Stable slow-release antioxidant skin care composition emulsion as well as preparation method and application thereof
By using chitosan microcapsules in cosmetics to coat resveratrol-ATP nanoparticle complex and tea tree oil, and combined with nanobubblescent water, the problems of insufficient stability and low antioxidant performance are solved, and the long-term antioxidant and maintenance effects of the skin care composition are achieved.
Patent Information
- Application Number
- CN202411803887.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-10
- Publication Date
- 2025-03-11
AI Technical Summary
The stability of nanobubbles in existing cosmetics is insufficient and is prone to burst under external force, resulting in poor skin care effects. At the same time, the substances coated by nanobubble have low antioxidant performance and cannot effectively maintain the skin for a long time.
Chitosan microcapsules are used to coat the resveratrol-ATP nanoparticle complex and tea tree oil to form a stable sustained-release system, combined with nano sparkling water, and improve the stability and antioxidant effect of the skin care composition.
The long-term sustained release of the skin care composition is achieved, which significantly improves the antioxidant performance, inhibits the oxidative synthesis of melanin, promotes cell growth, and has a good scar removal effect.
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Figure CN119587414A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of cosmetics, and in particular to a stable and sustained-release antioxidant skin care composition emulsion, a preparation method thereof, and an application thereof. Background Art
[0002] With the rapid development of the cosmetics market, consumers are increasingly demanding greater efficacy and safety. Animal-derived active ingredients are commonly used in cosmetics, but they are increasingly being phased out due to their high cost and biosafety concerns. As a low-cost, no-harmful-residue alternative, nanobubble technology has become a research hotspot in the cosmetics field due to its unique physical and chemical properties, particularly its advantages in skin penetration and active ingredient release.
[0003] Nanobubbles can carry high concentrations of antioxidant gases (such as oxygen or hydrogen) and react directly with free radicals in the skin, quickly neutralizing them and reducing oxidative damage. At the same time, the small size of nanobubbles (20 to 200 nanometers) and the large specific surface area increase the contact area between antioxidant gases and free radicals, thereby further improving antioxidant efficiency. Furthermore, the tiny size and high kinetic energy of nanobubbles give them excellent skin permeability, allowing them to easily penetrate the skin barrier and bring antioxidants and active ingredients deep into the skin, increasing their utilization rate. By interacting with skin cells, nanobubbles can promote cellular absorption of antioxidants and enhance their efficacy. Furthermore, nanobubbles can form a stable dispersion system in cosmetics, reducing the degradation and inactivation of active ingredients, improving their stability in the formula, and effectively isolating oxygen and pollutants in the air, further protecting antioxidant ingredients.
[0004] While nanobubbles can improve the stability of the overall composition, they can still rupture under significant external forces, resulting in a decrease in the stability of the cosmetic. Furthermore, the substances currently encapsulated by nanobubbles have low antioxidant properties and lack a sustained-release effect, preventing them from providing long-term skin care. This results in cosmetics with limited effectiveness and no longer meets market requirements.
[0005] Therefore, how to improve the stability of cosmetics while improving their skin care effects has become a technical problem that needs to be urgently solved in this field. Summary of the Invention
[0006] The object of the present invention is to provide a stable sustained-release antioxidant skin care composition emulsion and its preparation method and application. The stable sustained-release antioxidant skin care composition emulsion provided by the present invention contains chitosan microcapsules, has a good sustained-release effect, and can maintain the skin for a long time. At the same time, the antioxidant skin care composition emulsion has a good antioxidant effect, can significantly inhibit the oxidative synthesis of melanin, and the antioxidant skin care composition emulsion can promote cell growth, which can help eliminate scars.
[0007] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:
[0008] The present invention provides a stable and sustained-release antioxidant skin care composition emulsion, which comprises, by mass percentage, 1.2-2.5% of a resveratrol-ATP nanoparticle complex, 1.0-3.0% of chitosan microcapsules, 0.8-2.3% of an active component, 7.2-14% of a stabilizing component, and the balance, nanobubble water;
[0009] The active components include tea tree oil, sodium hyaluronate and beta-glucan; the stabilizing components include glycerol, ethanol and carbomer;
[0010] The resveratrol-ATP nanoparticle complex and tea tree oil are coated inside the chitosan microcapsule.
[0011] Preferably, the mass ratio of resveratrol to ATP nanoparticles in the resveratrol-ATP nanoparticle complex is 1:(2-6).
[0012] Preferably, the particle size of the ATP nanoparticles is ≤75 nm.
[0013] Preferably, the active ingredients include 0.2-0.8% tea tree oil, 0.5-1.0% sodium hyaluronate and 0.1-0.5% β-glucan.
[0014] Preferably, the stabilizing component includes 3-8% glycerol, 4-5% ethanol and 0.2-1.0% carbomer.
[0015] Preferably, the pH value of the stable sustained-release antioxidant skin care composition emulsion is 5.5-6.0; the viscosity of the stable sustained-release antioxidant skin care composition emulsion is 2500-4000 mPa·s.
[0016] The present invention provides a method for preparing the stable sustained-release antioxidant skin care composition emulsion described in the above technical solution, comprising the following steps:
[0017] (1) mixing a resveratrol ethanol solution and an ATP aqueous solution, performing nano-processing, and then volatilizing the ethanol to obtain a resveratrol-ATP nanoparticle solution;
[0018] (2) mixing chitosan and acetic acid solution, and then adding phosphate buffer to obtain a chitosan solution;
[0019] (3) mixing the resveratrol-ATP nanoparticle solution obtained in step (1), the chitosan solution obtained in step (2), and tea tree oil to obtain a chitosan microcapsule composite solution;
[0020] (4) The chitosan microcapsule composite solution obtained in step (3), nano bubble water, sodium hyaluronate, β-glucan, glycerol, ethanol and carbomer are mixed to obtain a stable sustained-release antioxidant skin care composition emulsion.
[0021] Preferably, in step (1), the concentration of the resveratrol ethanol solution is 2-3 mmol / L, the concentration of the ATP aqueous solution is 4-6 mmol / L, and the volume ratio of the resveratrol ethanol solution to the ATP aqueous solution is 1:(0.5-1.5).
[0022] Preferably, the preparation method of nano bubble water in step (4) is: placing distilled water into a pressurized chamber, then introducing gas to the pressurized chamber until the pressure is 2 to 5 MPa, maintaining the pressure for 40 to 100 minutes, and then reducing the pressure to normal pressure at a pressure reduction rate of 0.1 MPa / min to obtain nano bubble water.
[0023] The present invention provides the use of the stable sustained-release antioxidant skin care composition emulsion described in the above technical solution or the stable sustained-release antioxidant skin care composition emulsion prepared by the preparation method described in the above technical solution in cosmetics.
[0024] The present invention provides a stable and sustained-release antioxidant skin care composition emulsion, which comprises, by mass percentage, 1.2-2.5% of a resveratrol-ATP nanoparticle complex, 1.0-3.0% of chitosan microcapsules, 0.8-2.3% of an active component, 7.2-14% of a stabilizing component, and the balance of nanobubble water; the active components comprise tea tree oil, sodium hyaluronate, and beta-glucan; the stabilizing component comprises glycerol, ethanol, and carbomer; the resveratrol-ATP nanoparticle complex and the tea tree oil are coated inside the chitosan microcapsules. The present invention uses nanobubbles as a template. The compounding of resveratrol and ATP nanoparticles can improve the water solubility of resveratrol, which is beneficial for the effective ingredients to exert anti-inflammatory, cell viability-enhancing and antioxidant effects. At the same time, the reducing property of the nanobubbles themselves further enhances the antioxidant effect. At the same time, the chitosan microcapsules can coat the resveratrol-ATP nanoparticles and tea tree oil to form a stable assembly system, which can integrate the solubilization of active ingredients with functional sustained release. The outermost layer of chitosan is antibacterial and anti-inflammatory. ATP has a two-stage hydrolysis and plays a more diverse role in regulating the solubility and release of resveratrol. The base combines with the encapsulated resveratrol through the π-π action to inhibit its oxidation and maintain its antioxidant function. Each component used for sustained release is functional. In this way, the antioxidant skin care composition emulsion can have a long-lasting skin care effect. The results of the examples show that in the resveratrol-ATP nanoparticle complex provided by the present invention, the particle size of the nanoparticles is mainly distributed within 50 nm, the antioxidant skin care composition emulsion has a good antioxidant effect on dopa molecules, and can significantly inhibit the oxidative synthesis of melanin. At the same time, the antioxidant skin care composition emulsion of the present invention can promote cell growth and can help eliminate scars. BRIEF DESCRIPTION OF THE DRAWINGS
[0025] Figure 1 This is a particle size distribution diagram of ATP nanoparticles used in Example 1 of the present invention;
[0026] Figure 2 This is a comparison curve of the antioxidant and melanin synthesis inhibition effects of the resveratrol-ATP nanoparticles obtained in step (1) of Example 1 of the present invention;
[0027] Figure 3 This is a cell distribution diagram after adding the antioxidant skin care composition emulsion provided in Example 1 of the present invention;
[0028] Figure 4 is the cell distribution diagram after adding PBS;
[0029] Figure 5 The inhibitory effect of the skin care compositions prepared in Example 1 and Comparative Examples 1 to 3 on melanin synthesis;
[0030] Figure 6The cell viability effects of the skin care compositions prepared in Example 1 and Comparative Examples 1 to 3. DETAILED DESCRIPTION
[0031] The present invention provides a stable and sustained-release antioxidant skin care composition emulsion, which comprises, by mass percentage, 1.2-2.5% of a resveratrol-ATP nanoparticle complex, 1.0-3.0% of chitosan microcapsules, 0.8-2.3% of an active component, 7.2-14% of a stabilizing component, and the balance, nanobubble water;
[0032] The active components include tea tree oil, sodium hyaluronate and beta-glucan; and the stabilizing components include glycerin, ethanol and carbomer.
[0033] In the present invention, unless otherwise specified, the raw materials used are commercially available products well known to those skilled in the art.
[0034] In terms of mass percentage, the stable sustained-release antioxidant skin care composition emulsion provided by the present invention includes 1.2 to 2.5% of a resveratrol-ATP nanoparticle complex, preferably 1.3 to 1.9%. In the present invention, the resveratrol-ATP nanoparticle complex is preferably formed by combining resveratrol and ATP nanoparticles through a π-π interaction. In the present invention, the mass ratio of resveratrol to ATP nanoparticles is preferably 1: (2 to 6), more preferably 1: (3 to 5), and further preferably 1: (4 to 4.5). In the present invention, resveratrol and ATP nanoparticles can form a resveratrol-ATP nanocomplex, thereby further enhancing the strong antioxidant and whitening effects of the stable sustained-release antioxidant skin care composition emulsion.
[0035] Based on the total mass percentage of the stable sustained-release antioxidant skin care composition emulsion as 100%, the resveratrol is preferably 0.2 to 0.5%, more preferably 0.3 to 0.4%. In the present invention, resveratrol has excellent antioxidant, anti-inflammatory and anti-aging properties. Resveratrol can neutralize free radicals, reduce the damage of oxidative stress to skin cells, thereby delaying skin aging. At the same time, resveratrol can inhibit the activity of tyrosinase, reduce melanin production, improve skin spots and pigmentation, and resveratrol can reduce the generation of inflammatory mediators, reduce skin inflammatory reactions, and is suitable for the care of sensitive skin. In addition, resveratrol can promote the synthesis of collagen, improve skin elasticity and firmness, and reduce the appearance of fine lines and wrinkles. The present invention, through the addition of resveratrol, can not only make the antioxidant skin care composition emulsion have good antioxidant, anti-inflammatory and anti-aging properties, but also can avoid the excessive cost caused by excessive use of resveratrol.
[0036] Based on the total mass percentage of the stable sustained-release antioxidant skin care composition emulsion as 100%, the ATP nanoparticles are preferably 1.0-2.0%, more preferably 1.2-1.5%; the particle size of the ATP nanoparticles is preferably ≤75nm, more preferably 15-50nm. In the present invention, ATP (adenosine triphosphate) nanoparticles have the effects of promoting skin cell energy metabolism, cell repair and anti-aging. In terms of promoting skin cell energy metabolism, ATP nanoparticles can provide energy for biological reaction processes, which can significantly improve the energy status of skin cells and improve skin health and appearance; in terms of cell repair and regeneration, ATP participates in the proliferation and repair process of cells, helping to accelerate the regeneration of skin cells and tissue repair; in terms of anti-aging, ATP can activate the AMPK signaling pathway in skin cells, enhance the antioxidant defense capacity of cells, and reduce the damage to the skin caused by oxidative stress. ATP can also regulate the calcium ion balance in cells, maintain the normal function and structure of cells, and delay the aging process of the skin.
[0037] The present invention provides a stable sustained-release antioxidant skin care composition emulsion comprising 1.0 to 3.0% chitosan microcapsules, preferably 1.5 to 2.5%, and more preferably 2.0 to 2.2% by mass. The chitosan microcapsules can form a protective film on the skin surface, reducing water evaporation, enhancing the skin barrier function, and promoting deep penetration of active ingredients. Chitosan also has an inhibitory effect on various bacteria and fungi, reducing the risk of skin infection. Chitosan can also accelerate wound healing, reduce scar formation, and provide excellent moisturizing effects.
[0038] In the present invention, the resveratrol-ATP nanoparticle complex and tea tree oil are encapsulated within chitosan microcapsules. The chitosan microcapsules preferably have a particle size of 80 to 150 nm, more preferably 90 to 120 nm, and even more preferably 100 nm. By utilizing chitosan microcapsules to encapsulate the resveratrol-ATP nanoparticle complex and tea tree oil, the present invention provides excellent protection and sustained release, further improving the overall stability and delivery efficiency of the skin care composition, achieving long-lasting protection.
[0039] By mass percentage, the stable sustained-release antioxidant skin care composition emulsion provided by the present invention includes 0.8 to 2.3% of active ingredients, preferably 1.2 to 1.8%, and more preferably 1.6%. In the present invention, the active ingredients include tea tree oil, sodium hyaluronate and β-glucan. In the present invention, the active ingredients are used to improve the antibacterial and anti-inflammatory, deep moisturizing and immunity capabilities of the skin care composition. Tea tree oil is a natural antibacterial and anti-inflammatory ingredient that can help reduce skin inflammation and infection; sodium hyaluronate (i.e., sodium hyaluronate) can provide deep moisturizing and enhance skin elasticity; β-glucan can enhance the skin's natural immunity and help resist external microbial invasion.
[0040] Based on the total weight percentage of the stable sustained-release antioxidant skin care composition emulsion as 100%, the active ingredients preferably include 0.2-0.8% tea tree oil, 0.5-1.0% sodium hyaluronate, and 0.1-0.5% beta-glucan, and more preferably 0.5% tea tree oil, 0.8% sodium hyaluronate, and 0.3% beta-glucan. The present invention utilizes a combination of these three ingredients to achieve a synergistic effect, further enhancing the skin care effect of the stable sustained-release antioxidant skin care composition emulsion when used as a cosmetic.
[0041] The stable, sustained-release antioxidant skin care composition emulsion provided by the present invention comprises, by mass percentage, 7.2 to 14%, preferably 8 to 12%, and more preferably 9.9% of a stabilizing component. In the present invention, the stabilizing component comprises glycerin, ethanol, and carbomer. In the present invention, the stabilizing component is used to maintain system stability and emulsification stability, thereby increasing the effective life of the stable, sustained-release antioxidant skin care composition emulsion. Glycerin is a humectant that can increase skin hydration; ethanol is used as a solvent and preservative to ensure system stability; and carbomer has good emulsifying properties, which can improve emulsification stability and provide a good skin feel.
[0042] Based on the total weight percentage of the stable sustained-release antioxidant skin care composition emulsion as 100%, the stabilizing components preferably include 3-8% glycerin, 4-5% ethanol, and 0.2-1.0% carbomer, preferably 5% glycerin, 4.5% ethanol, and 0.4% carbomer. The present invention further improves system stability and emulsion stability by combining these three components.
[0043] The stable, sustained-release antioxidant skin care composition emulsion provided by the present invention includes, by weight percentage, a balance of nanobubble water. The nanobubble water contains a large number of nanobubbles. The nanobubbles' tiny size and high kinetic energy enable them to easily penetrate the skin barrier, delivering skin care ingredients deep into the skin, thereby increasing their utilization. Furthermore, the nanobubbles form a stable dispersion within the product, reducing degradation and inactivation of active ingredients and improving stability, thereby facilitating product storage. During storage and use, the nanobubbles effectively isolate oxygen and pollutants from the air, further protecting the antioxidant ingredients.
[0044] The stable, sustained-release antioxidant skin care composition emulsion provided by the present invention preferably also includes phosphate and acetic acid. The specific amounts of phosphate and acetic acid used are not particularly limited and can be added based on the actual needs of chitosan solution preparation. A small amount has little effect on the performance of the stable, sustained-release antioxidant skin care composition emulsion.
[0045] In the present invention, the pH value of the stable sustained-release antioxidant skin care composition emulsion is preferably 6.5 to 7.0; the viscosity of the stable sustained-release antioxidant skin care composition emulsion is preferably 2500 to 4000 mPa·s, more preferably 3000 to 3500 mPa·s. In the present invention, when the pH value of the stable sustained-release antioxidant skin care composition emulsion does not meet the above requirements, the present invention preferably adds disodium hydrogen phosphate and / or citric acid to adjust the pH value. The present invention has no special limitation on the specific amount of the disodium hydrogen phosphate and / or citric acid, as long as the pH value of the stable sustained-release antioxidant skin care composition emulsion meets the requirements. The present invention can avoid irritation to the skin by controlling the pH value and viscosity of the stable sustained-release antioxidant skin care composition emulsion, and at the same time, can avoid the skin care composition being difficult to apply when applied.
[0046] The present invention uses nanobubbles as a template. The compounding of resveratrol and ATP nanoparticles can improve the water solubility of resveratrol, which is beneficial for the effective ingredients to exert anti-inflammatory, cell viability-enhancing and antioxidant effects. At the same time, the reducing property of the nanobubbles themselves further enhances the antioxidant effect. At the same time, the chitosan microcapsules can coat the resveratrol-ATP nanoparticles and tea tree oil to form a stable assembly system, which can integrate the solubilization of active ingredients with functional sustained release. The outermost layer of chitosan is antibacterial and anti-inflammatory. ATP has a two-stage hydrolysis and plays a more diverse role in regulating the solubility and release of resveratrol. The base combines with the encapsulated resveratrol through the π-π action to inhibit its oxidation and maintain its antioxidant function. Each component used for sustained release is functional. In this way, the antioxidant skin care composition emulsion can have a long-lasting skin care effect.
[0047] The present invention also provides a method for preparing the stable sustained-release antioxidant skin care composition emulsion described in the above technical solution, comprising the following steps:
[0048] (1) mixing a resveratrol ethanol solution and an ATP aqueous solution, performing nano-processing, and then volatilizing the ethanol to obtain a resveratrol-ATP nanoparticle solution;
[0049] (2) mixing chitosan and acetic acid solution, and then adding phosphate buffer to obtain a chitosan solution;
[0050] (3) mixing the resveratrol-ATP nanoparticle solution obtained in step (1), the chitosan solution obtained in step (2), and tea tree oil to obtain a chitosan microcapsule composite solution;
[0051] (4) The chitosan microcapsule composite solution obtained in step (3), nano bubble water, sodium hyaluronate, β-glucan, glycerol, ethanol and carbomer are mixed to obtain a stable sustained-release antioxidant skin care composition emulsion.
[0052] The invention mixes a resveratrol ethanol solution and an ATP aqueous solution, performs nano-processing, and then volatilizes the ethanol to obtain a resveratrol-ATP nanoparticle solution.
[0053] In the present invention, the concentration of the resveratrol ethanol solution is preferably 2-3 mmol / L, more preferably 2.5 mmol / L; the concentration of the ATP aqueous solution is preferably 4-6 mmol / L, more preferably 5 mmol / L; and the volume ratio of the resveratrol ethanol solution to the ATP aqueous solution is preferably 1:(0.5-1.5), more preferably 1:(0.8-1.2), and even more preferably 1:1. The present invention uses ethanol and water as solvents. Due to the different solubility of air in water and ethanol, a large number of nanobubbles can be generated during mixing, thereby increasing the nanobubble content in the solution.
[0054] In the present invention, the nano-processing method is preferably ultrasonic dispersion. The present invention has no particular restrictions on the power and time of the ultrasonic dispersion, as long as the particle size of the ATP nanoparticles meets the requirements. The present invention can reduce the particle size of ATP by ultrasonic dispersion to obtain ATP nanoparticles.
[0055] In the present invention, the method for volatilizing the ethanol is preferably vacuuming. The present invention does not specifically limit the specific operation and parameters of the vacuuming, and can be set according to vacuuming and volatilization operations well known to those skilled in the art. By volatilizing the ethanol, the present invention can avoid excessive ethanol content causing irritation to the skin.
[0056] The invention mixes chitosan and acetic acid solution, and then adds phosphate buffer solution to obtain chitosan solution.
[0057] In the present invention, the acetic acid solution is preferably an aqueous solution of acetic acid. The present invention has no particular limitation on the concentration and amount of the acetic acid solution, as long as chitosan can be completely dissolved in the acetic acid solution and the concentration of acetic acid in the chitosan solution meets the requirements.
[0058] In the present invention, the chitosan and acetic acid solution are preferably mixed by magnetic stirring. The present invention does not particularly limit the specific rate of the magnetic stirring, and can be determined according to the technical common sense of those skilled in the art. The present invention can accelerate the dissolution of chitosan by magnetic stirring.
[0059] In the present invention, the concentration of the phosphate buffer is preferably 0.01 mol / L. The present invention does not particularly limit the specific amount of the phosphate buffer (PBS) used, as long as the concentrations of chitosan and acetic acid in the chitosan solution meet the requirements. In the present invention, the concentration of chitosan in the chitosan solution is preferably 15 to 30 mg / mL, more preferably 20 to 25 mg / mL; the mass concentration of acetic acid in the chitosan solution is preferably 0.5 to 1.5%, more preferably 1%. By controlling the concentration of chitosan, the present invention facilitates the subsequent formation of chitosan microcapsules.
[0060] After obtaining the resveratrol-ATP nanoparticle solution and the chitosan solution, the present invention mixes the resveratrol-ATP nanoparticle solution, the chitosan solution and tea tree oil to obtain a chitosan microcapsule composite solution.
[0061] In the present invention, the resveratrol-ATP nanoparticle solution, chitosan solution and tea tree oil are preferably mixed in a manner that the resveratrol-ATP nanoparticle solution and tea tree oil are first mixed, and then the chitosan solution is added dropwise. The present invention does not particularly limit the rate of addition, and can be determined according to the technical common sense of those skilled in the art. The present invention is mixed in the above manner. During the addition of the chitosan solution, the chitosan will coat the resveratrol-ATP nanoparticles and tea tree oil in the solution, thereby forming chitosan microcapsules, thereby further improving the stability of the system and improving the transfer efficiency.
[0062] In the present invention, the particle size of the chitosan microcapsules in the chitosan microcapsule composite solution is preferably 80 to 150 nm, more preferably 90 to 120 nm, and even more preferably 100 nm.
[0063] After obtaining the chitosan microcapsule composite solution, the present invention mixes the chitosan microcapsule composite solution, nano bubble water, sodium hyaluronate, β-glucan, glycerol, ethanol and carbomer to obtain a stable and sustained-release antioxidant skin care composition emulsion.
[0064] In the present invention, the nanobubble water is preferably prepared in a nanobubble generating apparatus comprising a pressurization chamber, a slow decompression device, and a gas supply system. The present invention does not specifically limit the specific source of the nanobubble generating apparatus; commercially available products familiar to those skilled in the art can be used.
[0065] In the present invention, the method for preparing nanobubble water is preferably as follows: distilled water is placed in a pressurized chamber, gas is introduced to the chamber until the pressure reaches 2-5 MPa, the pressure is maintained for 40-100 minutes, and then the pressure is reduced to atmospheric pressure at a rate of 0.1 MPa / min to produce the nanobubble water. In the present invention, the gas is preferably nitrogen or air; the pressure is maintained for 60 minutes; and the pressure reduction is preferably achieved using a slow decompression device. In the present invention, the gas is first fully dissolved in the distilled water by applying a high pressure. During the decompression process, the supersaturated dissolved gas is gradually released, thereby forming nanobubbles and producing the nanobubble water.
[0066] In the present invention, the nanobubble water is preferably stored at low temperatures or with the addition of a stabilizer. The low-temperature storage temperature is preferably 1-4°C, more preferably 1-3°C, and even more preferably 1-2°C. The stabilizer is preferably vitamin C or glycerin. The specific amount of the stabilizer is not particularly limited; it only needs to be sufficient to maintain the nanobubble water at room temperature and pressure. This storage method prevents the nanobubbles in the nanobubble water from escaping or bursting.
[0067] The present invention has no particular limitation on the specific amount of the nanobubble water, as long as the total amount of the nanobubble water in the stable and sustained-release antioxidant skin care composition emulsion meets the requirements.
[0068] In the present invention, the chitosan microcapsule composite solution, nanobubble water, sodium hyaluronate, β-glucan, glycerol, ethanol, and carbomer are preferably mixed by high-speed stirring at low temperature. In the present invention, the low temperature is preferably 2-5°C, more preferably 4°C; the high-speed stirring rate is preferably 800-1200 r / min, more preferably 1000 r / min. The present invention does not specifically limit the time for high-speed stirring, as long as it can form a uniform emulsion. This method can avoid affecting the nanobubbles during the mixing process.
[0069] In the present invention, the chitosan microcapsule composite solution, nanobubble water, sodium hyaluronate, β-glucan, glycerol, ethanol, and carbomer are preferably mixed by first mixing the chitosan microcapsule composite solution and nanobubble water, then adding sodium hyaluronate, β-glucan, glycerol, and ethanol, and finally adding carbomer. The present invention ensures uniform mixing of the components by adding the raw materials stepwise.
[0070] In the present invention, the pH value of the stable sustained-release antioxidant skin care composition emulsion is preferably 6.5-7.0; the viscosity of the stable sustained-release antioxidant skin care composition emulsion is preferably 2500-4000 mPa·s, more preferably 3000 mPa·s.
[0071] The present invention mixes resveratrol and ATP and then performs nano-processing, so that the ATP particle size can be reduced and the ATP can be better compounded with resveratrol to form a resveratrol-ATP nanoparticle composite structure. Then, tea tree oil and chitosan are added. Chitosan will coat the resveratrol-ATP nanoparticles and tea tree oil in the process of forming chitosan microcapsules, thereby forming chitosan microcapsules with a coated structure of about 100 nm. The stability and skin absorption efficiency of the active ingredients are enhanced by nano-encapsulation technology and chitosan microcapsule technology. At the same time, antibacterial and anti-inflammatory ingredients are combined to achieve multiple skin care effects. Finally, nano-bubble water and other active ingredients and stabilizing components are added, so that the nano-bubble water has a good stability effect at room temperature, which can not only enable the skin care composition to be stored for a long time, but also the small size and high kinetic energy of the nano-bubbles enable them to easily penetrate the skin barrier, bring the skin care ingredients into the deep layers of the skin, and improve their utilization rate.
[0072] The preparation method provided by the present invention is simple, and the equipment used are all conventional equipment in the field, and no new equipment needs to be introduced, thereby reducing costs and being conducive to large-scale industrial promotion.
[0073] The present invention also provides the use of the stable sustained-release antioxidant skin care composition emulsion described in the above technical solution, or the stable sustained-release antioxidant skin care composition emulsion prepared by the preparation method described in the above technical solution, in cosmetics. The present invention does not particularly limit the specific method of such application, and the application can be carried out according to the technical common sense of those skilled in the art.
[0074] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions of the present invention. Obviously, the embodiments described are only some of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.
[0075] Example 1
[0076] A stable and sustained-release antioxidant skin care composition emulsion, comprising, by mass percentage, 1.5% resveratrol-ATP nanoparticle complex, 2.0% chitosan microcapsules, 1.6% active ingredient, 9.9% stabilizing ingredient, and the balance nanobubble water;
[0077] The resveratrol-ATP nanoparticle complex is formed by combining resveratrol and ATP nanoparticles through a π-π interaction; the mass ratio of resveratrol to ATP nanoparticles is 1:4, i.e., resveratrol is 0.3% and ATP nanoparticles are 1.2%; the chitosan microcapsule is coated with the resveratrol-ATP nanoparticle complex and tea tree oil;
[0078] The active components include 0.5% tea tree oil, 0.8% hyaluronic acid sodium salt and 0.3% beta-glucan; and the stabilizing components include 5% glycerol, 4.5% ethanol and 0.4% carbomer.
[0079] The preparation method of the stable sustained-release antioxidant skin care composition emulsion is as follows:
[0080] (1) A 2.5 mmol / L resveratrol ethanol solution and a 5 mmol / L ATP aqueous solution were mixed in a volume ratio of 1:1 and then nanosized by ultrasonic dispersion to reduce the particle size of ATP to less than 50 nm. The ethanol was then evaporated by vacuum extraction to obtain a resveratrol-ATP nanoparticle solution.
[0081] (2) chitosan and acetic acid aqueous solution were mixed and magnetically stirred until the chitosan was completely dissolved, and then 0.01 mol / L phosphate buffer was added until the concentration of chitosan in the solution was 20 mg / mL and the mass concentration of acetic acid was 1%, thereby obtaining a chitosan solution;
[0082] (3) mixing the resveratrol-ATP nanoparticle solution obtained in step (1) with tea tree oil, and then adding dropwise the chitosan solution obtained in step (2) to obtain a chitosan microcapsule composite solution; the particle size of the chitosan microcapsules in the chitosan microcapsule composite solution is about 100 nm;
[0083] (4) firstly mixing the chitosan microcapsule composite solution obtained in step (3) with nanobubble water, then adding sodium hyaluronate, β-glucan, glycerol and ethanol, and finally adding carbomer to obtain a stable sustained-release antioxidant skin care composition emulsion; the above mixing is carried out under high-speed stirring at low temperature, and the low temperature is 4°C;
[0084] The nanobubble water is prepared in a nanobubble generating device; the nanobubble generating device includes a pressurizing chamber, a slow decompression device, and a gas supply system. The nanobubble water preparation method comprises: placing distilled water in the pressurizing chamber, then introducing air to a pressure of 5 MPa in the pressurizing chamber, maintaining the pressure for 60 minutes to allow the gas to fully dissolve in the distilled water, then reducing the pressure in the pressurizing chamber to normal pressure at a rate of 0.1 MPa / min using the slow decompression device, to obtain the nanobubble water; and storing the nanobubble water at a low temperature of less than 4°C.
[0085] After testing, the pH value of the stable and sustained-release antioxidant skin care composition emulsion is 6.5; the viscosity of the stable and sustained-release antioxidant skin care composition emulsion is 3000 mPa·s, which is suitable for skin use.
[0086] The particle size distribution of ATP nanoparticles in the resveratrol-ATP nanoparticle solution obtained in step (1) of Example 1 was detected. The detection method was as follows: the resveratrol-ATP nanoparticle solution was evaporated to obtain resveratrol-ATP nanoparticle colloid, and then the resveratrol-ATP nanoparticle colloid was dispersed in distilled water, and the agglomerates were broken by ultrasonic treatment to ensure that the particles were evenly dispersed to obtain a sample. Then, 1.5 mL of the prepared sample was added to a cuvette, water was used as the solvent, the temperature was set to 25° C., and a Malvern particle size analyzer was started for measurement. The results of each measurement were recorded, including key indicators such as the particle size distribution curve, the average particle size, and the polydispersity index. The particle size distribution results of the ATP nanoparticles finally obtained are as follows: Figure 1 As shown. Figure 1 It can be seen that the ATP nanoparticles used in the present invention are mainly distributed within 50 nm.
[0087] The antioxidant and melanin synthesis inhibitory effects of the resveratrol-ATP nanoparticles obtained in step (1) of Example 1 were tested. The test method was as follows: a mixed solution of DOPA (1 mmol / L) and tyrosinase (0.1 mg / mL) (the solvent was 0.01 mol / L phosphate buffer) was used to simulate the in vivo melanin oxidation synthesis process, and then resveratrol-ATP nanoparticles were added (so that the concentration of resveratrol-ATP nanoparticles in the mixed solution was 1.5 wt.%). Dynamic monitoring of the absorbance of the mixed solution showed a significant co-assembly-induced antioxidant effect on the DOPA molecule. The control group did not add resveratrol-ATP nanoparticles. The results obtained are as follows: Figure 2 When resveratrol-ATP nanoparticles (1.5 wt.%) were added, the absorbance remained low, while the absorbance without resveratrol-ATP nanoparticles was higher, indicating that the oxidative synthesis of melanin was significantly inhibited after the addition of resveratrol-ATP nanoparticles.
[0088] The effect of the antioxidant skin care composition emulsion provided in Example 1 on cell viability was tested by seeding L929 fibroblasts at an appropriate density into a culture dish containing RPMI-1640 basal medium. The cells were cultured in a 37°C, 5% CO2 humidity incubator. The experimental group was treated with 1 / 10 volume of the antioxidant skin care composition emulsion, while the control group was treated with an equal amount of PBS. The cells were cultured for 24 hours. The results obtained at the same magnification were as follows: Figure 3 and Figure 4 As shown, Figure 3 The cell distribution after adding the antioxidant skin care composition emulsion, Figure 4 is the cell distribution after adding equal amount of PBS. Figure 3 and Figure 4 It can be seen from the comparison that after adding the antioxidant skin care composition emulsion provided by the present invention, the cell proliferation of the experimental group was significantly accelerated, indicating that the antioxidant skin care composition emulsion provided by the present invention can improve cell viability and accelerate cell reproduction.
[0089] Comparative Example 1
[0090] A skin care composition, comprising, by mass percentage, 1.5% resveratrol, 2.0% chitosan microcapsules, 1.6% active ingredient, 9.9% stabilizing ingredient, and the balance nanobubble water;
[0091] The chitosan microcapsules are coated with resveratrol and tea tree oil;
[0092] The active components include 0.5% tea tree oil, 0.8% hyaluronic acid sodium salt and 0.3% beta-glucan; and the stabilizing components include 5% glycerol, 4.5% ethanol and 0.4% carbomer.
[0093] The preparation method of the skin care composition is:
[0094] (1) A 2.5 mmol / L resveratrol ethanol solution and water were mixed in a volume ratio of 1:1 and then ultrasonically dispersed to obtain a resveratrol solution;
[0095] (2) chitosan and acetic acid aqueous solution were mixed and magnetically stirred until the chitosan was completely dissolved, and then 0.01 mol / L phosphate buffer was added until the concentration of chitosan in the solution was 20 mg / mL and the mass concentration of acetic acid was 1%, thereby obtaining a chitosan solution;
[0096] (3) mixing the resveratrol solution obtained in step (1) with tea tree oil, and then adding dropwise the chitosan solution obtained in step (2) to obtain a chitosan microcapsule composite solution;
[0097] (4) First, the chitosan microcapsule composite solution obtained in step (3) is mixed with the nanobubble water, and then sodium hyaluronate, β-glucan, glycerol and ethanol are added and mixed, and finally carbomer is added and mixed to obtain a skin care composition; the above mixing is carried out under high-speed stirring at a low temperature, and the low temperature is 4°C; the preparation method of the nanobubble water is the same as that in Example 1.
[0098] Comparative Example 2
[0099] A skin care composition, comprising, by mass percentage, 1.5% ATP nanoparticles, 2.0% chitosan microcapsules, 1.6% active ingredients, 9.9% stabilizing ingredients, and the balance nanobubble water;
[0100] The chitosan microcapsules are coated with ATP nanoparticles and tea tree oil;
[0101] The active components include 0.5% tea tree oil, 0.8% hyaluronic acid sodium salt and 0.3% beta-glucan; and the stabilizing components include 5% glycerol, 4.5% ethanol and 0.4% carbomer.
[0102] The preparation method of the skin care composition is:
[0103] (1) Ethanol and a 5 mmol / L ATP aqueous solution were mixed in a volume ratio of 1:1 and then subjected to nano-processing by ultrasonic dispersion to reduce the particle size of ATP to less than 50 nm. The ethanol was then evaporated by vacuum extraction to obtain an ATP nanoparticle solution.
[0104] (2) chitosan and acetic acid aqueous solution were mixed and magnetically stirred until the chitosan was completely dissolved, and then 0.01 mol / L phosphate buffer was added until the concentration of chitosan in the solution was 20 mg / mL and the mass concentration of acetic acid was 1%, thereby obtaining a chitosan solution;
[0105] (3) mixing the ATP nanoparticle solution obtained in step (1) with tea tree oil, and then adding dropwise the chitosan solution obtained in step (2) to obtain a chitosan microcapsule composite solution;
[0106] (4) First, the chitosan microcapsule composite solution obtained in step (3) is mixed with the nanobubble water, and then sodium hyaluronate, β-glucan, glycerol and ethanol are added and mixed, and finally carbomer is added and mixed to obtain a skin care composition; the above mixing is carried out under high-speed stirring at a low temperature, and the low temperature is 4°C; the preparation method of the nanobubble water is the same as that in Example 1.
[0107] Comparative Example 3
[0108] A skin care composition, comprising, by mass percentage, 1.5% of a resveratrol-ATP nanoparticle complex, 2.0% of chitosan microcapsules, 1.6% of an active ingredient, 9.9% of a stabilizing ingredient, and the balance being distilled water;
[0109] The resveratrol-ATP nanoparticle complex is formed by combining resveratrol and ATP nanoparticles through a π-π interaction; the mass ratio of resveratrol to ATP nanoparticles is 1:4, i.e., resveratrol is 0.3% and ATP nanoparticles are 1.2%; the chitosan microcapsule is coated with the resveratrol-ATP nanoparticle complex and tea tree oil;
[0110] The active components include 0.5% tea tree oil, 0.8% hyaluronic acid sodium salt and 0.3% beta-glucan; and the stabilizing components include 5% glycerol, 4.5% ethanol and 0.4% carbomer.
[0111] The preparation method of the skin care composition is:
[0112] (1) A 2.5 mmol / L resveratrol ethanol solution and a 5 mmol / L ATP aqueous solution were mixed in a volume ratio of 1:1 and then nanosized by ultrasonic dispersion to reduce the particle size of ATP to less than 50 nm. The ethanol was then evaporated by vacuum extraction to obtain a resveratrol-ATP nanoparticle solution.
[0113] (2) chitosan and acetic acid aqueous solution were mixed and magnetically stirred until the chitosan was completely dissolved, and then 0.01 mol / L phosphate buffer was added until the concentration of chitosan in the solution was 20 mg / mL and the mass concentration of acetic acid was 1%, thereby obtaining a chitosan solution;
[0114] (3) mixing the resveratrol-ATP nanoparticle solution obtained in step (1) with tea tree oil, and then adding dropwise the chitosan solution obtained in step (2) to obtain a chitosan microcapsule composite solution; the particle size of the chitosan microcapsules in the chitosan microcapsule composite solution is about 100 nm;
[0115] (4) First, the chitosan microcapsule composite solution obtained in step (3) is mixed with distilled water, and then sodium hyaluronate, β-glucan, glycerol and ethanol are added and mixed, and finally carbomer is added and mixed to obtain a skin care composition; the above mixing is carried out under conditions of high-speed stirring at low temperature, and the low temperature is 4°C.
[0116] The melanin synthesis inhibition effect of the skin care compositions prepared in Example 1 and Comparative Examples 1 to 3 was tested. The test method was as follows: a mixed solution of DOPA (1 mmol / L) and tyrosinase (0.1 mg / mL) (the solvent was 0.01 mol / L phosphate buffer) was used to simulate the melanin oxidation synthesis process in vivo. The mixed solution was then divided into four equal groups, and 1 / 10 volume of the skin care compositions provided in Example 1 and Comparative Examples 1 to 3 was added to each of the four mixed solutions. After 1500 minutes, the absorbance of the mixed solution was tested. The results are shown in FIG. Figure 5 As shown. Figure 5 It can be seen that after the skin care composition provided by the present invention is added, the absorbance of the mixed solution is the lowest, indicating that the skin care composition provided by the present invention has the most obvious inhibitory effect on the oxidative synthesis of melanin, while the absorbance of Comparative Example 2 is the highest, indicating that the skin care composition has the worst inhibitory effect on the oxidative synthesis of melanin after omitting the addition of resveratrol.
[0117] The cell viability effect of the skin care compositions prepared in Example 1 and Comparative Examples 1 to 3 was tested. The test method was as follows: 4 groups of equal amounts of fibroblasts L929 were inoculated at the same density into culture dishes containing RPMI-1640 basal medium, and the cells were then cultured in a 37°C, 5% CO2 humidity incubator. Subsequently, 1 / 10 volume of the skin care compositions prepared in Example 1 and Comparative Examples 1 to 3 were added and cultured for 24 hours. Finally, the number of fibroblasts L929 in the culture dish was calculated, and the number of fibroblasts L929 was used to characterize cell viability. The calculation method of cell viability is shown in Formula I: Q = M / M1 * 100%, Formula I; in Formula I, Q represents cell viability, M is the number of fibroblasts L929 obtained after culturing for 24 hours after adding the skin care composition, and M1 is the number of fibroblasts L929 obtained after culturing for 24 hours after adding the skin care composition provided in Example 1. The final results are shown in FIG. Figure 6 As shown. Figure 6 It can be seen that after the addition of the antioxidant skin care composition emulsion provided by the present invention, the number of fibroblasts L929 in the culture dish is the largest, while in Comparative Example 1, after the addition of ATP is lacking, the number of cells is the least, and in Comparative Example 2, after the addition of resveratrol is lacking, the number of cells is slightly higher than that of Comparative Example 1. After the nanobubble water is changed to distilled water, the number of cells in Comparative Example 3 is slightly lower than that in Example 1. By comparison, it can be seen that after the skin care composition provided in Example 1 of the present invention is added, the cell proliferation is the fastest, indicating that the antioxidant skin care composition emulsion provided by the present invention can significantly improve cell viability and accelerate cell reproduction through the composite synergistic effect of ATP, resveratrol and nanobubble water.
[0118] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as within the scope of protection of the present invention.
Claims
1. A stable sustained-release antioxidant skin care composition emulsion, comprising, by mass percentage: Resveratrol-ATP nanoparticle complex 1.2-2.5%, chitosan microcapsule 1.0-3.0%, active component 0.8-2.3%, stabilizing component 7.2-14% and the balance nanobubble water; The active components include tea tree oil, sodium hyaluronate and β-glucan; the stabilizing components include glycerol, ethanol and carbomer; The resveratrol-ATP nanoparticle complex and tea tree oil are coated inside the chitosan microcapsule.
2. The stable sustained-release antioxidant skin care composition emulsion according to claim 1, characterized in that: The mass ratio of resveratrol to ATP nanoparticles in the resveratrol-ATP nanoparticle complex is 1:(2-6).
3. The stable sustained-release antioxidant skin care composition emulsion according to claim 2, characterized in that: The particle size of the ATP nanoparticles is ≤75nm.
4. The stable sustained-release antioxidant skin care composition emulsion according to claim 1, characterized in that: The active components include 0.2-0.8% tea tree oil, 0.5-1.0% sodium hyaluronate and 0.1-0.5% beta-glucan.
5. The stable sustained-release antioxidant skin care composition emulsion according to claim 1, characterized in that: The stabilizing components include 3-8% glycerol, 4-5% ethanol and 0.2-1.0% carbomer.
6. The stable sustained-release antioxidant skin care composition emulsion according to claim 1, characterized in that: The pH value of the stable sustained-release antioxidant skin care composition emulsion is 5.5-6.0; the viscosity of the stable sustained-release antioxidant skin care composition emulsion is 2500-4000 mPa·s.
7. A method for preparing the stable sustained-release antioxidant skin care composition emulsion according to any one of claims 1 to 6, comprising the following steps: (1) mixing a resveratrol ethanol solution and an ATP aqueous solution, performing nano-processing, and then volatilizing the ethanol to obtain a resveratrol-ATP nanoparticle solution; (2) mixing chitosan and acetic acid solution, and then adding phosphate buffer to obtain a chitosan solution; (3) mixing the resveratrol-ATP nanoparticle solution obtained in step (1), the chitosan solution obtained in step (2), and tea tree oil to obtain a chitosan microcapsule composite solution; (4) The chitosan microcapsule composite solution obtained in step (3), nano bubble water, sodium hyaluronate, β-glucan, glycerol, ethanol and carbomer are mixed to obtain a stable sustained-release antioxidant skin care composition emulsion.
8. The preparation method according to claim 7, characterized in that: In the step (1), the concentration of the resveratrol ethanol solution is 2-3 mmol / L, the concentration of the ATP aqueous solution is 4-6 mmol / L, and the volume ratio of the resveratrol ethanol solution to the ATP aqueous solution is 1:(0.5-1.5).
9. The preparation method according to claim 7, characterized in that: The preparation method of the nano bubble water in step (4) is as follows: distilled water is placed in a pressurized chamber, gas is introduced into the pressurized chamber until the pressure is 2 to 5 MPa, the pressure is maintained for 40 to 100 minutes, and then the pressure is reduced to normal pressure at a pressure reduction rate of 0.1 MPa / min to obtain nano bubble water.
10. Use of the stable sustained-release antioxidant skin care composition emulsion according to any one of claims 1 to 6 or the stable sustained-release antioxidant skin care composition emulsion prepared by the preparation method according to any one of claims 7 to 9 in cosmetics.