A blue copper peptide composition and repair essence

Abstract

The application relates to the field of cosmetics, in particular to a blue copper peptide composition and a repairing essence. In the application, a blue copper peptide is coated by PEG grafted glyceride, PEG grafted plant-derived sterol and saturated fatty monoalcohol with a single chain of 16-30 carbons, and the surface of the blue copper peptide is modified by a polysaccharide composition, so that the stability, transdermal absorption performance and skin feeling of the blue copper peptide in the preparation of cosmetics are improved as a whole. Meanwhile, the above system can be used in an essence cream, and a better environment for the blue copper peptide to play a better effect is provided by the strong spreading and adhering performance of the essence cream system.

Description

Technical Field

[0001] This application relates to the field of cosmetics, and in particular to a blue copper peptide composition and a repairing essence. Background Technology

[0002] Blue copper peptides are small molecule complexes composed of three amino acids (glycine-histidine-lysine) and a copper ion. They possess repairing, anti-aging, and anti-inflammatory effects, and can also promote the synthesis of collagen and glycosaminoglycans on the skin surface, making them a novel cosmetic ingredient. Essence creams are skincare products between serums and creams; their texture is thicker than serums but lighter than creams, typically in a cream or gel-cream form. Compared to serums, they are more moisturizing, contain more oils, and have better water-locking effects. Therefore, using blue copper peptides in essence creams provides a better environment for them to remain in the skin, allowing them to fully exert their repairing and anti-aging effects while minimizing moisture loss.

[0003] While copper peptides possess good moisturizing and repairing effects, their application in cosmetics still presents certain challenges. Firstly, copper peptides are extremely sensitive to metal ion chelating agents; their copper ions are easily deactivated by EDTA, citric acid, and other chelating agents, leading to overall inactivation. Secondly, UV-catalyzed degradation is also a key issue causing structural damage and inactivation. Furthermore, the skin's absorption of copper peptides is also poor.

[0004] To improve the stability and absorption of copper peptides, a major research direction is to encapsulate them with compounds such as phospholipids to form liposomes or other forms of nanoparticles. Liposomes have a small particle size and good lipid solubility, allowing them to penetrate the stratum corneum and enter the skin. However, liposome preparation is cumbersome, and excessive phospholipids or other lipophilic encapsulation systems can lead to an overly thick cream texture, resulting in a long-lasting oily feel on the face. Furthermore, liposome preparation is difficult and tedious. Another approach is to combine copper peptides with carnitine tartaric acid to form an ionic liquid. However, carnitine tartaric acid is acidic, with a pH typically ranging from 3.5 to 4.5, limiting its overall concentration and potentially irritating the skin. It can also disrupt the stability of the emulsion, leading to a decrease in the overall structural stability of the serum. Summary of the Invention

[0005] Based on the above problems, the purpose of this application is to provide an essence cream system containing copper peptides, which can improve the stability of copper peptide components in the essence cream, improve its transdermal absorption performance, and at the same time have a good skin feel and a relatively simple preparation method.

[0006] First, this application provides a method for preparing a blue copper peptide composition, comprising the following steps: S1. Prepare an aqueous solution of blue copper peptide and an aqueous solution containing polysaccharides; S2. PEG-grafted glyceryl ester is mixed with PEG-grafted plant-derived sterols and saturated fatty monools with a single chain of not less than 16 carbons, and heated to melt to obtain an oily composite liquid. S3. Keep the temperature of the aqueous solution of blue copper peptide not higher than 40°C, slowly add the oily composite solution to the blue copper peptide, and then treat it by high-speed homogenization and / or ultrasound to obtain a homogenized solution. S4. Add the polysaccharide aqueous solution to the homogenizing solution to allow the components in the homogenizing solution to self-assemble and obtain a blue copper peptide composition suspension. S5. Freeze-dry the blue copper peptide composition suspension to obtain the blue copper peptide composition. The mass ratio of the polysaccharide to the copper peptide is 0.5 to 2. The mass of the PEG-grafted glycerol ester is 2 to 10 times the mass of the copper peptide. The mass of the plant-derived sterol is 0.1 to 1 times the mass of the copper peptide; The mass of the saturated fatty monool is 0.1 to 1 times the mass of the blue copper peptide; The polysaccharide is optionally selected from one or more of the following: hyaluronic acid and its salts, acetylated hyaluronic acid salts, β-glucan, trehalose, glycosyl trehalose, chitosan, deacetylated chitosan, carboxymethyl chitosan, hydroxypropyl deacetylated chitosan, sclerotium gum, biosaccharide gum-1, biosaccharide gum-2, biosaccharide gum-3, and biosaccharide gum-4.

[0007] In this scheme, an oily coating layer with a liposome-like structure is formed on the surface of an aqueous solution of copper peptides through the synergistic melt composite of PEG-grafted glycerols, PEG-grafted plant-derived sterols, and saturated fatty monools. The outer side of this coating structure contains PEG segments, which improve the overall fluidity of the coating membrane through the sterols and fatty alcohols. Overall, the coating layer, with PEG segments facing outwards and hydrophobic sterol and fatty alcohol segments facing inwards, physically isolates the copper peptide molecules within an aqueous core, effectively blocking direct contact with external oxygen, light, and metal ions, significantly reducing the oxidative degradation rate of the copper peptides. Building upon this, saturated fatty monools with 16–30 carbon single chains are inserted into the membrane structure formed by PEG-grafted glycerols and sterols. The hydrophobic stacking effect of their long-chain alkyl groups enhances the membrane's density and mechanical strength, thereby promoting the strength and stability of the subsequent coating structure.

[0008] Building upon the above, an aqueous polysaccharide solution is further introduced outside the oily coating layer. Through a cooling self-assembly process, the polysaccharide chains are wound around the outer layer of the PEG segments grafted with PEG glycerol esters. On one hand, the long polysaccharide chains form a hydration barrier on the outer layer of the micelles, preventing collisions and aggregation between micelles, reducing the particle size growth rate during storage, and thus improving the transdermal absorption capacity of the copper peptide. On the other hand, the polysaccharides form a stable microenvironment with a weakly acidic to neutral pH at the interface, maintaining the optimal pH range for the copper peptide and inhibiting conformational changes in the peptide chains caused by pH fluctuations.

[0009] Meanwhile, the PEG-grafted glycerides and PEG-grafted plant-derived sterols used in the above schemes possess strong hydrophilicity and molecular chain flexibility in their PEG segments. These components can form a continuous hydration layer on the skin surface, promoting hydration and swelling of the stratum corneum and reducing the tightness of intercellular connections. This hydration effect creates a favorable physicochemical environment for the transdermal penetration of copper peptides, enabling them to more easily cross the stratum corneum barrier and reach the target sites in the active epidermis and dermis. Simultaneously, the sterol core structure in the PEG-grafted plant-derived sterol molecule exhibits high structural affinity for the phospholipid bilayer in the skin cell membrane. When the composition comes into contact with the skin surface, the sterol core can insert into the lipid gaps of the stratum corneum, promoting close contact and local fusion between the encapsulation structure and the stratum corneum through an anchoring-like effect, achieving highly efficient delivery of copper peptides.

[0010] Furthermore, in terms of skin feel, the above-mentioned solution is more hydrophilic than the solution using phospholipids to prepare the coating system, providing a better moisturizing sensation. In addition to providing protection, polysaccharides in the above system also provide moisturizing and film-forming effects. The introduction of PEG segments can also reduce the unpleasant skin feel caused by the high viscosity of polysaccharides. Utilizing the hydrophilicity and spatial extension effect of PEG segments, an insulating layer is formed between polysaccharide molecules, effectively reducing the entanglement density between polysaccharide chains and providing a more refreshing skin feel.

[0011] Building upon the above, the blue copper peptide composition suspension was finally converted into a solid lyophilized powder via freeze-drying. The overall structure remained stable, and trehalose, glycosyltrehalose, and other lyophilization protectants formed an amorphous glassy matrix in the solid state, fixing the encapsulated structure within a stable network framework. The resulting blue copper peptide composition lyophilized powder exhibited better stability, higher activity retention, and provided superior moisturizing, anti-wrinkle, and repairing effects on the skin.

[0012] Preferably, in step S4, the polysaccharide aqueous solution is pre-cooled to 0-10°C when it is added.

[0013] In the above scheme, the aqueous polysaccharide solution is pre-cooled to 0-10°C and then added to the homogenizing liquid. When this low-temperature polysaccharide solution comes into contact with the higher-temperature homogenizing liquid, an instantaneous temperature gradient is formed in the interface region. This temperature gradient causes the PEG segments of the PEG-grafted glycerol ester to rapidly contract and wrap around the polysaccharide molecules, accelerating the self-assembly process and making the bond between the outer layer of polysaccharide and the oily coating layer tighter.

[0014] Preferably, the polysaccharide comprises 10-30% trehalose by mass of the polysaccharide.

[0015] Glycosyltrehalose is a derivative formed by glycosyltransferases transferring glucose groups onto trehalose molecules. It retains the core non-reducing 1,1-glycosidic bond structure of trehalose while adding additional hydroxyl sites. In the above-mentioned scheme, the introduction of glycosyltrehalose can form a denser hydrogen bond network, which helps to maintain the activity and integrity of the coating structure during freeze-drying and significantly improves the reconstitution effect. Simultaneously, glycosyltrehalose also provides better moisturizing properties, facilitating the penetration of copper peptides into the skin and significantly enhancing the skin feel.

[0016] Preferably, the polysaccharide is a combination of glycosyl trehalose and fully acetylated sodium hyaluronate.

[0017] In the above scheme, glycosyl trehalose can penetrate into the coating structure and form hydrogen bonds with the copper peptide for protection, while fully acetylated sodium hyaluronate, as a macromolecular backbone material, forms a supporting network structure during freeze-drying, preventing the collapse and fusion of the coating micelles. The significant difference in molecular weight between the two means that the skeletal voids created by the acetylated hyaluronic acid during cross-linking also contribute to the filling of glycosyl trehalose, effectively improving the reconstitution uniformity and dissolution rate of the freeze-dried system.

[0018] Building upon the above, sodium hyaluronate, after undergoing full acetylation modification, has some sodium carboxylate groups converted to acetyl groups, enhancing the molecule's hydrophobicity. This hydrophobic modification allows the fully acetylated sodium hyaluronate to better interact with the PEG segments and sterol structures of the oily coating layer, strengthening the interfacial binding force between the polysaccharide outer layer and the oily layer, reducing the risk of interlayer delamination during freeze-drying and storage. Furthermore, the stronger hydrophobicity facilitates its penetration into the lipid regions of the stratum corneum, synergistically allowing copper peptides to enter the intercellular matrix. Simultaneously, the fully acetylated hyaluronic acid also reduces apparent viscosity, giving the product a silky smooth application feel and rapid absorption. Overall, using acetylated hyaluronic acid can improve the skin feel and transdermal penetration performance of the system without compromising its stability.

[0019] Preferably, in step S2, silanetriol trehalose ether is also added, wherein the mass of silanetriol trehalose ether is 0.5 to 2 times the mass of the blue copper peptide.

[0020] The silanol trehalose molecule can form hydrogen bonds with the PEG segments of PEG-grafted glyceryl esters, while the hydrophobicity of the siloxane backbone allows it to embed into the hydrophobic regions of the oily coating layer. These effects enable the silanol trehalose molecule to act as a bridge between the hydrophilic polysaccharide outer layer and the hydrophobic oily layer, improving the stability and strength of the overall coating structure. Simultaneously, the silane segments provide better spreadability, allowing the trehalose portion to hydrate rapidly and produce an immediate feeling of hydration when the aforementioned copper peptide composition is applied in skincare and cosmetic products. Meanwhile, the siloxane forms breathable hydrophobic microdomains on the skin surface, reducing moisture evaporation and maintaining a soft, smooth feel, without the occlusive feeling of traditional silicone oils. It also provides better fluidity and spreadability during film application.

[0021] Preferably, the PEG-grafted glycerol ester is a combination of PEG-grafted triglyceride and long-chain PEG-grafted monoglyceride, wherein the mass ratio of the PEG-grafted triglyceride to the long-chain PEG-grafted monoglyceride is 1:2 to 9, wherein the PEG-grafted triglyceride is one or more selected from PEG-10 glycerol triisostearate, PEG-3 glycerol triisostearate, PEG-25 glycerol trioleate, PEG-5 glycerol triisostearate, and PEG-20 glycerol triisostearate, and wherein the chain length of the PEG in the long-chain PEG-grafted monoglyceride is 50 to 200.

[0022] PEG-grafted triglycerides, with three PEGylated branches, exhibit significant steric hindrance and strong emulsifying ability, making them suitable for forming initial coarse emulsion structures. Long-chain PEG-grafted monoglycerides, with a single long PEG chain, have a more regular interfacial arrangement, suitable for stabilizing refined nanoscale micelles. In the above scheme, the PEG-grafted triglycerides employ a short-chain structure, exhibiting stronger lipophilicity and good compatibility with sterols and fatty alcohols in oily complexes, which is beneficial for initial oil phase dispersion. Meanwhile, the long-chain PEG-grafted monoglycerides possess strong hydrophilicity, extending outwards during self-assembly to form a thick hydration layer, enhancing the steric stability of the micelles. Overall, this gradient design of combined long and short PEG chain lengths creates a smooth transition region between the hydrophobic core and hydrophilic shell of the coating structure, reducing interlayer stress, improving overall mechanical strength, and ensuring structural stability during freeze-drying and reconstitution, preventing the coating structure from breaking and providing better protection for the encapsulated copper peptides.

[0023] Preferably, in step S3, the high-speed homogenization speed is 8000–20000 rpm, and the homogenization time is 3–15 minutes; and / or, In step S3, the ultrasonic power is 50-500W, the processing time is 3-8 minutes, and a pulse mode is used with a pulse ratio of 1s on / 1s off to 5s on / 5s off; and / or, In step S3, after high-speed homogenization and / or ultrasonic treatment, the material is further filtered through a microporous membrane with a pore size of 0.2 to 2.0 μm.

[0024] Overall, the above method ensures that the aqueous solution of copper peptides is dispersed within a plating particle size range. After initial particle formation, filtration through a membrane removes uncoated free copper peptide aggregates, large micelles, and any potential impurity particles. This method results in uniformly sized, structurally intact, fine, and stable coated particles.

[0025] In addition, this application also provides a repair essence cream containing any of the above-mentioned blue copper peptide compositions, wherein the blue copper peptide composition accounts for 0.5 to 10% of the essence cream by mass.

[0026] In the above formulation, the composition accounts for 0.5% to 10% of the essence cream, which can generally meet the needs of daily repair, anti-inflammatory, and nourishing scenarios. The semi-occlusive cream texture of the essence cream has better skin retention than that of a regular essence cream, reducing the loss of active ingredients due to flow or evaporation; it also has a lighter texture than a face cream, reducing the obstruction of the oil barrier to the penetration of active ingredients.

[0027] Preferably, the repair essence cream contains the following components by weight percentage: Moisturizer 3-15%; Emollient 10-20%; Emulsifier 2-8%; Thickener 1-5%; Soothing agent 0.1-2%; Antioxidant 0.1-1%; Chelating agent 0-0.2%; Skin conditioning agent 0.5-5%; pH adjuster 0-0.5%; Blue copper peptide composition 0.5-10%; The remainder is a solvent, which contains water and glycerin.

[0028] In the above components, the humectant maintains the osmotic pressure of the aqueous phase, preventing dehydration of the outer polysaccharide layer of the composition; the emulsifier stabilizes the O / W emulsion structure and provides a dispersion carrier for the composition; and the thickener mainly functions to adjust viscosity, prevent micelle sedimentation, and improve dispersibility. Meanwhile, since the copper peptide is fully encapsulated in the system, a small amount of chelating agent will not adversely affect the copper peptide, nor will it cause precipitation or inactivation. Under short-term or low-temperature storage conditions, the addition of chelating agents such as EDTA will have virtually no adverse effects. Skin conditioning agents can be selected from stratum corneum-like lipids such as ceramides, squalane, and phytosterols. These ingredients can replenish the lipid deficiency in the skin barrier and repair the stratum corneum's structural integrity. After barrier repair, the skin's permeability resistance to active ingredients is reduced, further enhancing the absorption efficiency of the copper peptide. Simultaneously, ceramides and other ingredients synergistically promote intercellular lipid synthesis with the copper peptide in the dermis. Soothing agents can effectively reduce the slight irritation that may be caused by the copper peptide and other ingredients in the formula, improving the product's gentleness and tolerability.

[0029] Preferably, the preparation of the repair essence cream includes the following steps: S6. Mix the moisturizer, thickener, chelating agent, water, and glycerin to obtain an aqueous phase composition; mix the emollient, emulsifier, and soothing agent to obtain an oil phase composition; S7. Maintain the temperature at 50-80℃ and mix the oil phase composition and the aqueous phase composition to obtain the essence cream base; S8. Cool the essence cream base to no higher than 30°C, and while stirring, add the blue copper peptide composition, antioxidant, skin conditioning agent, and pH adjuster. Continue to mix evenly, let it stand and age, and then fill it.

[0030] In the above scheme, the aqueous phase composition and the oil phase composition are prepared separately through phase separation to ensure that each component is fully dissolved or melted at a suitable temperature. In step S7, the two phases are mixed at 50-80°C, which is higher than the melting point of most oils to ensure complete emulsification. After cooling, other components such as the blue copper peptide composition are added to the system to avoid loss of active compounds.

[0031] In summary, this application first uses PEG-grafted glyceryl esters, PEG-grafted plant-derived sterols, and saturated fatty monools with single chains of 16-30 carbons to encapsulate the copper peptides. The surface is then modified using a polysaccharide composition, which overall improves the stability, transdermal absorption performance, and skin feel of the copper peptides in cosmetic preparation. Furthermore, this system can be used in serums, where the strong spreading and adhesion properties of the serum system provide a better environment for the copper peptides to exert their effects. Detailed Implementation

[0032] The technical solutions in this application will be further described through the following specific embodiments.

[0033] In the following embodiments, the specifications for some raw materials are shown in Table 1.

[0034] Unless otherwise specified, all other ingredients are commercially available cosmetic grade or higher.

[0035] Example 1: This example first provides a blue copper peptide composition, which specifically includes the following steps: S1. Dissolve 0.5 parts by mass of blue copper peptide in 20 parts by mass of deionized water at 25°C with stirring at 200 rpm until the solution is clear and light blue. Store in the dark to obtain an aqueous solution of blue copper peptide.

[0036] Take 30 parts by weight of deionized water, add 0.4 parts by weight of fully acetylated sodium hyaluronate and 0.1 parts by weight of glycosyl trehalose to the deionized water, let stand for 30 minutes to allow it to fully hydrate and swell, then turn on the stirrer at 200 rpm and stir at 25°C for 20 minutes until completely dissolved, pre-cool to 4°C and set aside.

[0037] S2. Prepare 0.5 parts by weight of PEG-10 glyceryl triisostearate and 1.5 parts by weight of PEG-120 glyceryl stearate, and at the same time prepare 0.25 parts by weight of PEG-10-rapeseed oil sterol and 0.25 parts by weight of cetyl alcohol (hexadecyl alcohol). Mix them and heat to 70°C, stirring until a completely melted, homogeneous, and transparent solution is obtained to obtain an oily composite liquid. Keep it warm for later use.

[0038] S3. In a circulating water-cooled environment, control the temperature of the copper peptide aqueous solution to not exceed 40℃ (preferably within the range of 30-40℃). While maintaining stirring, add the oily composite solution dropwise to the copper peptide aqueous solution over a period of 20 minutes. Then, homogenize the solution using a high-speed homogenizer at 12000 rpm for 8 minutes. Next, use an ultrasonic processor for ultrasonic treatment at a power of 200W in pulse mode (3 seconds on / 2 seconds off) for 5 minutes. After ultrasonication, filter the solution through a 0.45μm microfiltration membrane and collect the filtrate to obtain the homogenized solution.

[0039] S4. The homogenizing liquid temperature is controlled at 25℃, and the stirring speed is maintained at 200 rpm. The pre-cooled polysaccharide aqueous solution at 4℃ is slowly added to the homogenizing liquid in S3. The addition time is 3 min. After the addition is completed, the stirring speed is maintained at 200 rpm for 30 min to allow the components in the homogenizing liquid to fully self-assemble and obtain the blue copper peptide composition suspension.

[0040] S5. The blue copper peptide composition suspension obtained in S4 is dispensed into freeze-drying trays and placed in a freeze dryer. The trays are cooled to -40°C at a rate of 1°C / min and held at this temperature for 4 hours to completely freeze the sample. A vacuum pump is then started to reduce the vacuum to below 10 Pa. The shelf temperature is increased to -10°C at a rate of 0.5°C / min and maintained at this temperature for 12 hours. Subsequently, the temperature is increased to 30°C at a rate of 0.5°C / min and held for another 5 hours. The sample is then plugged and removed from the freeze dryer under vacuum to obtain a loose, porous blue copper peptide composition freeze-dried cake. The freeze-dried cake is then pulverized and sieved (80 mesh) under dry, light-protected conditions to obtain the blue copper peptide composition powder.

[0041] In Examples 2 to 15, based on Example 1, the selection of polysaccharides was adjusted. While keeping the quality of the polysaccharides unchanged, the types and proportions of polysaccharides were substituted, as shown in Table 2.

[0042] Example 16 differs from Example 1 in that, in step S1, after preparing the aqueous solution containing polysaccharides, it is not pre-cooled but added to the homogenizing liquid at 25°C.

[0043] Examples 17-25 and Comparative Example 2, based on Example 1, have different ratios of PEG-grafted glycerol esters, as shown in Table 3.

[0044] Examples 26-27 and Comparative Example 3, based on Example 1, involved adjusting different fatty monools, as shown in Table 4.

[0045] Furthermore, based on Example 1, in step S2, different masses of silanetriol trehalose ether are added, as shown in Table 5.

[0046] The above embodiments will be prepared into an essence cream according to the following preparation method.

[0047] S6. Prepare materials as shown in Table 6: The aqueous phase composition and the oil phase composition were prepared respectively according to the following methods: Aqueous phase composition: Weigh out deionized water, glycerin, humectant, thickener, and chelating agent according to the formula. First, disperse the thickener with a small amount of glycerin, then add it to the remaining water. Heat to 75°C, stir until completely dissolved, and keep warm for later use.

[0048] Preparation of oil phase composition: Weigh out the emollient, emulsifier and soothing agent according to the formula, heat to 75°C, stir until completely melted and transparent, and keep warm for later use. S7. Keeping both the aqueous and oil phases at 75°C, slowly add the oil phase composition to the aqueous phase composition while stirring at 200 rpm. After addition, homogenize at 6000 rpm for 8 minutes to form a uniform and fine emulsion. After homogenization, continue stirring at 200 rpm and cool to 25°C at a rate of 0.5–1°C / min to obtain the essence cream base.

[0049] S8. While stirring at 200 rpm, add the blue copper peptide composition, antioxidant, skin conditioning agent, and pH adjuster prepared in the examples and comparative examples to the essence cream base in sequence. Stir for 3 minutes after each component is added until homogeneous, and then add the next component. After all components have been added, continue stirring for 20 minutes, then let it stand for 12 hours to age, and then fill into bottles to obtain the essence cream.

[0050] Corresponding to Examples 1 to 32, the prepared essence creams are sequentially labeled as Application Examples 1 to 32. Compared with Comparative Examples 1 to 3, the prepared essence creams are sequentially labeled as Comparative Application Examples 1 to 3.

[0051] The following experiments were conducted on the above embodiments, comparative examples, application examples, and comparative application examples: 1. The encapsulation efficiency of the lyophilized powders obtained in the examples and comparative examples was determined. The encapsulation efficiency was determined by the following method: the lyophilized powders were reconstituted in deionized water, placed in an ultrafiltration centrifuge tube, centrifuged at 4000 rpm for 30 min, the filtrate was collected, and then the cell wall was broken up (methanol:water = 1:1 was added, and the mixture was sonicated for 30 min). After centrifugation again, the total blue copper peptides were collected, and the encapsulation efficiency of the blue copper peptides was determined by HPLC.

[0052] 2. Take 1g of the lyophilized powder obtained in the examples and comparative examples, add 10mL of deionized water (25℃), shake gently, and record the time for complete reconstitution.

[0053] 3. Transdermal experiments were conducted on samples from some application examples and comparative examples using the vertical Franz diffusion cell method. Pig back skin, with a skin area controlled at 1.0 cm², was fixed between the supply and receiving chambers of the Franz diffusion cell, with the stratum corneum facing upwards towards the supply chamber. The receiving chamber was filled with PBS receiving solution (pH 7.4) to ensure sufficient contact between the dermis and the receiving solution. The assembled diffusion cell was placed in a constant temperature water bath at 37℃±0.5℃ for equilibration for 30 minutes. 0.5 g of the sample from the application examples and comparative examples was weighed and evenly applied to the skin surface on the supply chamber side. Subsequently, 1.0 mL samples were taken from the receiving chamber at 24 hours to determine the proportion of the cumulative transdermal amount to the total copper peptides over 24 hours. Simultaneously, after the experiment, the skin samples were removed, and any remaining sample was washed off with physiological saline. After homogenizing the skin, the skin retention rate (the proportion of copper peptides retained by the skin to the total copper peptides) was determined.

[0054] 4. Skin feel test: For samples in some application examples and comparison examples, 30 volunteers (aged 25-50, 10 each of dry, normal, and oily skin types) were recruited, and then evaluated according to the following criteria: Spreadability: 10 points = very easy to spread, 1 point = difficult to spread; Stickiness: 10 points = not sticky at all, 1 point = extremely sticky; Post-use hydration: 10 points = very hydrating, 1 point = dry and tight.

[0055] First, the results of Experiment 1 and Experiment 2 for the Examples and Comparative Examples are shown in Table 7.

[0056] In the table above, " / " indicates that no measurement was performed, which usually means that the encapsulation efficiency is too low and no measurement is required.

[0057] In the above experimental results, compared with Example 1, Comparative Example 1, which did not add polysaccharide, showed a significantly lower encapsulation efficiency. This indicates that without a polysaccharide protective layer, ice crystals directly damage the coating structure during freeze-drying, leading to the leakage of a large amount of copper peptides. This confirms the necessity of the polysaccharide outer layer for freeze-drying protection. In Examples 1-15, the composition of the polysaccharide was adjusted. Through Examples 1-16, it can be seen that the encapsulation efficiency increases with the degree of acetylation of hyaluronic acid. The anchoring effect between the hydrophobic acetyl segments and the hydrophobic core of the coating is evident: the higher the degree of acetylation, the more anchoring points, the stronger the bond between the polysaccharide layer and the coating, and the better the protective effect during freeze-drying. Comparing the polysaccharides, it can be seen that glycosyltrehalose showed better performance than trehalose in all experimental groups. The additional glycosyl branches of glycosyltrehalose provide more hydrogen bond sites, forming a denser hydrogen bond network with copper peptides during freeze-drying, significantly enhancing the protective effect. In Examples 7-9, using only sodium hyaluronate, the lack of dispersion and protection effects from glycosyl trehalose resulted in a significant decrease in both coating and resolubility. In Examples 10-12, the effect of the ratio of fully acetylated hyaluronic acid (HA) to trehalose was investigated. It was observed that when the ratio of HA was too low, the polysaccharide shell was incomplete. Examples 13-15 used alternative polysaccharides. The encapsulation rates of both biosaccharide gum-1 and hydroxypropyl deacetylated chitosan were lower than in Example 1. The positively charged chitosan may have caused electrostatic interference with the PEG chains, further reducing the encapsulation rate. Simultaneously, biosaccharide gum-1 also had a negative impact on the resolubility of the system. In Example 16, glycosyl trehalose was added at room temperature, lacking a low-temperature assembly step. It was observed that glycosyl trehalose could not modify the coating system, making it more prone to breakage during freeze-drying, leading to a decrease in encapsulation effectiveness.

[0058] In Comparative Example 2 and Examples 17-24, the effect of the PEG-grafted glycerol ester ratio was further investigated. Comparative Example 2 showed the lowest encapsulation efficiency; the coating formed by the non-PEGylated glycerol ester could not be stably dispersed in the aqueous phase and could not encapsulate the peptide. In other examples, long PEG chains imparted stronger hydrophilicity and hydration capacity to the coating surface, making it easier for water molecules to penetrate during resolution. In Example 22, short-chain glycerol stearate resulted in insufficient hydration layer and easy aggregation of the coating, leading to a certain reduction in both resolution and encapsulation effects. In Example 25, excessively long triglyceride PEG chains resulted in an overly large hydrophilic head group and a relatively short hydrophobic tail chain, reducing encapsulation capacity. In Example 18, the lack of triglyceride also led to a significant reduction in encapsulation effect. In Example 20, excessive amounts of glycerol triisostearate had a significant adverse effect on the strength of the encapsulation structure, also leading to a decrease in the mechanical strength of the system and a significant reduction in the encapsulation effect after resolution.

[0059] In Examples 26-27 and Comparative Example 3, the fatty monools were adjusted. In Example 27, lauryl alcohol was selected. Lauryl alcohol has weak hydrophobic interactions and cannot stably embed into the membrane structure, thus offering limited improvement to membrane strength. This makes the coating structure more prone to damage during homogenization and freeze-drying, leading to a decrease in coating efficiency. In Examples 28-32, the amount of silanetriol trehalose ether was adjusted. Overall, as the mass of silanetriol trehalose ether increased, the encapsulation efficiency increased with the amount of silanetriol trehalose ether added, showing a trend of first increasing and then decreasing, while the reconstitution rate decreased with increasing addition. This indicates that silanetriol trehalose ether has an interfacial synergistic effect. The silanol groups in it form hydrogen bonds with the ether oxygen atoms of the PEG chain, embedding themselves in the oil-water interfacial film as molecular bridges, making the interfacial film more compact and ordered. It also helps water molecules penetrate during resolution, thus achieving a better dispersion effect on the coated system. However, if its addition amount is too large, it will crowd out the ordered arrangement space of PEG grafted glycerol esters, destroy the interfacial film structure, and also lead to a decrease in overall hydrophobicity, thereby damaging the coated structure.

[0060] Experiment 4 was conducted on some of the above application examples, and the results are shown in Table 8.

[0061] As can be seen from the above application examples, overall, the higher the degree of acetylation and the presence of glycosyl trehalose, the significantly improved spreading performance, without causing a noticeable stickiness or a significant decrease in smoothness due to excessive hydrophobicity. Chitosans, due to their strong film-forming properties but insufficient lubrication, have significantly lower stickiness scores. Comparing application examples 20 and 21, it can be seen that the spreading performance is best when the ratio of triglycerides to monoglycerides is 1:3; PEG-120 has a slightly better silky feel and spreading performance than PEG-100. In examples 28-32, it can be seen that the spreading performance of the film is significantly enhanced after adding silanetriol trehalose ether. This is because the silanol hydroxyl groups of silanetriol trehalose ether form hydrogen bonds with the PEG chains and embed into the interfacial film, making the film structure more compact and ordered. At the same time, due to the good hydrophilicity of silanetriol trehalose ether, the overall moisturizing feel is also enhanced to a certain extent. However, excessive addition will produce a certain stickiness.

[0062] Furthermore, Experiment 3 was conducted on some application examples, and the results are shown in Table 9.

[0063] The above experiments show that, compared to Application Examples 1, 3, and 5, the substitution of acetyl groups significantly affects the transdermal performance of copper peptides. Higher acetylation results in greater overall hydrophobicity, leading to better affinity of the encapsulation structure for the stratum corneum within the overall hydrophilic essence cream system, thus enhancing transdermal performance. In Application Example 14, a chitosan system was used. Because chitosan carries a positive charge, it may interact electrostatically with the ether oxygen atoms of the PEG chain, interfering with the ordered hydration layer structure on the surface of the encapsulation, thus reducing skin permeability. In Application Example 20, the excessively high triglyceride content significantly increased the rigidity of the membrane structure, resulting in no significant reduction in skin retention rate, but making it more difficult to penetrate the stratum corneum to the back of the skin, thus reducing the transdermal effect. In Application Example 30, the addition of silanetriol trehalose ether may have a slight effect on increasing transdermal absorption, but this effect is not significant.

[0064] For example 30, further human skin experiments were conducted. The experiment was conducted in accordance with four standards: T / CAB-0152-2022 Test Method for Seven Efficacy of Cosmetics (Anti-wrinkle, Firming, Moisturizing, Oil Control, Repairing, Nourishing and Soothing), T / GDCA 009-2022 Human Evaluation Method for Repairing Efficacy of Cosmetics, T / GDCDC 021-2022 Test Method for Soothing Efficacy of Cosmetics, and T / TDCA 003-2021 Test Method for Firming Efficacy of Cosmetics. The study was also conducted with reference to "Research on Evaluation Method of Firming Efficacy of Cosmetics Based on Image Analysis" (Yang Zeru, Wei Yuexian, Fan Zhanhua, Liu Qi, Wang Min, Zhao Hua. Daily Chemical Industry, 2020, 50(12):854-860). The subjects were 8 males and 25 females aged 18-54 years, with an average age of 35.45 years. The treatment lasted for 14 days. The method of use was as follows: After cleansing, apply an appropriate amount of this product to the face and neck and wipe until fully absorbed. Used twice a day.

[0065] Facial testing was performed sequentially after sample use, and at 3, 7, and 14 days later. After 14 days, no adverse reactions such as erythema, edema, papules, or blisters were observed in any of the subjects.

[0066] The overall experimental results are shown in Table 10.

[0067] The above experimental results show that the essence cream in application example 30 can effectively produce repair and anti-wrinkle effects.

[0068] 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 method for preparing a blue copper peptide composition, characterized in that, Includes the following steps S1. Prepare an aqueous solution of blue copper peptide and an aqueous solution containing polysaccharides; S2. PEG-grafted glyceryl ester is mixed with PEG-grafted plant-derived sterols and saturated fatty monools with a single chain of not less than 16 carbons, and heated to melt to obtain an oily composite liquid. S3. Keep the temperature of the aqueous solution of blue copper peptide not higher than 40°C, slowly add the oily composite solution to the blue copper peptide, and then treat it by high-speed homogenization and / or ultrasound to obtain a homogenized solution. S4. Add the polysaccharide aqueous solution to the homogenizing solution to allow the components in the homogenizing solution to self-assemble and obtain a blue copper peptide composition suspension. S5. Freeze-dry the blue copper peptide composition suspension to obtain the blue copper peptide composition. The mass ratio of the polysaccharide to the copper peptide is 0.5 to 2. The mass of the PEG-grafted glycerol ester is 2 to 10 times the mass of the copper peptide. The mass of the plant-derived sterol is 0.1 to 1 times the mass of the copper peptide; The mass of the saturated fatty monool is 0.1 to 1 times the mass of the blue copper peptide; The polysaccharide is optionally selected from one or more of the following: hyaluronic acid and its salts, acetylated hyaluronic acid salts, β-glucan, trehalose, glycosyl trehalose, chitosan, deacetylated chitosan, carboxymethyl chitosan, hydroxypropyl deacetylated chitosan, sclerotium gum, biosaccharide gum-1, biosaccharide gum-2, biosaccharide gum-3, and biosaccharide gum-4.

2. The method for preparing a blue copper peptide composition according to claim 1, characterized in that, In step S4, the polysaccharide aqueous solution is pre-cooled to 0-10°C when it is added.

3. The method for preparing a blue copper peptide composition according to claim 1, characterized in that, The polysaccharide contains 10-30% trehalose by mass.

4. The method for preparing a blue copper peptide composition according to claim 3, characterized in that, The polysaccharide is a combination of glycosyl trehalose and fully acetylated sodium hyaluronate.

5. The method for preparing a blue copper peptide composition according to claim 1, characterized in that, In step S2, silanetriol trehalose ether is also added, wherein the mass of silanetriol trehalose ether is 0.5 to 2 times the mass of the blue copper peptide.

6. The method for preparing a blue copper peptide composition according to claim 1, characterized in that, The PEG-grafted glycerol ester is a combination of PEG-grafted triglyceride and long-chain PEG-grafted monoglyceride, wherein the mass ratio of PEG-grafted triglyceride to long-chain PEG-grafted monoglyceride is 1:2 to 9, wherein the PEG-grafted triglyceride is one or more of PEG-10 glycerol triisostearate, PEG-3 glycerol triisostearate, PEG-25 glycerol trioleate, PEG-5 glycerol triisostearate, and PEG-20 glycerol triisostearate, and wherein the chain length of PEG in the long-chain PEG-grafted monoglyceride is 50 to 200.

7. The method for preparing a blue copper peptide composition according to claim 1, characterized in that, In step S3, the high-speed homogenization speed is 8000–20000 rpm, and the homogenization time is 3–15 minutes; and / or, In step S3, the ultrasonic power is 50-500W, the processing time is 3-8 minutes, and a pulse mode is used with a pulse ratio of 1s on / 1s off to 5s on / 5s off; and / or, In step S3, after high-speed homogenization and / or ultrasonic treatment, the material is further filtered through a microporous membrane with a pore size of 0.2 to 2.0 μm.

8. A repairing essence cream, characterized in that, The composition comprises the blue copper peptide composition according to any one of claims 1 to 7, wherein the blue copper peptide composition comprises 0.5 to 10% by mass in the essence cream.

9. The repair essence cream according to claim 8, characterized in that, The repairing essence cream contains the following ingredients by weight percentage: Moisturizer 3-15%; Emollient 10-20%; Emulsifier 2-8%; Thickener 1-5%; Soothing agent 0.1-2%; Antioxidant 0.1-1%; Chelating agent 0-0.2%; Skin conditioning agent 0.5-5%; pH adjuster 0-0.5%; Blue copper peptide composition 0.5-10%; The remainder is a solvent, which contains water and glycerin.

10. The repair essence cream according to claim 8, characterized in that, The preparation of the repair essence cream includes the following steps: S6. Mix the moisturizer, thickener, chelating agent, water, and glycerin to obtain an aqueous phase composition; mix the emollient, emulsifier, and soothing agent to obtain an oil phase composition; S7. Maintain the temperature at 50-80℃ and mix the oil phase composition and the aqueous phase composition to obtain the essence cream base; S8. Cool the essence cream base to no higher than 30°C, and while stirring, add the blue copper peptide composition, antioxidant, skin conditioning agent, and pH adjuster. Continue to mix evenly, let it stand and age, and then fill it.

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