A highly active, stable, sustained-release composition and its use in skin care products
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- COSHIM COSMETICS (SHANGHAI) CO LTD
- Filing Date
- 2023-12-14
- Publication Date
- 2026-07-24
AI Technical Summary
The stability and effectiveness of active ingredients in existing skincare products are insufficient, and they are affected by factors such as light, temperature, pH, metal ions, oxidants, reducing agents and microorganisms. Existing encapsulation technologies have limited effectiveness.
Using fragmented porous silica as a carrier, active components such as blue copper peptide, gentian extract, and retinol are synthesized and encapsulated through a specific method to form a highly active and stable sustained-release composition. The porosity is improved by treating straw powder and ionic liquid, and the encapsulation effect is enhanced by combining anionic surfactants.
It effectively reduces the impact of light, temperature, pH, metal ions, oxidants and microorganisms on active ingredients, achieving sustained release of active ingredients and improving the stability and safety of skin care products.
Smart Images
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Abstract
Description
Technical Field
[0001] This application relates to the field of skincare technology, and more specifically, to a highly active, stable sustained-release composition and its application in skincare products. Background Technology
[0002] Skin is the body's first line of defense, most vulnerable to external environmental influences that can lead to damage, inflammation, or aging. With the rapid development of the skincare industry and people's increasing understanding of the importance of skincare, skincare knowledge is constantly growing, and the demand for effective skincare products is increasing year by year. The importance of the stability and effectiveness of active ingredients in skincare products is self-evident.
[0003] There are many factors that affect the stability of skincare products, such as:
[0004] 1. Light
[0005] Many ingredients become unstable under light exposure, mainly because certain wavelengths of light (such as ultraviolet light) promote oxidation, causing natural pigments to fade (e.g., lycopene, carotene), antioxidants (e.g., astaxanthin, grape seed extract), and discoloration. Therefore, skincare products often need to be stored away from light, and transparent containers should be used as little as possible.
[0006] 2. Temperature
[0007] For every 10°C increase in temperature, the rate of rancidity increases by 2-4 times. Furthermore, high temperatures accelerate the hydrolysis of fatty acids, providing growth conditions for microorganisms and thus exacerbating rancidity. In addition, high temperatures can affect the activity of active ingredients; for example, at temperatures above 50°C, β-arbutin accelerates its decomposition into hydroquinone. Therefore, β-arbutin should not be added at high temperatures during the production process. Skincare products can undergo accelerated high-temperature testing to observe changes in stability.
[0008] 3. pH value
[0009] Each ingredient has its own suitable pH range. If it's outside this range, its efficacy will be affected. For example, the same amount of fruit acid will have different effects in formulations with different pH levels. Some active ingredients (such as vitamin C, which is less prone to inactivation at pH < 4) will have significantly reduced efficacy if their pH is outside their suitable range. Cross-linked polymers (such as carbomer) require the addition of alkaline ingredients to neutralize them and adjust the pH to the appropriate level before they can exert their thickening effect. When designing the pH control range for skincare products, it should be as close as possible to the skin's natural pH, that is, slightly acidic or neutral (pH 5-7). A slightly acidic environment can also help cosmetics resist the invasion of external microorganisms.
[0010] 4. Metal ions
[0011] The main ions are copper, lead, zinc, aluminum, iron, nickel, manganese, and chromium. Some metal ions can significantly reduce the efficacy of existing or added antioxidants, while others can spontaneously oxidize and become catalysts for reactions. For example, 2 μg / g of iron ions can almost completely destroy the antioxidant activity of phenolic and quinone antioxidants. Furthermore, metal ions can disrupt the thickening system of a formula, causing irreversible changes in viscosity / hardness, thus affecting the consumer experience. In skincare product formulation, metal ion chelating agents (EDTA-2Na or sodium phytate) are typically added. Through the strong binding of the chelating agent molecules to the metal ions, the metal ions are encapsulated within the chelating agent, becoming stable compounds with larger molecular weights, thereby preventing the metal ions from exerting their effects.
[0012] 5. Oxidizing agents and reducing agents
[0013] Oxygen is the most common oxidant and a major, unavoidable factor causing oxidation or deterioration of raw materials. For example, betaine and betaine glycosides are easily degraded in the presence of oxygen. The reducing agent ascorbic acid has a good stabilizing effect on capsanthin; compared to the blank control, the absorbance of capsanthin solutions with added ascorbic acid decreases more slowly over time, and the higher the concentration of ascorbic acid, the stronger the degradation-retarding effect. Therefore, cosmetics need to be stored in airtight containers to minimize contact with air.
[0014] 6. Other
[0015] There are many other factors that affect the stability of cosmetics, such as preservatives (if there are none or insufficient preservatives, microorganisms will grow and the product will deteriorate), water activity (water activity affects microorganisms and the oxidation of oils), fragrance (its main function is to produce a pleasant smell and mask the smell of the product base; some fragrances may not be able to mask the smell of the raw materials over time), and so on.
[0016] In existing technologies, active ingredients in skincare products are mostly protected using encapsulation technology, which is often achieved through carriers such as cyclodextrins or liposomes. However, the encapsulation effect of cyclodextrins is limited, mainly affecting powder-like substances; while encapsulation with liposomes requires specialized equipment (such as high-pressure homogenizers), resulting in significant production limitations. Furthermore, the stability improvement effect of active ingredients encapsulated by carriers such as cyclodextrins or liposomes is limited. The stability of existing products with high levels of added active ingredients has not been well resolved. Based on the above, this application provides a highly active, stable, sustained-release composition and its application in skincare products. Summary of the Invention
[0017] To address the issues of poor stability and efficacy in products with high levels of added active ingredients, this application provides a highly active, stable, sustained-release composition and its application in skincare products.
[0018] In a first aspect, this application provides a highly active, stable sustained-release composition, employing the following technical solution:
[0019] A highly active, stable sustained-release composition comprising an active component and a carrier;
[0020] The active ingredients include at least one of the following: copper peptide, acetyl tetrapeptide-9, acetyl hexapeptide-8, gentian extract, witch hazel extract, aloe vera extract, yeast extract, hydrolyzed collagen, retinol, astaxanthin, lycopene, and superoxide dismutase.
[0021] The carrier is fragmented porous silica;
[0022] The mass ratio of the active component to the carrier is 1:18-20.
[0023] Preferably, the active components include copper peptide, gentian extract and retinol in a mass ratio of 1:3-5:8-11.
[0024] Preferably, the fractured porous silica is prepared by the following method:
[0025] S1. Control the mass ratio of straw powder, acetic acid aqueous solution, and ionic liquid to 1:8-10:0.3-0.5. After pretreating the straw powder with acetic acid aqueous solution, add ionic liquid and sonicate to obtain mixture I.
[0026] S2. Control the mass ratio of tetraethyl orthosilicate, 3-aminopropyltrihydroxysilane, and ethanol aqueous solution to 4-5:1-2:7-10. Add tetraethyl orthosilicate and 3-aminopropyltrihydroxysilane to the ethanol aqueous solution and stir to mix evenly to obtain mixture II.
[0027] S3. Mix mixture I and mixture II with anionic surfactant, let stand to precipitate, take the precipitate and calcine to obtain fragmented porous silica.
[0028] Preferably, the straw powder in step S1 is obtained by crushing corn straw or rice straw and passing it through a 300-350 mesh sieve.
[0029] Preferably, the ionic liquid in step S1 is 1-butyl-3-methylimidazolium acetate and / or 1-butyl-3-methylimidazolium hexafluorophosphate.
[0030] Preferably, the ionic liquid comprises 1-butyl-3-methylimidazolium acetate and 1-butyl-3-methylimidazolium hexafluorophosphate in a mass ratio of 1-3:1.
[0031] Preferably, the anionic surfactant in step S3 is sodium fatty alcohol polyoxyethylene ether sulfate and / or sodium dodecyl sulfate.
[0032] Preferably, the anionic surfactant comprises sodium fatty alcohol polyoxyethylene ether sulfate and sodium dodecyl sulfate in a mass ratio of 4-6:1.
[0033] Preferably, the calcination conditions in step S3 are: calcination temperature of 450-550℃ and calcination time of 3-5h in a nitrogen atmosphere.
[0034] Preferably, the composition is prepared by the following method:
[0035] The active component is dispersed in a solvent and dissolved by stirring at room temperature at a speed of 800-1000 r / min. Then, broken porous silica is added and the mixture is stirred and mixed for 1-2 hours to ensure that the broken porous silica uniformly coats the active component. Finally, the mixture is freeze-dried for 24 hours at a temperature of -30℃ and a vacuum of 5 Pa.
[0036] Secondly, this application provides an application of a highly active, stable sustained-release composition in skincare products, employing the following technical solution:
[0037] Application of a highly active, stable sustained-release composition in the preparation of skin care products.
[0038] In summary, this application has the following beneficial effects:
[0039] This application utilizes fragmented porous silica to encapsulate active ingredients such as copper peptides, gentian extract, and retinol, effectively solving the problems of easy inactivation and instability of active ingredients. The resulting composition, when used as an additive in skincare products, can effectively reduce the impact of light, temperature, pH, metal ions, oxidants, reducing agents, and microorganisms on the skincare product system itself. The fragmented porous silica of this application not only protects the high activity of active ingredients but also achieves a sustained-release effect. When used as an additive in skincare products, the resulting composition can effectively ensure the stability and safety of the skincare products themselves.
[0040] This application uses straw powder as a biological template agent. The straw powder is treated sequentially with an aqueous acetic acid solution and an ionic liquid, which loosens the structure of the straw powder, increases its porosity and active sites, and allows it to interact more fully with the surface of the straw powder during subsequent silica synthesis, promoting the deposition and formation of silica and improving the formation of fragmented porous silica.
[0041] This application uses tetraethyl silicate and 3-aminopropyltrihydroxysilane as silicon sources and treated straw powder as a biotemplate. In the presence of anionic surfactants, fragmented porous silica is synthesized. The fragmented porous silica prepared in this application has low density, high porosity, loose internal structure, and excellent adsorption performance. It can encapsulate active components in various forms such as powder, water, and oil without the need for special equipment, control the release time of active components, achieve a sustained-release effect, and thus achieve a long-lasting effect in added skin care products. The fragmented porous silica of this application can also improve the stability of active components, reduce the dissolution or aggregation of active components during use, and help maintain the high activity and stable efficacy of active components. Detailed Implementation
[0042] The present application will be further described in detail below with reference to the embodiments.
[0043] Examples 1-5 provide a highly active, stable sustained-release composition and its application in skincare products.
[0044] Example 1
[0045] A highly active, stable sustained-release composition comprising an active component and a carrier in a mass ratio of 1:18; wherein the active component comprises copper peptide, gentian extract and retinol in a mass ratio of 1:3:8.
[0046] The carrier is fragmented porous silica, which is prepared by the following method:
[0047] S1. Control the mass ratio of straw powder, acetic acid aqueous solution, and ionic liquid to 1:8:0.3. Add 325 mesh rice straw powder to 2% acetic acid aqueous solution and stir at 450 r / min for 1 h at 50℃. Control the ultrasonic power to be 550 W and the ultrasonic frequency to be 48 kHz. Add ionic liquid and sonicate for 20 min to obtain mixture I. The ionic liquid includes 1-butyl-3-methylimidazolium acetate and 1-butyl-3-methylimidazolium hexafluorophosphate in a mass ratio of 1:1.
[0048] S2. Control the mass ratio of tetraethyl orthosilicate, 3-aminopropyltrihydroxysilane, and ethanol aqueous solution to 4:1:7. Add tetraethyl orthosilicate and 3-aminopropyltrihydroxysilane to 30% ethanol aqueous solution and stir at 450 r / min for 30 min to obtain mixture II.
[0049] S3. Control the amount of anionic surfactant added to be 2% of the total mass of mixture I and mixture II. Add anionic surfactant to mixture I and mixture II, stir and mix at 450 r / min for 1 h, let stand and precipitate for 6 h, take the precipitate and calcine at 450℃ for 5 h in a nitrogen atmosphere to obtain broken porous silica. The anionic surfactant includes sodium fatty alcohol polyoxyethylene ether sulfate and sodium dodecyl sulfate in a mass ratio of 4:1.
[0050] A highly active, stable sustained-release composition is prepared by the following method:
[0051] The mass ratio of the active component, carrier, and 1,3-butanediol aqueous solution was controlled at 1:18:50. The active component was dispersed in an 18% (w / w) 1,3-butanediol aqueous solution and dissolved by stirring at 800 r / min at room temperature. Then, broken porous silica was added and the mixture was stirred and mixed for 2 h to ensure that the broken porous silica uniformly coated the active component. Finally, the mixture was freeze-dried for 24 h at -30 °C and a vacuum of 5 Pa to obtain the desired highly active and stable sustained-release composition.
[0052] Example 2
[0053] A highly active, stable sustained-release composition comprising an active component and a carrier in a mass ratio of 1:18.5; wherein the active components are copper peptide, gentian extract and retinol in a mass ratio of 1:3:11.
[0054] The carrier is fragmented porous silica, which is prepared by the following method:
[0055] S1. Control the mass ratio of straw powder, acetic acid aqueous solution, and ionic liquid to 1:8:0.5. Add 325 mesh rice straw powder to acetic acid aqueous solution with a mass fraction of 2.2% and stir at 450 r / min for 1 h at 50℃. Control the ultrasonic power to be 550 W and the ultrasonic frequency to be 48 kHz. Add ionic liquid and sonicate for 20 min to obtain mixture I. The ionic liquid includes 1-butyl-3-methylimidazolium acetate and 1-butyl-3-methylimidazolium hexafluorophosphate with a mass ratio of 1.5:1.
[0056] S2. Control the mass ratio of tetraethyl orthosilicate, 3-aminopropyltrihydroxysilane, and ethanol aqueous solution to 5:1:7. Add tetraethyl orthosilicate and 3-aminopropyltrihydroxysilane to ethanol aqueous solution with a mass fraction of 32% and stir at 450 r / min for 30 min to obtain mixture II.
[0057] S3. Control the amount of anionic surfactant added to be 2.5% of the total mass of mixture I and mixture II. Add anionic surfactant to mixture I and mixture II, stir and mix at 450 r / min for 1 h, let stand and precipitate for 6.5 h, take the precipitate and calcine at 480℃ for 4.5 h in a nitrogen atmosphere to obtain broken porous silica. The anionic surfactant includes sodium fatty alcohol polyoxyethylene ether sulfate and sodium dodecyl sulfate in a mass ratio of 4.5:1.
[0058] A highly active, stable sustained-release composition is prepared by the following method:
[0059] The mass ratio of the active component, carrier, and 1,3-butanediol aqueous solution was controlled at 1:18.5:50. The active component was dispersed in an 18% (w / w) 1,3-butanediol aqueous solution and dissolved by stirring at 850 r / min at room temperature. Then, broken porous silica was added and the mixture was stirred and mixed for 1.8 h to ensure that the broken porous silica uniformly coated the active component. Finally, the mixture was freeze-dried for 24 h at -30 °C and a vacuum of 5 Pa to obtain the desired highly active and stable sustained-release composition.
[0060] Example 3
[0061] A highly active, stable sustained-release composition comprising an active component and a carrier in a mass ratio of 1:19; wherein the active component comprises copper peptide, gentian extract and retinol in a mass ratio of 1:4:10.
[0062] The carrier is fragmented porous silica, which is prepared by the following method:
[0063] S1. Control the mass ratio of straw powder, acetic acid aqueous solution, and ionic liquid to 1:9:0.4. Add 325 mesh rice straw powder to acetic acid aqueous solution with a mass fraction of 2.5% and stir at 450 r / min for 1 h at 50℃. Control the ultrasonic power to be 550 W and the ultrasonic frequency to be 48 kHz. Add ionic liquid and sonicate for 20 min to obtain mixture I. The ionic liquid includes 1-butyl-3-methylimidazolium acetate and 1-butyl-3-methylimidazolium hexafluorophosphate with a mass ratio of 2:1.
[0064] S2. Control the mass ratio of tetraethyl orthosilicate, 3-aminopropyltrihydroxysilane, and ethanol aqueous solution to 5:2:8. Add tetraethyl orthosilicate and 3-aminopropyltrihydroxysilane to ethanol aqueous solution with a mass fraction of 33% and stir at 450 r / min for 30 min to obtain mixture II.
[0065] S3. Control the amount of anionic surfactant added to be 3% of the total mass of mixture I and mixture II. Add anionic surfactant to mixture I and mixture II, stir and mix at 450 r / min for 1 h, let stand and precipitate for 7 h, take the precipitate and calcine at 500℃ for 4 h in a nitrogen atmosphere to obtain broken porous silica. The anionic surfactant includes sodium fatty alcohol polyoxyethylene ether sulfate and sodium dodecyl sulfate in a mass ratio of 5:1.
[0066] A highly active, stable sustained-release composition is prepared by the following method:
[0067] The mass ratio of the active component, carrier, and 1,3-butanediol aqueous solution was controlled at 1:19:50. The active component was dispersed in an 18% (w / w) 1,3-butanediol aqueous solution and stirred at 9000 r / min at room temperature until dissolved. Then, broken porous silica was added and the mixture was stirred and mixed for 1.5 h to ensure that the broken porous silica uniformly coated the active component. Finally, the mixture was freeze-dried at -30℃ and 5 Pa for 24 h to obtain the desired highly active and stable sustained-release composition.
[0068] Example 4
[0069] A highly active, stable sustained-release composition comprising an active component and a carrier in a mass ratio of 1:19.5; wherein the active component comprises copper peptide, gentian extract and retinol in a mass ratio of 1:5:8.
[0070] The carrier is fragmented porous silica, which is prepared by the following method:
[0071] S1. Control the mass ratio of straw powder, acetic acid aqueous solution, and ionic liquid to 1:10:0.3. Add 325 mesh rice straw powder to acetic acid aqueous solution with a mass fraction of 2.8% and stir at 450 r / min for 1 h at 50 °C. Control the ultrasonic power to be 550 W and the ultrasonic frequency to be 48 kHz. Add ionic liquid and sonicate for 20 min to obtain mixture I. The ionic liquid includes 1-butyl-3-methylimidazolium acetate and 1-butyl-3-methylimidazolium hexafluorophosphate with a mass ratio of 2.5:1.
[0072] S2. Control the mass ratio of tetraethyl orthosilicate, 3-aminopropyltrihydroxysilane, and ethanol aqueous solution to 4:1:10. Add tetraethyl orthosilicate and 3-aminopropyltrihydroxysilane to ethanol aqueous solution with a mass fraction of 34% and stir at 450 r / min for 30 min to obtain mixture II.
[0073] S3. Control the amount of anionic surfactant added to be 3.5% of the total mass of mixture I and mixture II. Add anionic surfactant to mixture I and mixture II, stir and mix at 450 r / min for 1 h, let stand and precipitate for 7.5 h, take the precipitate and calcine at 520℃ for 3.5 h in a nitrogen atmosphere to obtain broken porous silica. The anionic surfactant includes sodium fatty alcohol polyoxyethylene ether sulfate and sodium dodecyl sulfate in a mass ratio of 5.5:1.
[0074] A highly active, stable sustained-release composition is prepared by the following method:
[0075] The mass ratio of the active component, carrier, and 1,3-butanediol aqueous solution was controlled at 1:19.5:50. The active component was dispersed in an 18% (w / w) 1,3-butanediol aqueous solution and dissolved by stirring at 950 r / min at room temperature. Then, broken porous silica was added and the mixture was stirred and mixed for 1.2 h to ensure that the broken porous silica uniformly coated the active component. Finally, the mixture was freeze-dried for 24 h at -30 °C and a vacuum of 5 Pa to obtain the desired highly active and stable sustained-release composition.
[0076] Example 5
[0077] A highly active, stable sustained-release composition comprising an active component and a carrier in a mass ratio of 1:20; wherein the active component comprises copper peptide, gentian extract and retinol in a mass ratio of 1:5:11.
[0078] The carrier is fragmented porous silica, which is prepared by the following method:
[0079] S1. Control the mass ratio of straw powder, acetic acid aqueous solution, and ionic liquid to 1:10:0.5. Add 3% acetic acid aqueous solution to 325 mesh rice straw powder and stir at 450 r / min for 1 h at 50℃. Control the ultrasonic power to be 550 W and the ultrasonic frequency to be 48 kHz. Add ionic liquid and sonicate for 20 min to obtain mixture I. The ionic liquid includes 1-butyl-3-methylimidazolium acetate and 1-butyl-3-methylimidazolium hexafluorophosphate in a mass ratio of 3:1.
[0080] S2. Control the mass ratio of tetraethyl orthosilicate, 3-aminopropyltrihydroxysilane, and ethanol aqueous solution to 5:2:10. Add tetraethyl orthosilicate and 3-aminopropyltrihydroxysilane to ethanol aqueous solution with a mass fraction of 35% and stir at 450 r / min for 30 min to obtain mixture II.
[0081] S3. Control the amount of anionic surfactant added to be 4% of the total mass of mixture I and mixture II. Add anionic surfactant to mixture I and mixture II, stir and mix at 450 r / min for 1 h, let stand and precipitate for 8 h, take the precipitate and calcine at 550℃ for 3 h in a nitrogen atmosphere to obtain broken porous silica. The anionic surfactant includes sodium fatty alcohol polyoxyethylene ether sulfate and sodium dodecyl sulfate in a mass ratio of 6:1.
[0082] A highly active, stable sustained-release composition is prepared by the following method:
[0083] The mass ratio of the active component, carrier, and 1,3-butanediol aqueous solution was controlled at 1:20:50. The active component was dispersed in an 18% (w / w) 1,3-butanediol aqueous solution and stirred at 1000 r / min at room temperature until dissolved. Then, broken porous silica was added and the mixture was stirred and mixed for 1 h to ensure that the broken porous silica uniformly coated the active component. Finally, the mixture was freeze-dried at -30℃ and 5 Pa for 24 h to obtain the desired highly active and stable sustained-release composition.
[0084] To verify the overall performance of the highly active and stable sustained-release compositions prepared in Examples 1-5 of this application, the applicant has set up Comparative Examples 1-7, as follows:
[0085] Comparative Example 1
[0086] A highly active, stable sustained-release composition comprising an active component and a carrier in a mass ratio of 1:18; wherein the active component comprises copper peptide, gentian extract and retinol in a mass ratio of 1:3:8.
[0087] The carrier is fragmented porous silica, which is prepared by the following method:
[0088] S1. Control the mass ratio of straw powder, deionized water, and ionic liquid to 1:8:0.3. Add 325-mesh rice straw powder to deionized water and stir at 50°C and 450 r / min for 1 h. Control the ultrasonic power to 550 W and the ultrasonic frequency to 48 kHz. Add ionic liquid and sonicate for 20 min to obtain mixture I. The ionic liquid includes 1-butyl-3-methylimidazolium acetate and 1-butyl-3-methylimidazolium hexafluorophosphate in a mass ratio of 1:1.
[0089] S2. Control the mass ratio of tetraethyl orthosilicate, 3-aminopropyltrihydroxysilane, and ethanol aqueous solution to 4:1:7. Add tetraethyl orthosilicate and 3-aminopropyltrihydroxysilane to 30% ethanol aqueous solution and stir at 450 r / min for 30 min to obtain mixture II.
[0090] S3. Control the amount of anionic surfactant added to be 2% of the total mass of mixture I and mixture II. Add anionic surfactant to mixture I and mixture II, stir and mix at 450 r / min for 1 h, let stand and precipitate for 6 h, take the precipitate and calcine at 450℃ for 5 h in a nitrogen atmosphere to obtain broken porous silica. The anionic surfactant includes sodium fatty alcohol polyoxyethylene ether sulfate and sodium dodecyl sulfate in a mass ratio of 4:1.
[0091] A highly active, stable sustained-release composition is prepared by the following method:
[0092] The mass ratio of the active component, carrier, and 1,3-butanediol aqueous solution was controlled at 1:18:50. The active component was dispersed in an 18% (w / w) 1,3-butanediol aqueous solution and dissolved by stirring at 800 r / min at room temperature. Then, broken porous silica was added and the mixture was stirred and mixed for 2 h to ensure that the broken porous silica uniformly coated the active component. Finally, the mixture was freeze-dried for 24 h at -30 °C and a vacuum of 5 Pa to obtain the desired highly active and stable sustained-release composition.
[0093] Comparative Example 2
[0094] A highly active, stable sustained-release composition comprising an active component and a carrier in a mass ratio of 1:18; wherein the active component comprises copper peptide, gentian extract and retinol in a mass ratio of 1:3:8.
[0095] The carrier is fragmented porous silica, which is prepared by the following method:
[0096] S1. Control the mass ratio of straw powder, acetic acid aqueous solution, and 1-butyl-3-methylimidazolium acetate to 1:8:0.3. Add 325-mesh rice straw powder to 2% acetic acid aqueous solution and stir at 450 r / min for 1 h at 50℃. Control the ultrasonic power to be 550 W and the ultrasonic frequency to be 48 kHz. Add 1-butyl-3-methylimidazolium acetate and sonicate for 20 min to obtain mixture I.
[0097] S2. Control the mass ratio of tetraethyl orthosilicate, 3-aminopropyltrihydroxysilane, and ethanol aqueous solution to 4:1:7. Add tetraethyl orthosilicate and 3-aminopropyltrihydroxysilane to 30% ethanol aqueous solution and stir at 450 r / min for 30 min to obtain mixture II.
[0098] S3. Control the amount of anionic surfactant added to be 2% of the total mass of mixture I and mixture II. Add anionic surfactant to mixture I and mixture II, stir and mix at 450 r / min for 1 h, let stand and precipitate for 6 h, take the precipitate and calcine at 450℃ for 5 h in a nitrogen atmosphere to obtain broken porous silica. The anionic surfactant includes sodium fatty alcohol polyoxyethylene ether sulfate and sodium dodecyl sulfate in a mass ratio of 4:1.
[0099] A highly active, stable sustained-release composition is prepared by the following method:
[0100] The mass ratio of the active component, carrier, and 1,3-butanediol aqueous solution was controlled at 1:18:50. The active component was dispersed in an 18% (w / w) 1,3-butanediol aqueous solution and dissolved by stirring at 800 r / min at room temperature. Then, broken porous silica was added and the mixture was stirred and mixed for 2 h to ensure that the broken porous silica uniformly coated the active component. Finally, the mixture was freeze-dried for 24 h at -30 °C and a vacuum of 5 Pa to obtain the desired highly active and stable sustained-release composition.
[0101] Comparative Example 3
[0102] A highly active, stable sustained-release composition comprising an active component and a carrier in a mass ratio of 1:18; wherein the active component comprises copper peptide, gentian extract and retinol in a mass ratio of 1:3:8.
[0103] The carrier is fragmented porous silica, which is prepared by the following method:
[0104] S1. The mass ratio of straw powder, acetic acid aqueous solution, and 1-butyl-3-methylimidazolium hexafluorophosphate was controlled at 1:8:0.3. 325-mesh rice straw powder was added to 2% acetic acid aqueous solution and stirred at 450 r / min for 1 h at 50 °C. The ultrasonic power was controlled at 550 W and the ultrasonic frequency at 48 kHz. 1-butyl-3-methylimidazolium hexafluorophosphate was added and ultrasonically treated for 20 min to obtain mixture I.
[0105] S2. Control the mass ratio of tetraethyl orthosilicate, 3-aminopropyltrihydroxysilane, and ethanol aqueous solution to 4:1:7. Add tetraethyl orthosilicate and 3-aminopropyltrihydroxysilane to 30% ethanol aqueous solution and stir at 450 r / min for 30 min to obtain mixture II.
[0106] S3. Control the amount of anionic surfactant added to be 2% of the total mass of mixture I and mixture II. Add anionic surfactant to mixture I and mixture II, stir and mix at 450 r / min for 1 h, let stand and precipitate for 6 h, take the precipitate and calcine at 450℃ for 5 h in a nitrogen atmosphere to obtain broken porous silica. The anionic surfactant includes sodium fatty alcohol polyoxyethylene ether sulfate and sodium dodecyl sulfate in a mass ratio of 4:1.
[0107] A highly active, stable sustained-release composition is prepared by the following method:
[0108] The mass ratio of the active component, carrier, and 1,3-butanediol aqueous solution was controlled at 1:18:50. The active component was dispersed in an 18% (w / w) 1,3-butanediol aqueous solution and dissolved by stirring at 800 r / min at room temperature. Then, broken porous silica was added and the mixture was stirred and mixed for 2 h to ensure that the broken porous silica uniformly coated the active component. Finally, the mixture was freeze-dried for 24 h at -30 °C and a vacuum of 5 Pa to obtain the desired highly active and stable sustained-release composition.
[0109] Comparative Example 4
[0110] A highly active, stable sustained-release composition comprising an active component and a carrier in a mass ratio of 1:18; wherein the active component comprises copper peptide, gentian extract and retinol in a mass ratio of 1:3:8.
[0111] The carrier is fragmented porous silica, which is prepared by the following method:
[0112] S1. Control the mass ratio of straw powder, acetic acid aqueous solution, and ionic liquid to 1:8:0.3. Add 325 mesh rice straw powder to 2% acetic acid aqueous solution and stir at 450 r / min for 1 h at 50℃. Control the ultrasonic power to be 550 W and the ultrasonic frequency to be 48 kHz. Add ionic liquid and sonicate for 20 min to obtain mixture I. The ionic liquid includes 1-butyl-3-methylimidazolium acetate and 1-butyl-3-methylimidazolium hexafluorophosphate in a mass ratio of 1:1.
[0113] S2. Control the mass ratio of tetraethyl orthosilicate and ethanol aqueous solution to 5:7. Add tetraethyl orthosilicate to 30% ethanol aqueous solution and stir at 450 r / min for 30 min to obtain mixture II.
[0114] S3. Control the amount of anionic surfactant added to be 2% of the total mass of mixture I and mixture II. Add anionic surfactant to mixture I and mixture II, stir and mix at 450 r / min for 1 h, let stand and precipitate for 6 h, take the precipitate and calcine at 450℃ for 5 h in a nitrogen atmosphere to obtain broken porous silica. The anionic surfactant includes sodium fatty alcohol polyoxyethylene ether sulfate and sodium dodecyl sulfate in a mass ratio of 4:1.
[0115] A highly active, stable sustained-release composition is prepared by the following method:
[0116] The mass ratio of the active component, carrier, and 1,3-butanediol aqueous solution was controlled at 1:18:50. The active component was dispersed in an 18% (w / w) 1,3-butanediol aqueous solution and dissolved by stirring at 800 r / min at room temperature. Then, broken porous silica was added and the mixture was stirred and mixed for 2 h to ensure that the broken porous silica uniformly coated the active component. Finally, the mixture was freeze-dried for 24 h at -30 °C and a vacuum of 5 Pa to obtain the desired highly active and stable sustained-release composition.
[0117] Comparative Example 5
[0118] A highly active, stable sustained-release composition comprising an active component and a carrier in a mass ratio of 1:18; wherein the active component comprises copper peptide, gentian extract and retinol in a mass ratio of 1:3:8.
[0119] The carrier is fragmented porous silica, which is prepared by the following method:
[0120] S1. Control the mass ratio of straw powder, acetic acid aqueous solution, and ionic liquid to 1:8:0.3. Add 325 mesh rice straw powder to 2% acetic acid aqueous solution and stir at 450 r / min for 1 h at 50℃. Control the ultrasonic power to be 550 W and the ultrasonic frequency to be 48 kHz. Add ionic liquid and sonicate for 20 min to obtain mixture I. The ionic liquid includes 1-butyl-3-methylimidazolium acetate and 1-butyl-3-methylimidazolium hexafluorophosphate in a mass ratio of 1:1.
[0121] S2. Control the mass ratio of tetraethyl orthosilicate, 3-aminopropyltrihydroxysilane, and ethanol aqueous solution to 4:1:7. Add tetraethyl orthosilicate and 3-aminopropyltrihydroxysilane to 30% ethanol aqueous solution and stir at 450 r / min for 30 min to obtain mixture II.
[0122] S3. Control the amount of sodium fatty alcohol polyoxyethylene ether sulfate added to be 2% of the total mass of mixture I and mixture II. Add sodium fatty alcohol polyoxyethylene ether sulfate to mixture I and mixture II, stir and mix at 450 r / min for 1 h, let stand and precipitate for 6 h, take the precipitate and calcine it at 450℃ for 5 h in a nitrogen atmosphere to obtain broken porous silica.
[0123] A highly active, stable sustained-release composition is prepared by the following method:
[0124] The mass ratio of the active component, carrier, and 1,3-butanediol aqueous solution was controlled at 1:18:50. The active component was dispersed in an 18% (w / w) 1,3-butanediol aqueous solution and dissolved by stirring at 800 r / min at room temperature. Then, broken porous silica was added and the mixture was stirred and mixed for 2 h to ensure that the broken porous silica uniformly coated the active component. Finally, the mixture was freeze-dried for 24 h at -30 °C and a vacuum of 5 Pa to obtain the desired highly active and stable sustained-release composition.
[0125] Comparative Example 6
[0126] A highly active, stable sustained-release composition comprising an active component and a carrier in a mass ratio of 1:18; wherein the active component comprises copper peptide, gentian extract and retinol in a mass ratio of 1:3:8.
[0127] The carrier is fragmented porous silica, which is prepared by the following method:
[0128] S1. Control the mass ratio of straw powder, acetic acid aqueous solution, and ionic liquid to 1:8:0.3. Add 325 mesh rice straw powder to 2% acetic acid aqueous solution and stir at 450 r / min for 1 h at 50℃. Control the ultrasonic power to be 550 W and the ultrasonic frequency to be 48 kHz. Add ionic liquid and sonicate for 20 min to obtain mixture I. The ionic liquid includes 1-butyl-3-methylimidazolium acetate and 1-butyl-3-methylimidazolium hexafluorophosphate in a mass ratio of 1:1.
[0129] S2. Control the mass ratio of tetraethyl orthosilicate, 3-aminopropyltrihydroxysilane, and ethanol aqueous solution to 4:1:7. Add tetraethyl orthosilicate and 3-aminopropyltrihydroxysilane to 30% ethanol aqueous solution and stir at 450 r / min for 30 min to obtain mixture II.
[0130] S3. Control the amount of sodium dodecyl sulfate added to be 2% of the total mass of mixture I and mixture II. Add sodium dodecyl sulfate to mixture I and mixture II, stir and mix at 450 r / min for 1 h, let stand and precipitate for 6 h, take the precipitate and calcine it at 450℃ for 5 h in a nitrogen atmosphere to obtain broken porous silica.
[0131] A highly active, stable sustained-release composition is prepared by the following method:
[0132] The mass ratio of the active component, carrier, and 1,3-butanediol aqueous solution was controlled at 1:18:50. The active component was dispersed in an 18% (w / w) 1,3-butanediol aqueous solution and dissolved by stirring at 800 r / min at room temperature. Then, broken porous silica was added and the mixture was stirred and mixed for 2 h to ensure that the broken porous silica uniformly coated the active component. Finally, the mixture was freeze-dried for 24 h at -30 °C and a vacuum of 5 Pa to obtain the desired highly active and stable sustained-release composition.
[0133] Comparative Example 7
[0134] A highly active, stable sustained-release composition comprising an active component and a carrier in a mass ratio of 1:18; wherein the active component comprises copper peptide, gentian extract and retinol in a mass ratio of 1:3:8.
[0135] The carrier is fragmented porous silica, which is prepared by the following method:
[0136] S1. Control the mass ratio of straw powder, acetic acid aqueous solution, and ionic liquid to 1:8:0.3. Add 325 mesh rice straw powder to 2% acetic acid aqueous solution and stir at 450 r / min for 1 h at 50℃. Control the ultrasonic power to be 550 W and the ultrasonic frequency to be 48 kHz. Add ionic liquid and sonicate for 20 min to obtain mixture I. The ionic liquid includes 1-butyl-3-methylimidazolium acetate and 1-butyl-3-methylimidazolium hexafluorophosphate in a mass ratio of 1:1.
[0137] S2. Control the mass ratio of tetraethyl orthosilicate, 3-aminopropyltrihydroxysilane, and ethanol aqueous solution to 4:1:7. Add tetraethyl orthosilicate and 3-aminopropyltrihydroxysilane to 30% ethanol aqueous solution and stir at 450 r / min for 30 min to obtain mixture II.
[0138] S3. Control the amount of anionic surfactant added to be 2% of the total mass of mixture I and mixture II. Add anionic surfactant to mixture I and mixture II, stir and mix at 450 r / min for 1 h, let stand and precipitate for 6 h, take the precipitate and dry it at 100℃ to constant weight to obtain broken porous silica.
[0139] A highly active, stable sustained-release composition is prepared by the following method:
[0140] The mass ratio of the active component, carrier, and 1,3-butanediol aqueous solution was controlled at 1:18:50. The active component was dispersed in an 18% (w / w) 1,3-butanediol aqueous solution and dissolved by stirring at 800 r / min at room temperature. Then, broken porous silica was added and the mixture was stirred and mixed for 2 h to ensure that the broken porous silica uniformly coated the active component. Finally, the mixture was freeze-dried for 24 h at -30 °C and a vacuum of 5 Pa to obtain the desired highly active and stable sustained-release composition.
[0141] Performance testing
[0142] The stability and sustained-release properties of the highly active and stable sustained-release compositions in Examples 1-5 and Comparative Examples 1-7 of this application were tested respectively, and the results are shown in Table 1 below:
[0143] Stability test: Weigh 10g of the above composition sample and place it under -20℃, 5℃, 50℃, 50℃ (protected from light) and -20℃ / 50℃ (thermal and cold cycling) conditions for 90 days. The concentration of active component in the composition before and after placement was determined by HPLC and the residual rate was calculated. The results are shown in Table 1.
[0144] Sustained-release test: The dialysis bag method was used, and the specific steps were as follows: 2g of the composition was added to a dialysis bag (molecular cutoff 14kDa), the two ends of the dialysis bag were clamped, and then the bag was placed in 200mL of release medium (70% PBS buffer and 30% anhydrous ethanol) at 37℃ and pH 6.8. The mixture was slowly stirred for 24h at a constant temperature water bath of 37℃ and a stirring speed of 150r / min. At 0.5, 2, 4, 8, 12, and 30, 3mL of release medium was aspirated and 3mL of the same release medium was added. The absorbance of the 3mL of release medium aspirated at 0.5, 2, 4, 8, 12, and 30 was measured at 478nm using a 755B UV spectrophotometer, and the release amount of the active component was calculated. The specific calculation formula is as follows:
[0145] In the formula: C n The content of the composition measured at each time point is V0, where V0 is the sampling volume at each time point and V1 is the total volume of the released medium. The test results are shown in Table 2.
[0146] Table 1. Stability of the compositions in Examples 1-5 and Comparative Examples 1-7
[0147]
[0148]
[0149] As shown in Table 1 above, the high-activity, stable sustained-release compositions prepared in Examples 1-5 of this application have significantly improved stability compared with the compositions in Comparative Examples 1-7. The high-activity, stable sustained-release compositions prepared in Examples 1-5 of this application have excellent stability and can be stored stably for a long time.
[0150] Table 2 shows the stability of the compositions in Examples 1-5 and Comparative Examples 1-7.
[0151]
[0152] As shown in Table 2 above, the highly active and stable sustained-release compositions prepared in Examples 1-5 exhibit a significant sustained release effect, and their sustained-release performance is significantly better than that of the compositions prepared in Comparative Examples 1-7.
[0153] This specific embodiment is merely an explanation of this application and is not intended to limit it. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they fall within the scope of the claims of this application.
Claims
1. A highly active, stable sustained-release composition, characterized in that, Includes active components and carriers; The active ingredients include at least one of the following: copper peptide, acetyl tetrapeptide-9, acetyl hexapeptide-8, gentian extract, witch hazel extract, aloe vera extract, yeast extract, hydrolyzed collagen, retinol, astaxanthin, lycopene, and superoxide dismutase. The carrier is fragmented porous silica; The mass ratio of the active component to the carrier is 1:18-20; The fragmented porous silica is prepared by the following method: S1. Control the mass ratio of straw powder, acetic acid aqueous solution, and ionic liquid to 1:8-10:0.3-0.
5. After pretreating the straw powder with acetic acid aqueous solution, add ionic liquid and sonicate to obtain mixture I. S2. Control the mass ratio of tetraethyl orthosilicate, 3-aminopropyltrihydroxysilane, and ethanol aqueous solution to 4-5:1-2:7-10. Add tetraethyl orthosilicate and 3-aminopropyltrihydroxysilane to the ethanol aqueous solution and stir to mix evenly to obtain mixture II. S3. Mix mixture I and mixture II with anionic surfactant, let stand to precipitate, take the precipitate and calcine to obtain fragmented porous silica. The ionic liquid comprises 1-butyl-3-methylimidazolium acetate and 1-butyl-3-methylimidazolium hexafluorophosphate in a mass ratio of 1-3:1; The anionic surfactant comprises sodium fatty alcohol polyoxyethylene ether sulfate and sodium dodecyl sulfate in a mass ratio of 4-6:
1. The calcination conditions in step S3 are as follows: calcination temperature of 450-550℃ and calcination time of 3-5h in a nitrogen atmosphere.
2. The highly active, stable sustained-release composition according to claim 1, characterized in that, The active ingredients include copper peptide, gentian extract and retinol in a mass ratio of 1:3-5:8-11.
3. The highly active, stable sustained-release composition according to claim 1, characterized in that, The composition is prepared by the following method: The active component is dispersed in a solvent, stirred and dissolved at room temperature, then broken porous silica is added, and after continued stirring and mixing, it is freeze-dried to obtain the final product.
4. The use of a highly active, stable sustained-release composition as described in any one of claims 1-3 in the preparation of skin care products.