtotal 100 100 100 result Capsule essence Capsule essence Capsule essence
[0068] <Prescription Examples 1~3> Cream
[0069] Weigh the aqueous phase and heat it to 80–90°C to dissolve it. Weigh the oil phase and heat it to 80–90°C to dissolve it. Mix these and stir with a homomixer. Add a neutralizing agent and stir. Cool to 30°C and add additives. Degas the mixture to complete the manufacturing process.
[0070] division Ingredients (Weight%) Prescription Example 1 Prescription Example 2 Prescription Example 3 premier Solubil ORG-1300 Glycerin Butylene Glycol Dipropylene Glycol EDTA-2Na Allantoin Carbomer-940 (2% solution) Purified Water 15530.020.120to 100 15530.020.110to 100 15530.020.110to 100 paid Cetearyl alcohol, shea butter, microcrystalline wax, Solubil ORG-1300, glyceryl monostearate, cetyl ethylhexanoate, vegetable squalant, ethylhexanoin 32151353 32151353 32151353 Chinese Arginine 10% Solution Purified Water 22 22 22 adding Example 12 Example 13 10- -10 55 subtotal 100 100 100 result Capsule cream Capsule cream Capsule cream
[0072] <Prescription Example: Shampoo>
[0073] division Ingredients (Weight%) Prescription Example 1 Prescription Example 2 Prescription Example 3 premier Purified water Polytüternium-10 50.30.25 50.30.25 50.30.25 Glycerin, Guar, Hydroxypropyltrimonium Chloride, Disodium EDTA, Betaine, Panthenol 20.250.050.250.2 20.250.050.250.2 20.250.050.250.2 adding Sodium C14-16 olefin sulfonate, coco-betaine cocamide, mipapropylene glycol urate 22200.250.55 22200.250.55 22200.250.55 adding Sodium hyaluronate 0.1 0.1 0.1 adding Citric acid (10% solution) 1 1 1 adding 1,2-HexanediolCaprylylGlycol 0.90.3 0.90.3 0.90.3 adding spices 0.6 0.6 0.6 adding Example 16 Example 17 10 01 0.50.5 subtotal 100 100 100 result Viscous gel Viscous gel Viscous gel
[0075] <Prescription Example: Rinse>
[0076] division Ingredients (Weight%) Prescription Example 1 Prescription Example 2 Prescription Example 3 premier Purified water, disodium EDTA, propylene glycol, panthenol, betaine, cetrimonium chloride 70.950.0520.213 70.950.0520.213 70.950.0520.213 paid Stearamidopropyl dimethylamine cetyl alcohol cyclopentasiloxane steartrimonium chloride behentrimonium chloride 1.56.52.521 1.56.52.521 1.56.52.521 adding Amodimethicone Hydrolyzed Collagen 42.7 42.7 42.7 adding 1,2-HexanediolCaprylylGlycol 0.50.3 0.50.3 0.50.3 adding spices 0.8 0.8 0.8 adding Example 12 Example 13 10 01 0.50.5 subtotal 100 100 100 result milky white cream milky white cream milky white cream
[0078] <Prescription Example: Hair Loss Prevention Ampoule>
[0079] division Ingredients (Weight%) Prescription Example 1 Prescription Example 2 Prescription Example 3 premier Purified Water PEG-75, Lanolin, Allantoin, Butylene Glycol, Panthenol, Cyclodextrin, Sodium Guaiazulene Sulfonate & Gardenia Extract, Arginine 82.240.30.120.20.20.050.31 82.240.30.120.20.20.050.31 82.240.30.120.20.20.050.31 adding Ethanol Menthol Salicylic Acid Triethyl Citrate 50.30.251 50.30.251 50.30.251 adding Ethanol PEG-60 Hydrogenated Castor Oil Butylene Glycol Fragrance 50.30.251 50.30.251 50.30.251 adding 1,2-hexanediol 0.5 0.5 0.5 Example 12 Example 13 10 01 0.50.5 subtotal 100 100 100 result Light green transparent liquid Light green transparent liquid Light green transparent liquid
[0080] <Experimental Example>
[0081] <Experimental Example 1> Analysis of Underwater Particle Structure
[0082] Figure 4 shows the results of observing particles using a polarizing microscope with Example 3. The shape of the particle diameter was observed by attaching an objective lens capable of 1,000x magnification to the polarizing microscope. According to Figure 4, it can be seen that a cross-shaped structure is formed inside the white, round particles, which means that a multi-lamellar structure is formed. This can be used as a method to increase stability by encapsulating various drugs inside.
[0084] <Experimental Example 2> Evaluation of Long-term Stability of Dual Polymer Matrix Capsules
[0085] Table 5 is a graph showing the results of measuring long-term stability by encapsulating 2% fisetin inside a double polymer matrix capsule. All three samples contained 2% fisetin, and stability was observed under the same conditions. The results are the quantitative analysis results by HPLC after 30 days in a 45°C incubator of Example 18 containing 2% fisetin in a double-encapsulated water-in-oil type, Comparative Example 1 containing 2% unencapsulated fisetin, and Comparative Example 2 containing a single liquid crystal emulsion sample.
[0086] division Ingredient Name (Weight%) Comparative Example 1 Comparative Example 2 Example 18 Water type (non-capsule) Non-capsule Fisetin 2% - - Water-in-water type (single capsule) Capsule using Example 13 - Single-layer liquid crystal capsule fisetin 2% - Double Matrix Capsule Triple matrix capsule using Example 13 - - Double-matrix capsules, fisetin 2% subtotal 100 100 100 Appearance (45℃ incubation, after 4 weeks) discolored discolored stability Appearance (after 4 weeks of 45℃ incubation) Viscosity also decreased Viscosity also decreased Good Quantitative analysis (45℃ incubation, after 4 weeks) 0.68% 1.12% 1.95% Overall results error error Good
[0087] In the case of Comparative Examples 1, 2, and 18, the content was the same at 2% immediately after preparation. In the case of Comparative Examples 1 and 2, stability decreased sharply after 4 weeks, with residual amounts of fisetin appearing as 34% and 56%, respectively. On the other hand, in the case of 18 of the present invention, the content of fisetin was 2% immediately after preparation, and after 4 weeks, the content was 1.95%, showing a residual amount of 97.5%. Based on these results, the double matrix encapsulated composition showed significantly superior stability compared to the non-capsulated and single-encapsulated compositions.
[0088] <Experimental Example 3> Evaluation of General O / W Emulsion
[0089] Comparative Examples 3 to 7 were presented to experimentally demonstrate the performance differences between general emulsions and double capsules and to provide a more convincing explanation of the performance differences. Accordingly, the oil phase was weighed, heated and dissolved, and well dispersed by stirring with a disperser mixer at 500–1500 rpm for 10 minutes. The aqueous phase was heated and dissolved, and the oil phase was slowly added to the aqueous phase and stirred with a homomixer at 4000 rpm for 5 minutes. Then, a neutralizing agent was added and stirred with a homomixer at 4000 rpm for 5 minutes. Afterward, the mixture was cooled to 50°C, the active ingredient was added and stirred at 4000 rpm for 2 minutes, and then cooled to 30°C and vacuum degassing was performed to complete the preparation of Comparative Examples 3 to 7.
[0090] Here, the most commonly used polysorbate-60 and PEG-60 hydrogenated castor oil were applied. The appearance of Comparative Example 4 was a high-viscosity cream, with a pH of 5.8 and a specific gravity of 0.998. The average size of the emulsion particles was 8.9 μm.
[0091] division Ingredients (Weight%) Comparative Example 3 Comparative Example 4 Comparative Example 5 Comparative Example 6 Comparative Example 7 Yoo Sang-bu Caprylic / Capric Triglyceride Hydrogenated Polydecene Cetearyl Alcohol Microcrystalline Wax Polysorbate-60 PEG-60 Hydrogenated Castor Oil 553232 553232 553232 553232 553232 Awards Division Glycerol, Dipropylene Glycol, 1,2-Hexanediol, Ethylhexylglycerin, Carbomer-940 (2% solution), Purified Water 7320.11545.4 7320.11545.4 7320.11545.4 7320.11545.4 7320.11545.4 Chinese Arginine 10% Solution Purified Water 1.55 1.55 1.55 1.55 1.55 Active ingredient GHK-CuAHK-CuPisetinQuercetinCordycepin 1---- -1--- --1-- ---1- ----1 subtotal 100 100 100 100 100 result General oil painting General oil painting General oil painting General oil painting General oil painting
[0092] <Experimental Example 4> Evaluation of Moisturizing Power
[0093] Figure 6 is a graph showing the skin moisturizing ability evaluation. The moisturizing ability evaluation was conducted on 20 men and women aged 20 to 50 using a moisturizing ability meter. The difference in moisturizing ability was measured using Comparative Example 4 and Example 17. It was observed that immediately after application, both samples showed a rapid increase to the 58% range. In the case of Comparative Example 4, it was found that the moisturizing ability decreased rapidly over time, dropping to a level similar to that before application. However, in the case of Example 17, it showed an effect approximately five times superior to before application, reaching 25.8% after 4 hours, 21.6% after 6 hours, and 15.8% after 8 hours.
[0094] <Experimental Example 5> Evaluation of Transdermal Absorption
[0095] Figure 7 is a schematic diagram of the transdermal absorption of a double matrix encapsulated sample according to the embodiments. According to this, the embodiments have many advantages in cosmetic dermatology because they facilitate transdermal absorption. It is an example where the advantages include ensuring long-term stability of the active ingredient, expressing a beautiful appearance, and enabling rapid skin absorption so that efficacy can be achieved with a small amount.
[0096] Figure 8 is a graph showing the transdermal absorption experiment through the examples. The evaluation of transdermal absorption was performed by applying a sample to artificial skin using a French cell, sampling over a period of up to 10 hours, and measuring the extent of transdermal absorption through HPLC quantitative analysis. The drug used as the measurement indicator was AHK-Cu, which was quantitatively analyzed and expressed as a percentage. Comparative Example 4 showed an absorption rate of 0.05% after 1 hour and 1.28% after 10 hours. On the other hand, Example 17 showed an absorption rate of 1.96% after 1 hour and 9.52% after 10 hours. This is interpreted as general emulsions being unable to penetrate the artificial skin layer due to their large and coarse particle size, whereas Example 17 is interpreted as the single liquid crystal particles released when the double capsule breaks smoothly forming nanoparticles, allowing them to easily penetrate the artificial skin.
[0097] <Experimental Example 6> Evaluation of Stability of Double Capsules
[0098] Figure 9 is a graph evaluating the stability of the double capsule. For Comparative Example 4, the single capsule of Example 7, and the double capsule of Example 13, samples stored in a 45°C incubator for 3 months were analyzed for residual amounts via HPLC quantitative analysis, and stability was measured by converting them into a percentage. In the case of Comparative Example 4, the indicator substance was present at approximately 12.6%, while Example 7 (single capsule) was 61.5% and Example 13 (double capsule) was 98.5%, indicating that the double capsule showed significantly superior stability compared to other sample groups. This is a meaningful result that proves that the polymer matrix capsule coats the liquid crystal particles of the single capsule, preventing contact with the outside and blocking oxygen, thereby maintaining a stable state without oxidation.
[0099] Although the present invention has been described with reference to the attached drawings, it is understood that various modifications and variations may be made within the scope of the technical spirit of the invention. Therefore, the scope of the present invention should not be limited to the described embodiments, but should be defined by the claims set forth below as well as equivalents thereof. Explanation of the symbols
[65535] doesn't exist
Claims
Claim 1 A step of providing an oil phase component for preparing an oil phase component; a step of providing a water phase component for preparing a water phase component; a first mixing step of mixing the oil phase component and the water phase component in a ratio of 1:5 to 1:7; a step of providing an active ingredient for preparing a first mixed solution by mixing an active ingredient into the mixture after the first mixing step; a first encapsulation step of passing the first mixed solution through a nanomixer at a high pressure of 100 to 1000 bar to form an oil-in-water type liquid crystal emulsion comprising nanoparticles having a non-phospholipid multilayer lamellar liquid crystal structure of at least three layers, in which the active ingredient is encapsulated; a second mixing step of preparing a second mixed solution by mixing the liquid crystal emulsion with a polymer solution in which a PEG (polyethylene glycol)-based polymer capable of water gelation is dissolved; and a second encapsulation step of passing the second mixed solution through a nozzle and dropping it to obtain a double matrix capsule particle containing the nanoparticles of the liquid crystal structure inside and having a gelled polymer matrix on the outside of the nanoparticles. A method for manufacturing a double matrix capsule comprising: a liquid crystal emulsion containing 3 to 5.1 weight% of a surfactant including sucrose polycotton seed date and polyglyceryl-10 behenate / eicosadioate; a polymer content of 0.05 to 1 weight% of the polymer solution; and a surfactant content including polyglyceryl-10 stearate and polyglyceryl-10 oleate of 0.5 to 5 weight%. Claim 2 A method for manufacturing a double matrix capsule according to claim 1, wherein the size of the double matrix capsule particles is 0.1㎛ to 5mm. Claim 3 A method for manufacturing a double matrix capsule according to claim 1, wherein the oil phase component comprises a surfactant for forming a primary capsule, a polyalcohol, and an oil component. Claim 4 A method for manufacturing a double matrix capsule according to claim 1, wherein the aqueous components include purified water, a thickening agent, a skin irritation-relieving component, a skin moisturizing component, and a preservative component. Claim 5 A method for manufacturing a double matrix capsule according to claim 1, wherein the active ingredient is one or more substances selected from the group consisting of GHK-Cu, AHK-Cu, fisetin, quercetin, idebenone, vitamin, resveratrol, caffeine, adenosine, cordycepin, niacinamide, and genistein. Claim 6 A method for manufacturing a double matrix capsule according to claim 1, wherein the polymer is PEG-240 / HDI copolymer bis-decyltetradeceth-20 ether. Claim 7 delete Claim 8 delete