Vitamin-loaded spicules and their manufacturing method
Vitamin-loaded spicules, produced through high-pressure impregnation and coating, address the need for stable, natural vitamin delivery in cosmetics, enhancing skin health and stability.
Patent Information
- Application Number
- JP2023560647
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Priority Date
- 2023-03-23
- Filing Date
- 2023-07-24
- Publication Date
- 2026-01-20
- Estimated Expiration
- 2043-07-24
AI Technical Summary
The cosmetics industry seeks natural, environmentally friendly ingredients that effectively deliver active ingredients to the skin without causing skin dryness, rashes, inflammation, or skin cancer, and there is a need for improved methods to stabilize and enhance the delivery of vitamins in cosmetic compositions.
Vitamin-loaded spicules are produced by impregnating spicules with vitamins and forming an organic coating layer on their surface, using high-pressure vacuum impregnation and coating with organic and silica layers to stabilize the vitamins and enhance transdermal absorption.
The vitamin-loaded spicules maintain vitamin stability and enhance transdermal delivery, providing effective antioxidant properties and skin benefits such as improved skin condition, reduced wrinkles, and increased elasticity.
Smart Images

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Abstract
Description
[Technical Field]
[0001] The present invention relates to vitamin-loaded spicules, their production method, and uses. The vitamin-loaded spicules of the present invention can be used in cosmetic compositions containing vitamins as active ingredients. [Background technology]
[0002] As appearance is increasingly recognized as a measure of health, interest in skin health has grown. In the cosmetics industry, interest is growing in environmentally friendly materials that are harmless to the human body and have functional effects on the skin. Synthetic surfactants, pigments, antioxidants, and chemical preservatives found in cosmetics are known to dry out the skin and potentially cause rashes, inflammation, skin diseases, and even skin cancer. This has led to a strong demand for cosmetics that use natural substances as their primary ingredients instead of chemical ingredients that are harmful to the skin. Research into naturally derived functional substances is also gaining attention in the field of functional cosmetics, which emphasizes the additional functional effects of cosmetics.
[0003] Among these natural substances, spicules (sponge spicules), also known as sponges, are primitive marine organisms lacking muscles, nerves, or organs. There are over 5,000 species of sponges, and they are found at any depth. Spigules are needle-shaped skeletal structures found in the bodies of invertebrates, primarily composed of silica and calcium carbonate. The fibrous skeletons of sponges have the ability to absorb nutrients via capillary action and are used in a variety of fields, including medical applications. For example, sponge spicules contain antibiotics for the treatment of osteomyelitis and are used for the treatment and prevention of the disease. Because of their needle-like structure, sponge-derived spicules are particularly suitable for delivering active ingredients to the transdermal layer of the skin, and attempts have been made to use them in cosmetic compositions. Summary of the Invention [Problem to be solved by the invention]
[0004] One aspect of the present invention is to provide vitamin-loaded spicules.
[0005] One aspect of the present invention is to provide a method for producing vitamin-loaded spicules.
[0006] One aspect of the present invention is to provide a cosmetic composition comprising vitamin-loaded spicules. [Means for solving the problem]
[0007] One embodiment of the present invention provides a vitamin-loaded spicule comprising a spicule body having an inner hole and an organic coating layer formed on the outer surface of the spicule body, the spicule containing a vitamin component within the inner hole.
[0008] In some embodiments, the vitamin component may be one or more selected from the group consisting of vitamin A, vitamin B, vitamin C, vitamin D, vitamin E, and vitamin K.
[0009] In some embodiments, the organic coating layer may include an organic polymer or a natural polymer.
[0010] In some embodiments, the organic polymer may be one or more selected from the group consisting of polyvinyl alcohol (PVA), polyglycolide (PGA), poly-L-lactide (PLLA), poly-D-lactide (PDLA), poly-D,L-lactide (PDLLA), lactide-glycolide copolymer (PLGA), polytrimethylene carbonate (TMC), polydioxanone (PDO), poly(ε-caprolactone) (PCL), poly-3-hydroxybutyrate (P3HB), poly-4-hydroxybutyrate (P4HB), polyhydroxyvalerate (PHV), polyhydroxyhexanoate (PHH), polyhydroxyoctanoate (PHO), and copolymers thereof.
[0011] In some embodiments, the organic coating layer may include a silica coating.
[0012] In some embodiments, the organic coating layer may include an amino coating on the silica coating.
[0013] In some embodiments, the organic coating layer may include an organic material layer containing an organic polymer or a natural polymer on the amino coating.
[0014] In some embodiments, the organic coating layer may be covalently bonded to the amino coating.
[0015] One embodiment of the present invention provides a method for manufacturing vitamin-loaded spicules, including the steps of preparing a spicule body having an inner hole, impregnating the inner hole with a vitamin component, and forming an organic coating layer on the surface of the spicule body.
[0016] In some embodiments, the step of impregnating the vitamin component may include placing the spicules together with the vitamin component into a vacuum container and forming a vacuum inside the vacuum container at a pressure of 30 MPa or more.
[0017] In some embodiments, forming the organic coating layer may include reacting the spicules with an organic coating solution containing an organic polymer or a natural polymer.
[0018] In some embodiments, forming the organic coating layer may include coating the surface of the spicule with silica.
[0019] In some embodiments, forming the organic coating layer may include introducing amino groups onto the silica coating.
[0020] In some embodiments, forming the organic coating layer may include bonding the organic coating to amino groups of the silica coating.
[0021] One embodiment of the present invention provides a cosmetic composition containing the vitamin-loaded spicules as an active ingredient.
[0022] In some embodiments, the cosmetic composition may be for improving skin condition, reducing wrinkles, increasing elasticity, or moisturizing skin.
[0023] In some embodiments, the cosmetic composition may have the formulation of a skin lotion, skin softener, skin toner, astringent, lotion, milk lotion, moisturizing lotion, nourishing lotion, massage cream, nourishing cream, moisturizing cream, eye cream, hand cream, foundation, essence, nourishing essence, eye essence, pack, soap, cleansing foam, cleansing lotion, cleansing cream, body lotion, body cream, body cleanser, suspension, gel, powder, paste, mask pack, sheet, or aerosol. [Effects of the Invention]
[0024] The spicules of the present invention can contain large amounts of vitamin components, such as vitamin C, in their pores, and an organic coating layer can be formed on their outer surfaces, stably maintaining the vitamin components in the pores even when the temperature changes or over time. Therefore, the antioxidant properties of the vitamin components can be effectively preserved even when the environment changes. Furthermore, the vitamin-loaded spicules can penetrate the vitamin components deep into the skin, increasing the transdermal absorption of the vitamin components, and can be used in highly functional cosmetic compositions. [Brief explanation of the drawings]
[0025] [Figure 1]FIG. 1 is a schematic flow diagram illustrating a method for producing vitamin-loaded spicules according to an embodiment. [Figure 2] FIG. 2 is a graph showing the results of long-term stability evaluation of vitamin-loaded spicules and compositions of Examples and Comparative Examples. [Figure 3] FIG. 3 is a graph showing the amount of vitamin released over time for vitamin-loaded spicules and compositions of the Examples and Comparative Examples. [Figure 4] FIG. 4 is a graph showing the results of evaluating the antioxidant capacity over time for vitamin-loaded spicules and compositions of Examples and Comparative Examples. DETAILED DESCRIPTION OF THE INVENTION
[0026] One aspect of the present invention provides a vitamin-loaded spicule, which includes a spicule body having an internal cavity, an organic coating layer on the outer surface of the spicule body, and a vitamin component contained within the internal cavity.
[0027] The terms "spicules," "spicules," or "needle-like structures" refer to fine needle-like structures that constitute the skeleton of sponges. The terms "spicules," "spicules," and "needle-like structures" may be used interchangeably.
[0028] The term "sponge" simply refers to a metazoan animal belonging to the Porifera phylum, which may be Spongilla lacustris.
[0029] The spicules may be composed of calcium or silica and may have a porous interior. The spicules may have an I-type structure, a Y-type structure, or an X-type structure. Specifically, the spicules may be monoaxon, triaxon, tetraxon, or polyaxon. Furthermore, the triaxon structure may be triactine or hexactine. The "monoaxon" refers to a needle-like spicule with a pointed tip. Preferably, the spicules may have an I-type structure or a monoaxon structure.
[0030] The spicules may be obtained from sponges and further purified.
[0031] The spicules may include a spicule body and an internal bore within the body, the internal bore may extend through the body, or the spicules may have a shape in which the internal bore is surrounded by the body.
[0032] In some embodiments, the spicules may have a long needle or tubular shape in a particular direction, and the inner holes may be formed in the longitudinal direction of the spicules. For example, the inner holes may penetrate the spicules in the longitudinal direction. The inner holes may have a tubular shape that penetrates the spicules in the longitudinal direction.
[0033] The spicules may contain vitamin components within their inner pores. For example, the spicules may have the vitamin components supported within their inner pores. The inner pores may be closed by the organic coating layer. After the vitamin components are supported within the spicules, the inner pores may be closed by the organic coating layer. For example, if the inner pores have a tubular shape that penetrates the spicules in the longitudinal direction, both ends of the tubular shape may be closed by the organic coating layer.
[0034] The spicules of the present invention are characterized by containing pure spicules from which all natural impurities have been removed, and therefore the spicules may contain vitamin components in their internal porous structure.
[0035] The vitamin component may be a cosmetically effective component, and may include a component for improving or enhancing skin function, a component for preventing deterioration of skin condition, or a component for complementing skin defects or highlighting skin advantages.
[0036] In some embodiments, the vitamin component may be one or more selected from the group consisting of vitamin A, vitamin B, vitamin C, vitamin D, vitamin E, and vitamin K. Vitamin B may be vitamin B1, B2, B3, B5, B6, B7, B9, or B 12 Vitamin D may include vitamin D1, D2, D3, D4 or B5. Vitamin K may include vitamin K1 or K2.
[0037] The vitamin component may be dissolved in a suitable solvent and then supported in the pores. As a water-soluble vitamin, vitamin B or vitamin C may be dissolved in a hydrophilic solvent such as water and then supported in the pores. As an oil-soluble vitamin, vitamin A, vitamin D, vitamin E, or vitamin K may be dissolved in a hydrophobic solvent and then supported in the pores.
[0038] The spicules may contain at least one vitamin component in the porous structure inside the spicules or on the surface. Furthermore, the spicules may contain two or more vitamin components. Specifically, the spicules may contain a first vitamin component or a second vitamin component. Specifically, the first vitamin component may be encapsulated in the porous structure inside the spicules, and the second vitamin component may be coated on the surface.
[0039] The spicules include an organic coating layer on the outer surface of the spicule body, the organic coating layer can at least partially cover the outer surface of the spicule body, or the organic coating layer can be in direct contact with the outer surface of the spicule body.
[0040] The organic coating layer may block the vitamin component from leaking out of the pores. The organic coating layer may protect the component in the pores from temperature changes. For example, the organic coating layer may prevent the component in the pores from being decomposed or denatured due to an increase in temperature. When the spicules are used, the organic coating layer may be decomposed to release the component in the pores.
[0041] In some embodiments, the organic coating layer may include an organic polymer material or a natural polymer material. For example, the organic coating layer may be formed of the organic polymer material or the natural polymer material.
[0042] In some embodiments, the organic polymer may be polyvinyl alcohol (PVA), polyglycolide (PGA), poly-L-lactide (PLLA), poly-D-lactide (PDLA), poly-D,L-lactide (PDLLA), L-lactide-co-glycolide (PLGA), polytrimethylene carbonate (TMC), polydioxanone (PDO), poly(ε-caprolactone) (PCL), poly-3-hydroxybutyrate (poly-3-hydroxybutyrate), or the like. The organic polymer material may include at least one selected from the group consisting of poly-4-hydroxybutyrate (P3HB), poly-4-hydroxybutyrate (P4HB), polyhydroxyvalerate (PHV), polyhydroxyhexanoate, polyhydroxyoctanoate (PHO), and copolymers thereof. Preferably, the organic polymer material may be PVA.
[0043] In some embodiments, the natural polymer may include catgut.
[0044] In some embodiments, the organic coating layer may include a silica coating. The silica coating refers to a coating of a material containing silicon dioxide (SiO2). The silica coating may be formed from a silica precursor.
[0045] Some specific examples of the silica precursor may be tetraethylorthosilicate (TEOS), siloxane (siloxane polymer), etc. The silica coating can modify the surface of the needle-shaped body to improve the binding performance with other coating components or active ingredients.
[0046] In some embodiments, the organic coating layer may include an amino coating on the silica coating. The amino coating may be coated with an amino precursor containing an amino group (—NH). The amino coating may introduce amino groups onto the surface of the silica coating. For example, the amino coating may form an amino coating layer on the silica coating layer formed from the silica coating. Alternatively, the amino coating may be integrated with the silica coating to form an amino-modified silica coating.
[0047] The amino coating refers to coating the surface of the spicule with a substance or amino acid containing an amino group at its terminal, which modifies the surface of the silica coating and allows an organic coating to be strongly bonded to the surface of the silica coating.
[0048] In some embodiments, the amino coating may be an aminosilane coating and / or a lysine coating.
[0049] The term "aminosilane" refers to an N-silyl compound in which hydrogen is replaced by an amino group, and has the chemical formula SiH4. The aminosilane may be used as a silane coupling agent to form a hydrophilic coating layer.
[0050] The aminosilane may be N-2-(aminoethyl)-3-aminopropylmethyldimethoxysilane, N-2-(aminoethyl)-3-aminopropyltrimethoxysilane, 3-triethoxysilyl-N-(1,3 dimethylbutylidene)propylamine, N-phenyl-3-aminopropyltrimethoxysilane, N-(vinylbenzyl-2-aminoethyl-3-aminopropyltrimethoxysilane hydrochloride), N-(vinylbenzyl)-2-aminoethyl-3-aminopropyltrimethoxysilane hydrochloride, 3-aminopropyltrimethoxysilane, 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane hydrolysate, its derivative, or a combination thereof. Preferably, the aminosilane may be 3-aminopropyltrimethoxysilane.
[0051] In some embodiments, the organic coating layer may include an organic material layer including an organic polymer or a natural polymer on the amino coating. The organic material layer may be formed of the organic polymer or the natural polymer. The organic material layer may form a layered structure on the amino coating layer including the amino coating, or may be integrated with the amino coating layer. For example, the organic coating layer may have a layered structure in which the silica coating layer, the amino coating layer, and the organic material layer are sequentially stacked, or may have a structure in which they are partially integrated with each other.
[0052] In some embodiments, the organic coating may be covalently bonded to the amino coating. In this case, the organic material may stably coat the surface of the spicules and effectively protect the vitamin substance contained in the pores. Therefore, decomposition, denaturation, and leakage of the vitamin substance may be effectively prevented over time, due to environmental changes such as temperature changes, etc.
[0053] One aspect of the present invention provides a method for manufacturing vitamin-loaded spicules, which includes the steps of preparing a spicule body having an inner hole, impregnating the inner hole with a vitamin component, and forming an organic coating layer on the surface of the spicule body.
[0054] The pore-containing spicules can be obtained from sponges, and the spicules may be washed to remove organic and inorganic impurities.
[0055] The washing is for removing organic impurities present in the inner bore of the needle-shaped body and can be carried out using purified water and a basic or acidic solution. Preferably, the washing of the needle-shaped body can be carried out by washing the needle-shaped body with purified water one or more times, followed by treatment with an acidic solution such as sulfuric acid, hydrochloric acid, hydrofluoric acid, or hydrogen peroxide, and / or a basic solution such as sodium hydroxide or potassium hydroxide.
[0056] The step of impregnating the inner hole with the vitamin component may include injecting the vitamin component into the inner hole of the spicule through a high-pressure vacuum. For example, when the spicule including the inner hole and the vitamin component are placed in a vacuum container and a vacuum is formed in the vacuum container, the vitamin component may migrate into the inner hole.
[0057] The vacuum container may include a vacuum pack or the like.
[0058] The vitamin ingredients may be dissolved in a suitable solvent to form a vitamin solution, which may then be injected into the bore.
[0059] In some embodiments, the step of impregnating the spicules with the vitamin ingredients may involve placing the spicules and the vitamin ingredients together in a vacuum container, and forming a vacuum inside the vacuum container at a pressure of 30 MPa or more. For example, the vacuum pressure may be 300 MPa or less. Preferably, the vacuum pressure may be 30 MPa to 300 MPa, 40 MPa to 300 MPa, 50 MPa to 300 MPa, 30 MPa to 200 MPa, 40 MPa to 200 MPa, 50 MPa to 200 MPa, 30 MPa to 150 MPa, 40 MPa to 150 MPa, or 50 MPa to 150 MPa.
[0060] In some embodiments, the vacuum application may be performed for 1 minute to 20 minutes, for example, 1 minute to 15 minutes or 1 minute to 10 minutes.
[0061] An organic coating layer may be formed on the surface of the spicule. The organic coating layer may be formed by coating the surface of the spicule with an organic substance or a precursor thereof. The organic substance or precursor thereof may include an organic polymer substance or a natural polymer substance. For example, the step of forming the organic coating layer may include reacting the spicule with an organic coating solution containing an organic polymer substance or a natural polymer substance.
[0062] In some embodiments, the organic polymer may be polyvinyl alcohol (PVA), polyglycolide (PGA), poly-L-lactide (PLLA), poly-D-lactide (PDLA), poly-D,L-lactide (PDLLA), L-lactide-co-glycolide (PLGA), polytrimethylene carbonate (TMC), polydioxanone (Polypdioxa The organic polymer material may include at least one selected from the group consisting of poly(ε-caprolactone) (PDO), poly(ε-caprolactone) (PCL), poly-3-hydroxybutyrate (P3HB), poly-4-hydroxybutyrate (P4HB), polyhydroxyvalerate (PHV), polyhydroxyhexanoate (PHH), polyhydroxyoctanoate (PHO), and copolymers thereof. Preferably, the organic polymer material may be PVA.
[0063] In some embodiments, the natural polymer may include catgut.
[0064] The organic material precursors may be dissolved in a suitable solvent to form an organic coating solution, which may include hydrophilic solvents such as water or alcohols, or hydrophobic solvents such as aliphatic or aromatic hydrocarbons.
[0065] In some embodiments, forming the organic coating layer may include coating the surface of the spicule with silica, which may be formed by reacting the surface of the spicule with a silica precursor.
[0066] Some specific examples of the silica precursor may be tetraethylorthosilicate (TEOS), siloxane (siloxane polymer), etc. The silica coating can modify the surface of the needle-shaped body to improve the binding performance with other coating components or active ingredients.
[0067] The silica coating is preferably carried out at 25 to 50°C for 30 minutes to 2 hours, and may include ultra-high pressure treatment in which a pressure of 50 to 300 MPa is applied for 1 to 10 minutes. The above conditions can result in the best silica coating.
[0068] In some embodiments, forming the organic coating layer may include introducing amino groups onto the silica coating by coating the silica-coated spicules with an amino precursor containing an amino group (—NH).
[0069] For example, the amino coating may form an amino coating layer on top of the silica coating layer formed from the silica coating, or the amino coating may be integrated with the silica coating to form an amino-modified silica coating.
[0070] In some embodiments, the amino precursor may be an aminosilane and / or an amino acid, and the amino precursor may be dissolved or dispersed in a suitable solvent (e.g., water).
[0071] The aminosilane may be N-2-(aminoethyl)-3-aminopropylmethyldimethoxysilane, N-2-(aminoethyl)-3-aminopropyltrimethoxysilane, 3-triethoxysilyl-N-(1,3 dimethylbutylidene)propylamine, N-phenyl-3-aminopropyltrimethoxysilane, N-(vinylbenzyl)-2-aminoethyl-3-aminopropyltrimethoxysilane hydrochloride, N-(vinylbenzyl)-2-aminoethyl-3-aminopropyltrimethoxysilane hydrochloride, 3-aminopropyltrimethoxysilane, 3-aminopropyltrimethoxysilane, a hydrolyzate of 3-aminopropyltriethoxysilane, a derivative thereof, or a combination thereof. Preferably, the aminosilane may be 3-aminopropyltrimethoxysilane.
[0072] In some embodiments, forming the organic coating layer may include bonding an organic substance to the amino group of the silica coating. For example, the spicules on which the amino-group-introduced silica coating is formed may be reacted with an organic substance or a precursor thereof to bond the organic substance to the amino group, the silica coating, and the spicules.
[0073] The formed organic material layer may form a layered structure on the amino coating layer including the amino coating, or may be integrated with the amino coating layer. For example, the organic coating layer may have a layered structure in which the silica coating layer, the amino coating layer, and the organic material layer are sequentially stacked, or may have a structure in which these are partially integrated with each other.
[0074] For example, the method for manufacturing the vitamin-loaded spicules may include the steps of cleaning the spicules, impregnating the inner holes of the cleaned spicules with vitamin components, coating the exterior of the spicules with the vitamin components impregnated into the inner holes with silica, coating the silica-coated spicules with amino, and coating the silica-coated spicules with an organic substance.
[0075] One aspect of the present invention provides a cosmetic composition containing the vitamin-loaded spicules as an active ingredient.
[0076] The spicules are the same as those described above. Furthermore, the cosmetic composition may be for whitening, improving skin condition, peeling, reducing wrinkles, improving elasticity, or moisturizing skin.
[0077] The spicules may be contained in an amount of 0.1 to 10% by weight based on the total weight of the cosmetic composition. Specifically, the spicules may be contained in an amount of 0.2 to 10% by weight, 0.3 to 10% by weight, 1 to 10% by weight, 1 to 5% by weight, 1 to 8% by weight, 1 to 5% by weight, 0.5 to 3% by weight, or 1 to 3% by weight.
[0078] For example, the content of the spicules is not particularly limited, but may be preferably 0.1 to 5 parts by weight based on 100 parts by weight of the cosmetic composition, which can exhibit the best transdermal absorption rate and skin improving effect.
[0079] The cosmetic composition may be a formulation commonly used in cosmetics. In some embodiments, the composition may be prepared as a skin lotion, skin softener, skin toner, astringent, lotion, milk lotion, moisturizing lotion, nourishing lotion, massage cream, nourishing cream, moisturizing cream, eye cream, hand cream, foundation, essence, nourishing essence, eye essence, pack, soap, cleansing foam, cleansing lotion, cleansing cream, body lotion, body cream, body cleanser, suspension, gel, powder, paste, mask pack or sheet, or aerosol composition. Furthermore, the composition may be applied in various forms suitable for providing moisture to the skin, such as a gel or cream, a paste, or a solid, and specifically may be a particulate gel cream such as a sherbet or slush. Such formulations may be prepared according to conventional methods in the art.
[0080] In some embodiments, the composition may further comprise at least one selected from the group consisting of oils, purified water, emulsifiers, dispersants, pigments, fragrances, sunscreens, sweeteners, vitamins, and sequestering agents. In some embodiments, the composition may further comprise 0.1% to 3.0% by weight of a preservative. The amount of the additional ingredients, such as oils, can be easily determined by one skilled in the art within a range that does not impair the objects and effects of the present invention.
[0081] The cosmetic composition according to some embodiments may preferably be a cream formulation. For example, when the cosmetic composition has a cream formulation, the coated spicules of the present invention may be uniformly contained, which may be effective in moisturizing the skin and also effective in allowing the spicules to penetrate the skin.
[0082] The cosmetic composition according to some embodiments may further include any conventional cosmetic ingredient selected from additional ingredients commonly used in cosmetics, such as dispersants, thickeners, pigments, fragrances, fillers, preservatives, antiseptics, neutralizing agents, sunscreens, sweeteners, vitamins, free radical scavengers, sequestering agents, and mixtures thereof.
[0083] The skin-improving active ingredient contained in the cosmetic composition may include an ingredient for improving or enhancing skin function, an ingredient for preventing deterioration of skin condition, or an ingredient for correcting skin imperfections or highlighting skin advantages. The content of the active ingredient is not particularly limited, but may preferably be 0.05 to 1 part by weight based on 100 parts by weight of the cosmetic composition. In addition to the active ingredient, the cosmetic composition according to the present invention may also contain various ingredients commonly found in cosmetic compositions. For example, it may contain all substances commonly used in mask sheets, such as dispersants, thickeners, surfactants, preservatives, moisturizers, stabilizers, solubilizers, pigments, and fragrances.
[0084] According to some embodiments, the cosmetic composition may have a skin exfoliating effect and may also have a wrinkle reducing effect.
[0085] The cosmetic composition according to an embodiment of the present invention may further include purified water, an antioxidant, a stabilizer, a pigment, or a fragrance, which are commonly used in the field of cosmetic compositions.
[0086] Furthermore, the cosmetic composition according to an embodiment of the present invention may be prepared using a conventional formulation, specifically, it may be formulated as a solution, suspension, emulsion, paste, gel, cream, lotion, powder, emulsion foundation, wax foundation, spray, or the like.
[0087] Hereinafter, embodiments will be described in detail with reference to the accompanying drawings.
[0088] However, since the embodiments can be modified in various ways, the scope of the patent application is not limited or restricted by these embodiments, and all modifications, equivalents, and alternatives to the embodiments should be understood as being included in the scope of the patent.
[0089] The terms used in the examples are used for the purpose of explanation only and should not be construed as limiting. The singular term includes the plural term unless the context clearly dictates otherwise. In this specification, the terms "comprise" or "have" and the like are intended to specify the presence of features, numbers, steps, operations, components, parts, or combinations thereof described in the specification, and should be understood as not precluding the possibility of the presence or addition of one or more other features, numbers, steps, operations, components, parts, or combinations thereof.
[0090] Unless otherwise defined, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by a person of ordinary skill in the art to which the embodiments pertain. Terms as defined in commonly used dictionaries should be interpreted to have a meaning consistent with the contextual meaning of the relevant art, and should not be interpreted as idealized or overly formal unless expressly defined in this application.
[0091] Preparation Example 1. Preparation of spicules
[0092] Needle-shaped structures were extracted from the Russian sponge Spongila lacustris L. to prepare spicules (spicules) containing internal pores. 100 g of spicules were placed in 1,000 mL of purified water to remove salts, and then filtered through a 400-mesh polyethylene (PE) filter. The spicules remaining on the filter were then washed twice with purified water. The spicules were then placed in 1,000 mL of 70% (v / v) aqueous ethanol solution for sterilization, filtered through a 400-mesh polyethylene filter, and the spicules remaining on the filter were then washed twice with purified water. The washed spicules were then placed in a dryer (Hanbaek Science Co., Ltd.) and dried at 50°C.
[0093] To remove impurities remaining in the dried spicules, the dried spicules were placed in 1,000 mL of 35% (v / v) hydrogen peroxide (H2O2) (Sanchong Chemical Co., Ltd.) and sonicated for 1 hour at 60°C, 300 W, and 40 kHz using an ultrasonic cleaner (Seongdong Ultrasonics Co., Ltd.). The mixture was then filtered through a 400-mesh polyethylene filter, and the spicules remaining on the filter were washed with 500 mL of purified water, a process repeated three times. The washed spicules were then placed in a dryer and dried at 50°C.
[0094] 500 mL of 1N HCl (Sigma-Aldrich) was added to 100 g of spicules and allowed to react for 1 hour. 500 mL of 1N NaOH (Sigma-Aldrich) was then added to neutralize the mixture. 1,000 mL of 10% sodium percarbonate was then added and allowed to react for 1 hour to remove organic impurities from the inner pores, yielding washed spicules.
[0095] Production Example 2: Production of Vitamin C Spicules
[0096] A 10 g mixture of 1 part by weight of spicules, 98.9 parts by weight of purified water, and 0.1 part by weight of vitamin C (accorbic acid, Sigma-Aldrich) was placed in a plastic bag, evacuated, and then pressurized at 150 MPa for 5 minutes using a high-pressure processor (Ilshin Autoclave, Suflux®) to load vitamin C into the pores of the spicules. The mixture was then filtered through a 400-mesh polyethylene filter, and the spicules remaining on the filter were stored in 1-pentanol.
[0097] Example 1. Preparation of silica-coated spicules
[0098] A mixture of 1 part by weight of vitamin C spicules, 98 parts by weight of purified water, and 1 part by weight of tetraethylorthosilicate was reacted at room temperature for 1 hour to coat the spicules with silica.
[0099] Example 2. Preparation of amino-coated spicules
[0100] To 1 part by weight of the spicules from Example 1, 0.01 parts by weight of 3-aminopropyltrimethoxysilane and 98.99 parts by weight of water were added, and the mixture was allowed to react at room temperature for 1 hour to coat the spicules with amino groups. The spicules were then washed with 500 mL of purified water, and this process was repeated three times.
[0101] Example 3. Preparation of polyvinyl alcohol-coated spicules
[0102] To 1 part by weight of the spicules of Example 2, 10 parts by weight of polyvinyl alcohol (molecular weight 30,000 to 70,000 Da) and 89 parts by weight of water were added, and the mixture was allowed to react at room temperature for 1 hour to coat the spicules with polyvinyl alcohol.
[0103] Comparative Example 1. Preparation of Purified Spicule Sample
[0104] The spicules of Production Example 1 were washed with 500 mL of purified water to prepare the spicules of Comparative Example 1.
[0105] Comparative Example 2. Preparation of Vitamin C Spicule Sample
[0106] The vitamin C spicules of Production Example 2 were washed three times with 500 mL of purified water to prepare spicules of Comparative Example 2. These needle-shaped structures were not coated with amino or polyvinyl alcohol.
[0107] Comparative Example 3. Preparation of Vitamin C Solution
[0108] Vitamin C was dissolved in purified water to prepare a vitamin C solution with a concentration of 100 μg / mL.
[0109] Experimental Example 1: Evaluation of remaining amount of vitamin C as a function of temperature
[0110] The initial vitamin C content of the spicules and compositions of the Examples and Comparative Examples was set to 100. The spicules and compositions of the Examples and Comparative Examples were placed at room temperature (27°C), 37°C, and 45°C.
[0111] After 7 days, the spicules and compositions of the Examples and Comparative Examples were added to 100% alcohol (ethyl alcohol) and reacted at 50°C for 1 hour. Samples were then collected and the vitamin C content was measured using Agilent high performance liquid chromatography (HPLC). HPLC was performed using an Agilent C18 column with a detector wavelength of 254 nm and a flow rate of 0.8 mΩ / min. A standard measurement graph was plotted using the peak height at 266 nm of the measured residue and a UV spectrometer. The relative amounts of vitamin C were measured using the UV spectrometer and are shown in Table 1 below.
[0112] [Table 1]
[0113] Referring to Table 1, it was confirmed that in the case of vitamin C spicules coated with PVA, the vitamin C content did not decrease even at high temperatures, and the initial content was maintained.
[0114] Experimental Example 2: Evaluation of long-term stability of vitamin C
[0115] The stability of vitamin C in the spicules and compositions of the Examples and Comparative Examples was evaluated over a long period of time. The spicules of each sample were stored in a dry state at room temperature for 1, 2, 4, 10, 20, and 30 days, and then the vitamin C content was measured by HPLC under the same conditions as in Experimental Example 1. The results are shown in Figure 2.
[0116] Referring to FIG. 2, it was confirmed that the vitamin C content held inside the PVA-coated vitamin C spicules was maintained even after a long period of time.
[0117] Experimental Example 3: Analysis of the amount of vitamin C remaining after its release from spicules
[0118] The residual amount of vitamin C in the spicules of the Example and Comparative Examples was analyzed based on the initial vitamin C content. Specifically, 1 part by weight of each spicule of the Example and Comparative Examples was added to 99 parts by weight of purified water, and the vitamin C content of each sample was measured after 0, 12, 24, 36, 48, and 60 hours at 37°C. The results are shown in Figure 3.
[0119] Referring to FIG. 3, it was confirmed that the vitamin C contained in the PVA-coated vitamin C spicules was slowly released at 37°C.
[0120] Experimental Example 4: Antioxidant activity analysis of vitamin C spicules
[0121] The antioxidant effect of vitamin C on the spicules and compositions of the Examples and Comparative Examples was analyzed using a DPPH assay. Specifically, DDPH (2,2-Diphenyl-1-picrylhydrazyl, Sigma-Aldrich) was dissolved in methanol at 0.1 mM to prepare a DPPH solution. The DPPH solution and each vitamin C sample were mixed in a volume ratio of 6:4 and incubated at room temperature for 30 minutes.
[0122] The absorbance of DPPH was measured using a spectrophotometer at a wavelength of 520 nm. The antioxidant capacity of vitamin C was measured at 37°C after 0, 12, 24, 36, 48, and 60 hours. The antioxidant capacity of a 100 μg / mL vitamin C solution was set at 100, and the relative values are shown in Figure 4.
[0123] Referring to Figure 4, it was confirmed that the PVA-coated vitamin C spicules maintained their excellent antioxidant effect over time.
Claims
1. a spicule body including an internal cavity; an organic coating layer formed on the outer surface of the spicule body; The cavity contains a vitamin component, which is vitamin C, The organic coating layer includes an organic polymeric substance or a natural polymeric substance, and the organic polymeric substance is at least one selected from the group consisting of polyvinyl alcohol (PVA), polyglycolide (PGA), poly-L-lactide (PLLA), poly-D-lactide (PDLA), poly-D,L-lactide (PDLLA), lactide-glycolide copolymer (PLGA), polytrimethylene carbonate (TMC), polydioxanone (PDO), poly(ε-caprolactone) (PCL), poly-3-hydroxybutyrate (P3HB), poly-4-hydroxybutyrate (P4HB), polyhydroxyvalerate (PHV), polyhydroxyhexanoate (PHH), polyhydroxyoctanoate (PHO), and copolymers thereof. A vitamin-loaded spicule characterized by:
2. The organic coating layer comprises a silica coating. The vitamin-loaded spicules according to claim 1.
3. The vitamin-loaded spicules of claim 2 , wherein the organic coating layer comprises an amino coating on the silica coating.
4. The organic coating layer comprises an organic material layer containing the organic polymer material or the natural polymer material on the amino coating. The vitamin-loaded spicules according to claim 3.
5. the organic coating layer is covalently bonded to the amino coating; The vitamin-loaded spicules according to claim 4.
6. A method for producing vitamin-loaded spicules, comprising the steps of: providing the spicule body including the internal bore; impregnating the inner cavity with the vitamin component; forming the organic coating layer on the surface of the spicule body; A method for producing vitamin-loaded spicules, comprising:
7. the step of forming the organic coating layer includes reacting the spicule with an organic coating solution containing the organic polymer or the natural polymer; A method for producing the vitamin-loaded spicules according to claim 6.
8. the step of forming the organic coating layer includes coating the surface of the spicule body with silica; A method for producing the vitamin-loaded spicules according to claim 6.
9. The method of claim 8, wherein the step of forming the organic coating layer comprises introducing an amino group onto the silica coating. A method for producing the vitamin-loaded spicules according to claim 8.
10. The step of forming the organic coating layer includes bonding an organic coating to the amino groups. A method for producing the vitamin-loaded spicules according to claim 9.
11. A composition comprising the vitamin-loaded spicules of claim 1 as an active ingredient. A cosmetic composition characterized by:
12. For improving skin condition, wrinkle reduction, elasticity enhancement, or skin moisturization. The cosmetic composition according to claim 11.
13. Having a formulation of a skin lotion, skin softener, skin toner, astringent, lotion, milk lotion, moisturizing lotion, nourishing lotion, massage cream, nourishing cream, moisturizing cream, eye cream, hand cream, foundation, essence, nourishing essence, eye essence, pack, soap, cleansing foam, cleansing lotion, cleansing cream, body lotion, body cream, body cleanser, suspension, gel, powder, paste, mask pack or sheet, or aerosol, The cosmetic composition according to claim 11.
Citation Information
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