A skin care lyophilized powder containing collagen polypeptide and a preparation method thereof

Abstract

The application relates to the technical field of skin care products, and particularly discloses a skin care freeze-dried powder containing collagen polypeptides and a preparation method thereof. The freeze-dried powder comprises active components, synergistic repair polysaccharides, moisturizers, freeze-drying protectants and preservatives and the like. The core of the freeze-dried powder is that the active components are modified fish collagen peptides which are cross-linked by glutamine transaminase and modified by methyl pyrrolidone silanol ketone, so that the stability and biological activity of the product are significantly improved. Meanwhile, a specific compounded polysaccharide system of beta-glucan, tremella polysaccharide and sodium hyaluronate is adopted in the formula, and a moisturizer prepared by ultrasonic cross-linking of chondroitin sulfate and sodium alginate is adopted, so that the components synergistically act to jointly enhance the repair and moisturizing effects and use skin feeling of the product. The application also provides a corresponding preparation method. Through an optimized freeze-drying process, the problems of traditional freeze-dried powder, such as easy moisture absorption, single effect and poor reconstitution are effectively solved, and finally a skin care freeze-dried powder product with excellent comprehensive performance is obtained.

Description

Technical Field

[0001] This application relates to the field of skincare technology, and more specifically, to a skincare freeze-dried powder containing collagen peptides and its preparation method. Background Technology

[0002] With socio-economic development and increased consumer awareness of skincare, the skincare market is undergoing a transformation and upgrade from basic moisturizing to functional products such as high-efficiency repair and anti-aging. Against this backdrop, ingredients with clearly defined biological activities, especially those capable of repairing the skin barrier and delaying signs of aging, are increasingly becoming the focus of market and scientific research.

[0003] Collagen, the most important extracellular matrix structural protein in the dermis, forms a three-dimensional network scaffold that maintains skin elasticity and firmness. However, with age and the influence of external environmental factors, the synthesis rate of collagen in the human body slows down and its loss intensifies, leading to signs of aging such as sagging skin and wrinkles. Directly supplementing collagen was once the mainstream approach, but its large molecular structure makes it difficult to penetrate the stratum corneum, limiting its bioavailability. Therefore, research has turned its attention to its hydrolysis products—collagen peptides. Collagen peptides are small molecular weight fragments obtained from the enzymatic or chemical hydrolysis of collagen, typically with a molecular weight below several thousand Daltons, possessing superior skin permeability and absorption rate. Studies have shown that these small peptides not only provide moisturizing functions but also act as biosignaling molecules, promoting the proliferation and differentiation of skin fibroblasts, thereby efficiently stimulating the synthesis of endogenous collagen and elastin, achieving anti-wrinkle, firming, and deep repair effects from a mechanistic perspective.

[0004] Currently, the mainstream formulations of commercially available skincare products containing collagen peptides are still liquid serums, lotions, and creams. However, the long-term stability of this active ingredient in a liquid water-based system faces serious challenges: First, collagen peptides are prone to chemical degradation and hydrolysis in aqueous solutions, leading to a significant decrease in their biological activity over time; second, the nutrient-rich liquid environment provides a breeding ground for microorganisms, placing extremely high demands on the preservative system, while potent preservatives themselves may pose a risk of skin irritation; third, during production, storage, and transportation, light, oxygen, and temperature fluctuations can accelerate its inactivation process, resulting in a significant reduction in the actual efficacy of the product within its shelf life after opening.

[0005] To overcome the aforementioned stability challenges, freeze-drying technology has been introduced into the skincare industry. Freeze-dried powder formulations are produced by rapidly freezing the solution at extremely low temperatures, followed by direct sublimation of the ice crystals in a high-vacuum environment. This effectively removes moisture and "locks" the active ingredients in a dry, solid structure. This anhydrous state significantly inhibits chemical degradation and microbial growth, theoretically providing an ideal long-term preservation solution for unstable active ingredients such as collagen peptides.

[0006] Based on the above statements, this application proposes a skin care freeze-dried powder containing collagen peptides and its preparation method. Summary of the Invention

[0007] To address the common problems of single active ingredients, insufficient synergy, poor reconstitution performance, poor user experience, weak physical stability, and easy moisture absorption and clumping in currently available collagen peptide freeze-dried powders, this application provides a skin care freeze-dried powder containing collagen peptides and its preparation method.

[0008] In the first aspect, this application provides a skin care freeze-dried powder containing collagen peptides, using the following technical solution: A skin care freeze-dried powder containing collagen peptides is obtained by freeze-drying a freeze-dried liquid, wherein the freeze-dried liquid comprises the following raw materials in weight percentage: 6-10% active ingredients, 1-5% synergistic repair polysaccharides, 5-15% moisturizer, 10-20% freeze-drying protectant, 1-3% preservative, and the balance being deionized water. The active component is modified fish collagen peptide.

[0009] Preferably, the synergistic repair polysaccharide comprises β-glucan, tremella polysaccharide, and sodium hyaluronate in a mass ratio of 5-7:5-7:1.

[0010] Preferably, the moisturizer comprises glycerin, panthenol, and chondroitin sulfate cross-linked polymer in a mass ratio of 3-5:1-3:1.

[0011] Preferably, the chondroitin sulfate cross-linked polymer is prepared by the following method: chondroitin sulfate and sodium alginate are dissolved in water by stirring, the pH of the solution is adjusted to 4.8-5.6, stirring is continued, and ultrasonic cross-linking is performed while stirring. After the treatment is completed, the solution is spray-dried to obtain the chondroitin sulfate cross-linked polymer.

[0012] Preferably, the ultrasonic crosslinking conditions include: ultrasonic power of 150-350W, ultrasonic frequency of 60-160kHz, and crosslinking time of 15-35min.

[0013] Preferably, the spray drying conditions include: an inlet air temperature of 140-160℃, an outlet air temperature of 70-90℃, and a drying time of 2-4 hours.

[0014] Preferably, the freeze-drying protectant comprises trehalose, mannitol, and β-cyclodextrin in a mass ratio of 5-7:1-3:1.

[0015] Preferably, the preservative comprises white willow bark extract and anisic acid in a mass ratio of 2-4:1.

[0016] Preferably, the modified fish collagen peptide is prepared by the following method: after pretreating the fish collagen peptide powder, an enzyme is added for cross-linking modification to obtain a modification solution. After cooling the modification solution, a silanizing agent is added for site-specific modification. After purifying the site-specific modified product, it is spray-dried to obtain the modified fish collagen peptide.

[0017] Preferably, the specific preparation steps of the modified fish collagen peptide are as follows: Fish collagen peptide powder with a molecular weight of 2000-5000 Daltons is dissolved in deionized water to prepare a peptide solution with a mass concentration of 5-15%, and the pH is adjusted to 6.5-7.5; 0.03-0.05% of the total mass of the peptide solution is added to transglutaminase, and the mixture is stirred at 45-55℃ and pH 6.5-7.0 for 1-3 hours to obtain a modified solution; the modified solution is cooled to 25-35℃, and methylpyrrolidone silanolone with a molar ratio of 1:50-70 to the collagen peptide is added, and the mixture is stirred in the dark for 2-4 hours to obtain a modified reaction solution; the modified reaction solution is separated and purified using an ultrafiltration membrane with a molecular weight cutoff of 1000 Daltons, and the filtrate is collected; the inlet air temperature is set to 140-160℃ and the outlet air temperature to 60-70℃, and the mixture is spray-dried to constant weight to obtain the modified fish collagen peptide.

[0018] Secondly, this application provides a method for preparing a skin care freeze-dried powder containing collagen peptides, using the following technical solution: A method for preparing a skin care freeze-dried powder containing collagen peptides includes the following steps: S1. Weigh out the active ingredients, synergistic repair polysaccharides, moisturizer, freeze-drying protectant, preservative and deionized water according to the weight percentages mentioned above, and set aside for later use; S2. Heat deionized water to 70-80℃, add synergistic repair polysaccharide, moisturizer and preservative and stir to dissolve to obtain aqueous phase; S3. Cool the aqueous phase to 20-30℃, add the active component and freeze-drying protectant, and stir to dissolve; S4. Adjust the pH to 5.0-6.0 and cool to -50 to -40℃ to obtain pre-frozen material; S5. Heat the pre-frozen material to -10-0℃ under a vacuum of 10-30Pa and maintain for 1-2 hours. Then heat the pre-frozen material to 25-30℃ until the water content is less than 3%, and the skin care freeze-dried powder containing collagen peptides is obtained.

[0019] In summary, this application has the following beneficial effects: This application utilizes a unique process combining enzymatic cross-linking and silanization modification to prepare modified fish collagen peptides. This process not only effectively preserves the bioactivity that promotes collagen regeneration but also significantly enhances the product's stability, skin affinity, and compatibility in formulations, laying a solid foundation for the core efficacy of the freeze-dried powder.

[0020] To address the limitations of single active ingredients, this application innovatively constructs a synergistic repair polysaccharide system composed of β-glucan, tremella polysaccharide, and sodium hyaluronate in a specific ratio. This system, together with modified collagen peptides and a moisturizing network composed of cross-linked polymers of glycerol, panthenol, and chondroitin sulfate, produces multiple synergistic effects, achieving simultaneous enhancement of anti-aging, repair, moisturizing, and soothing effects, thus meeting the market's demand for comprehensive skincare solutions.

[0021] Regarding stability and user experience, this application designs a composite freeze-drying preservative system composed of trehalose, mannitol, and β-cyclodextrin in an optimized ratio. This system forms a stable network support structure during freeze-drying, ensuring the freeze-dried cakes are plump and porous. This not only significantly improves the product's physical stability, effectively preventing breakage or clumping due to vibration during transportation and storage, but also allows the freeze-dried powder to rapidly and completely reconstitute within tens of seconds of contact with water, greatly enhancing ease of use and user experience. Furthermore, the combination of white willow bark extract and anethole acid—a natural plant-based preservative—in the formula provides broad-spectrum and highly effective preservation while avoiding the irritation risks associated with traditional preservatives, making the product gentler and safer.

[0022] Finally, the preparation method of this application has clearly defined process parameters and a reasonable step design. In particular, the precise control of pre-freezing temperature, vacuum degree, and staged heating drying procedure ensures a high survival rate of active ingredients during the freeze-drying process and guarantees that the moisture content of the final product is consistently below 3%, achieving product quality uniformity and long-term storage stability, making it very suitable for large-scale industrial production. In summary, this application has successfully developed a collagen peptide skincare freeze-dried powder product with comprehensive efficacy, high stability, excellent user experience, and suitability for industrialization. Detailed Implementation

[0023] The present application will be further described in detail below with reference to embodiments. It should be understood that the specific embodiments described herein are only for explaining the present application and are not intended to limit the scope of the present application.

[0024] Where specific techniques or conditions are not specified in the examples, they shall be performed in accordance with the techniques or conditions described in the literature in this field, or in accordance with the product instructions. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased through legitimate channels.

[0025] Unless otherwise specified, the experimental methods used in the following embodiments are conventional methods. Unless otherwise specified, the experimental materials used in the following embodiments are commercially available products.

[0026] The white willow bark extract was purchased from Xi'an Lvtian Biotechnology Co., Ltd., CAS No.: 138-52-3; Anisic acid was purchased from Shandong Aowei Chemical Co., Ltd., CAS No.: 100-09-4; Fish collagen peptides were purchased from Xi'an Tianguangyuan Biotechnology Co., Ltd. The transglutaminase was purchased from Beijing Solarbio Technology Co., Ltd., CAS No.: 80146-85-6.

[0027] Examples 1-3 provide a skin care freeze-dried powder containing collagen peptides and its preparation method.

[0028] Example 1 A skin care freeze-dried powder containing collagen peptides is prepared by freeze-drying a freeze-dried liquid, wherein the freeze-dried liquid comprises the following raw materials by weight percentage: 6% active ingredient, 1% synergistic repair polysaccharide, 5% moisturizer, 10% freeze-drying protectant, 1% preservative, and the balance being deionized water.

[0029] The synergistic repair polysaccharides include β-glucan, Tremella fuciformis polysaccharide, and sodium hyaluronate in a mass ratio of 5:5:1.

[0030] The humectant comprises glycerin, panthenol, and chondroitin sulfate cross-linked polymer in a mass ratio of 3:1:1. The chondroitin sulfate cross-linked polymer is prepared by the following method: chondroitin sulfate and sodium alginate are dissolved in water by stirring, the pH of the solution is adjusted to 4.8, stirring is continued, and ultrasonic cross-linking is performed while stirring. The ultrasonic power is controlled at 150W, the ultrasonic frequency at 60kHz, and the cross-linking time at 35min. After the treatment is completed, the inlet air temperature is controlled at 140℃, the outlet air temperature at 70℃, and the product is spray-dried for 4h to obtain the chondroitin sulfate cross-linked polymer.

[0031] The freeze-drying protectant consists of trehalose, mannitol, and β-cyclodextrin in a mass ratio of 5:1:1.

[0032] The preservatives include white willow bark extract and anethole acid in a mass ratio of 2:1.

[0033] The active component is modified fish collagen peptide, and the modified fish collagen peptide is prepared by the following method: Fish collagen peptide powder with a molecular weight of 2000 Daltons was dissolved in deionized water to prepare a 5% (w / w) peptide solution, and the pH was adjusted to 6.5. 0.03% (w / w) of transglutaminase was added to the total peptide solution, and the mixture was stirred at 45°C and pH 6.5 for 1 hour to obtain a modified solution. The modified solution was cooled to 25°C, and methylpyrrolidone silanolone with a molar ratio of 1:50 to the collagen peptides was added. The mixture was stirred in the dark for 2 hours to obtain a modified reaction solution. The modified reaction solution was separated and purified using an ultrafiltration membrane with a molecular weight cutoff of 1000 Daltons, and the filtrate was collected. The inlet air temperature was set to 140°C and the outlet air temperature to 60°C, and the mixture was spray-dried to constant weight to obtain the modified fish collagen peptide.

[0034] A method for preparing a skin care freeze-dried powder containing collagen peptides includes the following steps: S1. Weigh out the active ingredients, synergistic repair polysaccharides, moisturizer, freeze-drying protectant, preservative and deionized water according to the weight percentages mentioned above, and set aside for later use; S2. Heat deionized water to 70°C, add synergistic repair polysaccharide, moisturizer and preservative and stir to dissolve to obtain aqueous phase; S3. Cool the aqueous phase to 20°C, add the active component and freeze-drying protectant, and stir to dissolve; S4. Adjust the pH to 5.0 and cool to -50℃ to obtain the pre-frozen material; S5. The pre-frozen material is heated to -10℃ under a vacuum of 10Pa and maintained for 1 hour. Then the pre-frozen material is heated to 25℃ until the water content is less than 3%, thus obtaining skin care freeze-dried powder containing collagen peptides.

[0035] Example 2 A skin care freeze-dried powder containing collagen peptides is prepared by freeze-drying a freeze-dried liquid, wherein the freeze-dried liquid comprises the following raw materials by weight percentage: 8% active ingredients, 3% synergistic repair polysaccharides, 10% moisturizer, 15% freeze-drying protectant, 2% preservative, and the balance being deionized water.

[0036] Among them, the synergistic repair polysaccharides include β-glucan, Tremella fuciformis polysaccharide and sodium hyaluronate in a mass ratio of 6:6:1.

[0037] The humectant comprises glycerin, panthenol, and chondroitin sulfate cross-linked polymer in a mass ratio of 4:2:1. The chondroitin sulfate cross-linked polymer is prepared by the following method: chondroitin sulfate and sodium alginate are dissolved in water by stirring, the pH of the solution is adjusted to 5.2, stirring is continued, and ultrasonic cross-linking is performed while stirring. The ultrasonic power is controlled at 250W, the ultrasonic frequency at 100kHz, and the cross-linking time at 25min. After the treatment is completed, the inlet air temperature is controlled at 150℃, the outlet air temperature at 80℃, and the product is spray-dried for 3h to obtain the chondroitin sulfate cross-linked polymer.

[0038] The freeze-drying protectant consists of trehalose, mannitol, and β-cyclodextrin in a mass ratio of 6:2:1.

[0039] The preservatives include white willow bark extract and anethole acid in a mass ratio of 3:1.

[0040] The active component is modified fish collagen peptide, and the modified fish collagen peptide is prepared by the following method: Fish collagen peptide powder with a molecular weight of 4000 Daltons was dissolved in deionized water to prepare a 10% peptide solution, and the pH was adjusted to 7.0. 0.04% of transglutaminase was added to the total peptide solution, and the mixture was stirred at 50℃ and pH 6.8 for 2 hours to obtain a modified solution. The modified solution was cooled to 30℃, and methylpyrrolidone silanolone with a molar ratio of 1:60 to the collagen peptides was added. The mixture was stirred in the dark for 3 hours to obtain a modified reaction solution. The modified reaction solution was separated and purified using an ultrafiltration membrane with a molecular weight cutoff of 1000 Daltons, and the filtrate was collected. The inlet air temperature was set to 150℃ and the outlet air temperature to 65℃, and the mixture was spray-dried to constant weight to obtain the modified fish collagen peptide.

[0041] A method for preparing a skin care freeze-dried powder containing collagen peptides includes the following steps: S1. Weigh out the active ingredients, synergistic repair polysaccharides, moisturizer, freeze-drying protectant, preservative and deionized water according to the weight percentages mentioned above, and set aside for later use; S2. Heat deionized water to 75°C, add synergistic repair polysaccharide, moisturizer and preservative and stir to dissolve to obtain aqueous phase; S3. Cool the aqueous phase to 25°C, add the active component and freeze-drying protectant, and stir to dissolve; S4. Adjust the pH to 5.5 and cool to -45℃ to obtain the pre-frozen material; S5. The pre-frozen material is heated to -5°C under a vacuum of 20Pa and maintained for 1.5 hours. Then the pre-frozen material is heated to 28°C until the water content is less than 3%, thus obtaining skin care freeze-dried powder containing collagen peptides.

[0042] Example 3 A skin care freeze-dried powder containing collagen peptides is obtained by freeze-drying a freeze-dried liquid, wherein the freeze-dried liquid comprises the following raw materials in weight percentage: 10% active ingredients, 5% synergistic repair polysaccharides, 15% moisturizer, 20% freeze-drying protectant, 3% preservative, and the balance being deionized water.

[0043] The synergistic repair polysaccharides include β-glucan, Tremella fuciformis polysaccharide, and sodium hyaluronate in a mass ratio of 7:7:1.

[0044] The humectant comprises glycerin, panthenol, and chondroitin sulfate cross-linked polymer in a mass ratio of 5:3:1. The chondroitin sulfate cross-linked polymer is prepared by the following method: chondroitin sulfate and sodium alginate are dissolved in water by stirring, the pH of the solution is adjusted to 5.6, stirring is continued, and ultrasonic cross-linking is performed while stirring. The ultrasonic power is controlled at 350W, the ultrasonic frequency at 160kHz, and the cross-linking time at 15min. After the treatment is completed, the inlet air temperature is controlled at 160℃, the outlet air temperature at 90℃, and spray drying is performed for 2h to obtain the chondroitin sulfate cross-linked polymer.

[0045] The freeze-drying protectant consists of trehalose, mannitol, and β-cyclodextrin in a mass ratio of 7:3:1.

[0046] The preservatives include white willow bark extract and anethole acid in a mass ratio of 4:1.

[0047] The active component is modified fish collagen peptide, and the modified fish collagen peptide is prepared by the following method: Fish collagen peptide powder with a molecular weight of 5000 Daltons was dissolved in deionized water to prepare a peptide solution with a mass concentration of 15%, and the pH was adjusted to 7.5. 0.05% of the total mass of the peptide solution was added to transglutaminase, and the mixture was stirred at 55°C and pH 7.0 for 3 hours to obtain a modified solution. The modified solution was cooled to 35°C, and methylpyrrolidone silanolone with a molar ratio of 1:70 to collagen peptides was added. The mixture was stirred in the dark for 4 hours to obtain a modified reaction solution. The modified reaction solution was separated and purified using an ultrafiltration membrane with a molecular weight cutoff of 1000 Daltons, and the filtrate was collected. The inlet air temperature was set to 160°C and the outlet air temperature to 70°C, and the mixture was spray-dried to constant weight to obtain the modified fish collagen peptide.

[0048] A method for preparing a skin care freeze-dried powder containing collagen peptides includes the following steps: S1. Weigh out the active ingredients, synergistic repair polysaccharides, moisturizer, freeze-drying protectant, preservative and deionized water according to the weight percentages mentioned above, and set aside for later use; S2. Heat deionized water to 80°C, add synergistic repair polysaccharide, moisturizer and preservative and stir to dissolve to obtain aqueous phase; S3. Cool the aqueous phase to 30°C, add the active component and freeze-drying protectant, and stir to dissolve; S4. Adjust the pH to 6.0 and cool to -40℃ to obtain the pre-frozen material; S5. The pre-frozen material is heated to 0°C under a vacuum of 30Pa and maintained for 2 hours. Then the pre-frozen material is heated to 30°C until the water content is less than 3%, thus obtaining skin care freeze-dried powder containing collagen peptides.

[0049] To verify the overall performance of the collagen peptide-containing freeze-dried skincare powders prepared in Examples 1-3 of this application, the applicant set up Comparative Examples 1-5, as follows: Comparative Example 1 A skin care freeze-dried powder containing collagen peptides is prepared by freeze-drying a freeze-dried liquid, wherein the freeze-dried liquid comprises the following raw materials by weight percentage: 8% active ingredients, 3% synergistic repair polysaccharides, 10% moisturizer, 15% freeze-drying protectant, 2% preservative, and the balance being deionized water.

[0050] Among them, the synergistic repair polysaccharides include β-glucan, Tremella fuciformis polysaccharide and sodium hyaluronate in a mass ratio of 6:6:1.

[0051] The humectant comprises glycerin, panthenol, and chondroitin sulfate cross-linked polymer in a mass ratio of 4:2:1. The chondroitin sulfate cross-linked polymer is prepared by the following method: chondroitin sulfate and sodium alginate are dissolved in water by stirring, the pH of the solution is adjusted to 5.2, stirring is continued, and ultrasonic cross-linking is performed while stirring. The ultrasonic power is controlled at 250W, the ultrasonic frequency at 100kHz, and the cross-linking time at 25min. After the treatment is completed, the inlet air temperature is controlled at 150℃, the outlet air temperature at 80℃, and the product is spray-dried for 3h to obtain the chondroitin sulfate cross-linked polymer.

[0052] The freeze-drying protectant consists of trehalose, mannitol, and β-cyclodextrin in a mass ratio of 6:2:1.

[0053] The preservatives include white willow bark extract and anethole acid in a mass ratio of 3:1.

[0054] The active ingredient is fish collagen peptide.

[0055] A method for preparing a skin care freeze-dried powder containing collagen peptides includes the following steps: S1. Weigh out the active ingredients, synergistic repair polysaccharides, moisturizer, freeze-drying protectant, preservative and deionized water according to the weight percentages mentioned above, and set aside for later use; S2. Heat deionized water to 75°C, add synergistic repair polysaccharide, moisturizer and preservative and stir to dissolve to obtain aqueous phase; S3. Cool the aqueous phase to 25°C, add the active component and freeze-drying protectant, and stir to dissolve; S4. Adjust the pH to 5.5 and cool to -45℃ to obtain the pre-frozen material; S5. The pre-frozen material is heated to -5°C under a vacuum of 20Pa and maintained for 1.5 hours. Then the pre-frozen material is heated to 28°C until the water content is less than 3%, thus obtaining skin care freeze-dried powder containing collagen peptides.

[0056] Comparative Example 2 A skin care freeze-dried powder containing collagen peptides is prepared by freeze-drying a freeze-dried liquid, wherein the freeze-dried liquid comprises the following raw materials by weight percentage: 8% active ingredients, 3% synergistic repair polysaccharides, 10% moisturizer, 15% freeze-drying protectant, 2% preservative, and the balance being deionized water.

[0057] Among them, the synergistic repair polysaccharides include β-glucan, Tremella fuciformis polysaccharide and sodium hyaluronate in a mass ratio of 6:6:1.

[0058] The humectant comprises glycerin, panthenol, and chondroitin sulfate cross-linked polymer in a mass ratio of 4:2:1. The chondroitin sulfate cross-linked polymer is prepared by the following method: chondroitin sulfate and sodium alginate are dissolved in water by stirring, the pH of the solution is adjusted to 5.2, stirring is continued, and ultrasonic cross-linking is performed while stirring. The ultrasonic power is controlled at 250W, the ultrasonic frequency at 100kHz, and the cross-linking time at 25min. After the treatment is completed, the inlet air temperature is controlled at 150℃, the outlet air temperature at 80℃, and the product is spray-dried for 3h to obtain the chondroitin sulfate cross-linked polymer.

[0059] The freeze-drying protectant consists of trehalose, mannitol, and β-cyclodextrin in a mass ratio of 6:2:1.

[0060] The preservatives include white willow bark extract and anethole acid in a mass ratio of 3:1.

[0061] The active component is modified fish collagen peptide, and the modified fish collagen peptide is prepared by the following method: Fish collagen peptide powder with a molecular weight of 4000 Daltons was dissolved in deionized water to prepare a 10% peptide solution, and the pH was adjusted to 7.0. The peptide solution was cooled to 30°C, and methylpyrrolidone silanol ketone with a molar ratio of 1:60 to collagen peptides was added. The mixture was stirred in the dark for 3 hours to obtain a modified reaction solution. The modified reaction solution was separated and purified using an ultrafiltration membrane with a molecular weight cutoff of 1000 Daltons, and the filtrate was collected. The inlet air temperature was set to 150°C and the outlet air temperature to 65°C, and the mixture was spray-dried to constant weight to obtain the modified fish collagen peptide.

[0062] A method for preparing a skin care freeze-dried powder containing collagen peptides includes the following steps: S1. Weigh out the active ingredients, synergistic repair polysaccharides, moisturizer, freeze-drying protectant, preservative and deionized water according to the weight percentages mentioned above, and set aside for later use; S2. Heat deionized water to 75°C, add synergistic repair polysaccharide, moisturizer and preservative and stir to dissolve to obtain aqueous phase; S3. Cool the aqueous phase to 25°C, add the active component and freeze-drying protectant, and stir to dissolve; S4. Adjust the pH to 5.5 and cool to -45℃ to obtain the pre-frozen material; S5. The pre-frozen material is heated to -5°C under a vacuum of 20Pa and maintained for 1.5 hours. Then the pre-frozen material is heated to 28°C until the water content is less than 3%, thus obtaining skin care freeze-dried powder containing collagen peptides.

[0063] Comparative Example 3 A skin care freeze-dried powder containing collagen peptides is prepared by freeze-drying a freeze-dried liquid, wherein the freeze-dried liquid comprises the following raw materials by weight percentage: 8% active ingredients, 3% synergistic repair polysaccharides, 10% moisturizer, 15% freeze-drying protectant, 2% preservative, and the balance being deionized water.

[0064] Among them, the synergistic repair polysaccharides include β-glucan, Tremella fuciformis polysaccharide and sodium hyaluronate in a mass ratio of 6:6:1.

[0065] The humectant comprises glycerin, panthenol, and chondroitin sulfate cross-linked polymer in a mass ratio of 4:2:1. The chondroitin sulfate cross-linked polymer is prepared by the following method: chondroitin sulfate and sodium alginate are dissolved in water by stirring, the pH of the solution is adjusted to 5.2, stirring is continued, and ultrasonic cross-linking is performed while stirring. The ultrasonic power is controlled at 250W, the ultrasonic frequency at 100kHz, and the cross-linking time at 25min. After the treatment is completed, the inlet air temperature is controlled at 150℃, the outlet air temperature at 80℃, and the product is spray-dried for 3h to obtain the chondroitin sulfate cross-linked polymer.

[0066] The freeze-drying protectant consists of trehalose, mannitol, and β-cyclodextrin in a mass ratio of 6:2:1.

[0067] The preservatives include white willow bark extract and anethole acid in a mass ratio of 3:1.

[0068] The active component is modified fish collagen peptide, and the modified fish collagen peptide is prepared by the following method: Fish collagen peptide powder with a molecular weight of 4000 Daltons was dissolved in deionized water to prepare a peptide solution with a mass concentration of 10%, and the pH was adjusted to 7.0. 0.04% of the total mass of the peptide solution was added to transglutaminase, and the mixture was stirred at 50°C and pH 6.8 for 2 hours to obtain a modified solution. The modified solution was separated and purified using an ultrafiltration membrane with a molecular weight cutoff of 1000 Daltons, and the filtrate was collected. The inlet air temperature was set to 150°C and the outlet air temperature to 65°C, and the mixture was spray-dried to constant weight to obtain the modified fish collagen peptide.

[0069] A method for preparing a skin care freeze-dried powder containing collagen peptides includes the following steps: S1. Weigh out the active ingredients, synergistic repair polysaccharides, moisturizer, freeze-drying protectant, preservative and deionized water according to the weight percentages mentioned above, and set aside for later use; S2. Heat deionized water to 75°C, add synergistic repair polysaccharide, moisturizer and preservative and stir to dissolve to obtain aqueous phase; S3. Cool the aqueous phase to 25°C, add the active component and freeze-drying protectant, and stir to dissolve; S4. Adjust the pH to 5.5 and cool to -45℃ to obtain the pre-frozen material; S5. The pre-frozen material is heated to -5°C under a vacuum of 20Pa and maintained for 1.5 hours. Then the pre-frozen material is heated to 28°C until the water content is less than 3%, thus obtaining skin care freeze-dried powder containing collagen peptides.

[0070] Comparative Example 4 A skin care freeze-dried powder containing collagen peptides is prepared by freeze-drying a freeze-dried liquid, wherein the freeze-dried liquid comprises the following raw materials by weight percentage: 8% active ingredients, 3% synergistic repair polysaccharides, 10% moisturizer, 15% freeze-drying protectant, 2% preservative, and the balance being deionized water.

[0071] Among them, the synergistic repair polysaccharides include β-glucan and Tremella fuciformis polysaccharides in a mass ratio of 6:7.

[0072] The humectant comprises glycerin, panthenol, and chondroitin sulfate cross-linked polymer in a mass ratio of 4:2:1. The chondroitin sulfate cross-linked polymer is prepared by the following method: chondroitin sulfate and sodium alginate are dissolved in water by stirring, the pH of the solution is adjusted to 5.2, stirring is continued, and ultrasonic cross-linking is performed while stirring. The ultrasonic power is controlled at 250W, the ultrasonic frequency at 100kHz, and the cross-linking time at 25min. After the treatment is completed, the inlet air temperature is controlled at 150℃, the outlet air temperature at 80℃, and the product is spray-dried for 3h to obtain the chondroitin sulfate cross-linked polymer.

[0073] The freeze-drying protectant consists of trehalose, mannitol, and β-cyclodextrin in a mass ratio of 6:2:1.

[0074] The preservatives include white willow bark extract and anethole acid in a mass ratio of 3:1.

[0075] The active component is modified fish collagen peptide, and the modified fish collagen peptide is prepared by the following method: Fish collagen peptide powder with a molecular weight of 4000 Daltons was dissolved in deionized water to prepare a 10% peptide solution, and the pH was adjusted to 7.0. 0.04% of transglutaminase was added to the total peptide solution, and the mixture was stirred at 50℃ and pH 6.8 for 2 hours to obtain a modified solution. The modified solution was cooled to 30℃, and methylpyrrolidone silanolone with a molar ratio of 1:60 to the collagen peptides was added. The mixture was stirred in the dark for 3 hours to obtain a modified reaction solution. The modified reaction solution was separated and purified using an ultrafiltration membrane with a molecular weight cutoff of 1000 Daltons, and the filtrate was collected. The inlet air temperature was set to 150℃ and the outlet air temperature to 65℃, and the mixture was spray-dried to constant weight to obtain the modified fish collagen peptide.

[0076] A method for preparing a skin care freeze-dried powder containing collagen peptides includes the following steps: S1. Weigh out the active ingredients, synergistic repair polysaccharides, moisturizer, freeze-drying protectant, preservative and deionized water according to the weight percentages mentioned above, and set aside for later use; S2. Heat deionized water to 75°C, add synergistic repair polysaccharide, moisturizer and preservative and stir to dissolve to obtain aqueous phase; S3. Cool the aqueous phase to 25°C, add the active component and freeze-drying protectant, and stir to dissolve; S4. Adjust the pH to 5.5 and cool to -45℃ to obtain the pre-frozen material; S5. The pre-frozen material is heated to -5°C under a vacuum of 20Pa and maintained for 1.5 hours. Then the pre-frozen material is heated to 28°C until the water content is less than 3%, thus obtaining skin care freeze-dried powder containing collagen peptides.

[0077] Comparative Example 5 A skin care freeze-dried powder containing collagen peptides is prepared by freeze-drying a freeze-dried liquid, wherein the freeze-dried liquid comprises the following raw materials by weight percentage: 8% active ingredients, 3% synergistic repair polysaccharides, 10% moisturizer, 15% freeze-drying protectant, 2% preservative, and the balance being deionized water.

[0078] The synergistic repair polysaccharide consists of β-glucan and sodium hyaluronate in a mass ratio of 6:7.

[0079] The humectant comprises glycerin, panthenol, and chondroitin sulfate cross-linked polymer in a mass ratio of 4:2:1. The chondroitin sulfate cross-linked polymer is prepared by the following method: chondroitin sulfate and sodium alginate are dissolved in water by stirring, the pH of the solution is adjusted to 5.2, stirring is continued, and ultrasonic cross-linking is performed while stirring. The ultrasonic power is controlled at 250W, the ultrasonic frequency at 100kHz, and the cross-linking time at 25min. After the treatment is completed, the inlet air temperature is controlled at 150℃, the outlet air temperature at 80℃, and the product is spray-dried for 3h to obtain the chondroitin sulfate cross-linked polymer.

[0080] The freeze-drying protectant consists of trehalose, mannitol, and β-cyclodextrin in a mass ratio of 6:2:1.

[0081] The preservatives include white willow bark extract and anethole acid in a mass ratio of 3:1.

[0082] The active component is modified fish collagen peptide, and the modified fish collagen peptide is prepared by the following method: Fish collagen peptide powder with a molecular weight of 4000 Daltons was dissolved in deionized water to prepare a 10% peptide solution, and the pH was adjusted to 7.0. 0.04% of transglutaminase was added to the total peptide solution, and the mixture was stirred at 50℃ and pH 6.8 for 2 hours to obtain a modified solution. The modified solution was cooled to 30℃, and methylpyrrolidone silanolone with a molar ratio of 1:60 to the collagen peptides was added. The mixture was stirred in the dark for 3 hours to obtain a modified reaction solution. The modified reaction solution was separated and purified using an ultrafiltration membrane with a molecular weight cutoff of 1000 Daltons, and the filtrate was collected. The inlet air temperature was set to 150℃ and the outlet air temperature to 65℃, and the mixture was spray-dried to constant weight to obtain the modified fish collagen peptide.

[0083] A method for preparing a skin care freeze-dried powder containing collagen peptides includes the following steps: S1. Weigh out the active ingredients, synergistic repair polysaccharides, moisturizer, freeze-drying protectant, preservative and deionized water according to the weight percentages mentioned above, and set aside for later use; S2. Heat deionized water to 75°C, add synergistic repair polysaccharide, moisturizer and preservative and stir to dissolve to obtain aqueous phase; S3. Cool the aqueous phase to 25°C, add the active component and freeze-drying protectant, and stir to dissolve; S4. Adjust the pH to 5.5 and cool to -45℃ to obtain the pre-frozen material; S5. The pre-frozen material is heated to -5°C under a vacuum of 20Pa and maintained for 1.5 hours. Then the pre-frozen material is heated to 28°C until the water content is less than 3%, thus obtaining skin care freeze-dried powder containing collagen peptides.

[0084] Comparative Example 6 A skin care freeze-dried powder containing collagen peptides is prepared by freeze-drying a freeze-dried liquid, wherein the freeze-dried liquid comprises the following raw materials by weight percentage: 8% active ingredients, 3% synergistic repair polysaccharides, 10% moisturizer, 15% freeze-drying protectant, 2% preservative, and the balance being deionized water.

[0085] Among them, the synergistic repair polysaccharides include β-glucan, Tremella fuciformis polysaccharide and sodium hyaluronate in a mass ratio of 6:6:1.

[0086] The moisturizers include glycerin, panthenol, and chondroitin sulfate in a mass ratio of 4:2:1.

[0087] The freeze-drying protectant consists of trehalose, mannitol, and β-cyclodextrin in a mass ratio of 6:2:1.

[0088] The preservatives include white willow bark extract and anethole acid in a mass ratio of 3:1.

[0089] The active component is modified fish collagen peptide, and the modified fish collagen peptide is prepared by the following method: Fish collagen peptide powder with a molecular weight of 4000 Daltons was dissolved in deionized water to prepare a 10% peptide solution, and the pH was adjusted to 7.0. 0.04% of transglutaminase was added to the total peptide solution, and the mixture was stirred at 50℃ and pH 6.8 for 2 hours to obtain a modified solution. The modified solution was cooled to 30℃, and methylpyrrolidone silanolone with a molar ratio of 1:60 to the collagen peptides was added. The mixture was stirred in the dark for 3 hours to obtain a modified reaction solution. The modified reaction solution was separated and purified using an ultrafiltration membrane with a molecular weight cutoff of 1000 Daltons, and the filtrate was collected. The inlet air temperature was set to 150℃ and the outlet air temperature to 65℃, and the mixture was spray-dried to constant weight to obtain the modified fish collagen peptide.

[0090] A method for preparing a skin care freeze-dried powder containing collagen peptides includes the following steps: S1. Weigh out the active ingredients, synergistic repair polysaccharides, moisturizer, freeze-drying protectant, preservative and deionized water according to the weight percentages mentioned above, and set aside for later use; S2. Heat deionized water to 75°C, add synergistic repair polysaccharide, moisturizer and preservative and stir to dissolve to obtain aqueous phase; S3. Cool the aqueous phase to 25°C, add the active component and freeze-drying protectant, and stir to dissolve; S4. Adjust the pH to 5.5 and cool to -45℃ to obtain the pre-frozen material; S5. The pre-frozen material is heated to -5°C under a vacuum of 20Pa and maintained for 1.5 hours. Then the pre-frozen material is heated to 28°C until the water content is less than 3%, thus obtaining skin care freeze-dried powder containing collagen peptides.

[0091] Performance testing To verify the superior effects of the collagen peptide-containing freeze-dried skincare powder described in this application, a series of performance tests were conducted on the products prepared in Examples 1-3 and Comparative Examples 1-6. The tests included: product physical properties; in vitro moisturizing performance; in vitro cellular efficacy; and human sensory evaluation.

[0092] 1. Test methods and conditions Sample preparation: All examples and comparative samples were redissolved in the same volume of deionized water under the same conditions (temperature 25±1℃, relative humidity 50±5%), and tested after standing for 5 minutes.

[0093] In vitro moisturizing rate test: Referring to the "QB / T 4256-2011 Guidelines for Evaluation of Moisturizing Efficacy of Cosmetics", a skin moisture content test probe was used to measure the change in moisture content of the synthetic film coated with the sample after 2h and 4h in a constant temperature and humidity chamber (temperature 21±1℃, relative humidity 50±2%), and the moisturizing rate was calculated.

[0094] Cell proliferation activity test (repair efficacy): Human fibroblasts (HSF cells) were used, and the effect of different concentrations of sample solutions on the proliferation rate of a UVB-induced photodamage cell model was determined by the CCK-8 assay.

[0095] Human sensory evaluation: Thirty healthy female volunteers aged 25-45 were invited to participate in a single-blind test of the product without their knowledge. The volunteers used the product once a day for 28 consecutive days, and then rated it on four aspects (out of 10): moisturizing sensation, refreshing feeling, skin softness, and overall satisfaction.

[0096] 2. Test Results and Analysis (1) Product physical properties and stability Table 1. Test Results of Product Physical Properties and Stability Conclusion: The products in Examples 1-3 showed the best performance in terms of appearance, reconstitution speed, and stability. Comparative Example 1 (unmodified peptide) and Comparative Example 2 (without enzyme cross-linking) showed significantly reduced activity retention, demonstrating that the modification process greatly improved the stability of the active ingredient. Comparative Example 5 (without Tremella polysaccharide) had the longest reconstitution time and a sticky texture, confirming the important role of Tremella polysaccharide in regulating the product's texture.

[0097] (2) In vitro moisturizing properties Table 2 Results of in vitro moisturizing rate test (n=3, X±SD) Conclusion: Examples 1-3 significantly outperformed all comparative examples in both short-term (2h) and long-term (4h) moisturizing performance. Comparative Example 4 (without sodium hyaluronate) showed the most significant decrease in moisturizing performance, especially at 2h, demonstrating the strong immediate water-binding ability of sodium hyaluronate. Comparative Example 6 (ordinary chondroitin sulfate) also had a significantly lower moisturizing rate than the examples, demonstrating the advantage of cross-linked polymers in long-lasting moisturizing.

[0098] (3) In vitro cell repair efficacy Table 3 Effect of UVB damage on the proliferation rate of HSF cells (n=6, X±SD) Conclusion: Examples 1-3 exhibited the strongest cell proliferation-promoting capacity at both concentrations, indicating optimal repair potential. The repair effects of Comparative Examples 1, 2, and 3 were significantly weakened, fully demonstrating the decisive role of the two-step modification process (enzyme cross-linking + silanization modification) in enhancing the bioactivity of collagen peptides. While Comparative Examples 4 and 5 showed better results than the protein-modified missing group, they were less effective than the examples, indicating that the complete polysaccharide complex system has a synergistic promoting effect on repair.

[0099] (4) Sensory evaluation Table 4. Average scores of human sensory evaluation over 28 days (n=30, 10-point scale) Conclusion: Examples 1-3 achieved the highest scores across all four sensory indicators, resulting in the best overall experience. Comparative Example 4 (without sodium hyaluronate) had significantly lower scores in moisturizing and skin smoothness. Comparative Example 5 (without tremella polysaccharide) showed a sharp drop in refreshing score, confirming its key role in regulating stickiness. The low overall satisfaction with Comparative Examples 1, 2, and 3 indicates that the modification process not only improved efficacy but also enhanced the final user experience.

[0100] 3. Conclusion The above performance test data fully demonstrate that the modified fish collagen peptides prepared by cross-linking with transglutaminase and modifying with methylpyrrolidone silanolone in this application are significantly superior to unmodified or partially modified collagen peptides in terms of stability, moisturizing properties, and repair activity; the specific ratio of β-glucan, tremella polysaccharide, and sodium hyaluronate plays a clear synergistic role in moisturizing, repairing, and providing excellent skin feel, and none of them can be omitted; the chondroitin sulfate cross-linked polymer prepared by a specific process has superior long-lasting moisturizing performance compared to ordinary chondroitin sulfate; the skin care freeze-dried powder prepared in the examples of this application has excellent comprehensive performance, significantly superior to various comparative products, reflecting the creativity and progress of the overall formulation and process design.

[0101] 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 skincare freeze-dried powder containing collagen peptides, characterized in that, It is prepared by freeze-drying a freeze-dried liquid, wherein the freeze-dried liquid comprises the following raw materials by weight percentage: 6-10% active component, 1-5% synergistic repair polysaccharide, 5-15% humectant, 10-20% freeze-drying protectant, 1-3% preservative, and the balance being deionized water. The active component is modified fish collagen peptide.

2. The skin-care freeze-dried powder containing collagen peptides according to claim 1, characterized in that, The synergistic repair polysaccharide comprises β-glucan, tremella polysaccharide, and sodium hyaluronate in a mass ratio of 5-7:5-7:

1.

3. The skincare freeze-dried powder containing collagen peptides according to claim 1, characterized in that, The moisturizer comprises glycerin, panthenol, and chondroitin sulfate cross-linked polymer in a mass ratio of 3-5:1-3:

1.

4. The skin-care freeze-dried powder containing collagen peptides according to claim 3, characterized in that, The chondroitin sulfate cross-linked polymer was prepared by the following method: chondroitin sulfate and sodium alginate were dissolved in water by stirring, the pH of the solution was adjusted to 4.8-5.6, stirring was continued, and ultrasonic cross-linking was performed while stirring. After the treatment was completed, the solution was spray-dried to obtain the chondroitin sulfate cross-linked polymer.

5. The skin-care freeze-dried powder containing collagen peptides according to claim 4, characterized in that, The ultrasonic crosslinking conditions include: ultrasonic power of 150-350W, ultrasonic frequency of 60-160kHz, and crosslinking time of 15-35min.

6. The skincare freeze-dried powder containing collagen peptides according to claim 1, characterized in that, The freeze-drying protectant comprises trehalose, mannitol, and β-cyclodextrin in a mass ratio of 5-7:1-3:

1.

7. The skin-care freeze-dried powder containing collagen peptides according to claim 1, characterized in that, The preservatives include white willow bark extract and anisic acid in a mass ratio of 2-4:

1.

8. The skin-care freeze-dried powder containing collagen peptides according to claim 1, characterized in that, The modified fish collagen peptide is prepared by the following method: fish collagen peptide powder is pretreated, cross-linked by enzyme to obtain a modified solution, the modified solution is cooled, a silanizing agent is added for site-specific modification, the site-specific modified product is purified and spray-dried to obtain the modified fish collagen peptide.

9. The skin-care freeze-dried powder containing collagen peptides according to claim 8, characterized in that, The specific preparation steps of the modified fish collagen peptide are as follows: Dissolve fish collagen peptide powder with a molecular weight of 2000-5000 Daltons in deionized water to prepare a peptide solution with a mass concentration of 5-15%, and adjust the pH to 6.5-7.5; add 0.03-0.05% of the total mass of the peptide solution with transglutaminase, and stir the reaction at 45-55℃ and pH 6.5-7.0 for 1-3 hours to obtain a modified solution; cool the modified solution to 25-35℃, add methylpyrrolidone silanol ketone with a molar ratio of 1:50-70 to the collagen peptide, and stir the reaction in the dark for 2-4 hours to obtain a modified reaction solution; separate and purify the modified reaction solution using an ultrafiltration membrane with a molecular weight cutoff of 1000 Daltons, and collect the filtrate; set the inlet air temperature to 140-160℃ and the outlet air temperature to 60-70℃, and spray dry to constant weight to obtain the modified fish collagen peptide.

10. A method for preparing a skin care freeze-dried powder containing collagen peptides as described in any one of claims 1-9, characterized in that, Includes the following steps: S1. Weigh out the active ingredients, synergistic repair polysaccharides, moisturizer, freeze-drying protectant, preservative and deionized water according to the weight percentages mentioned above, and set aside for later use; S2. Heat deionized water to 70-80℃, add synergistic repair polysaccharide, moisturizer and preservative and stir to dissolve to obtain aqueous phase; S3. Cool the aqueous phase to 20-30℃, add the active component and freeze-drying protectant, and stir to dissolve; S4. Adjust the pH to 5.0-6.0 and cool to -50 to -40℃ to obtain pre-frozen material; S5. Heat the pre-frozen material to -10-0℃ under a vacuum of 10-30Pa and maintain for 1-2 hours. Then heat the pre-frozen material to 25-30℃ until the water content is less than 3%, and the skin care freeze-dried powder containing collagen peptides is obtained.

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