Biomimetic moisturizing compositions containing hyaluronic acid of gradient molecular weight and methods of making the same
By leveraging the synergistic effect of gradient molecular weight hyaluronic acid and biomimetic lipid carriers, small and uniformly distributed liposomes were prepared and embedded in the hyaluronic acid network structure. This solved the problems of single layer and insufficient durability of traditional hyaluronic acid moisturizing compositions, achieving three-dimensional long-lasting moisturizing and skin barrier repair.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- LUOJIA (SHENZHEN) BIOTECHNOLOGY CO LTD
- Filing Date
- 2026-04-07
- Publication Date
- 2026-07-14
AI Technical Summary
Traditional hyaluronic acid moisturizing compositions, due to their single molecular weight and lack of biomimetic lipid carriers, cannot act on different layers of the skin simultaneously, resulting in limited moisturizing effect, insufficient duration of moisturization, low penetration efficiency of active ingredients, and inability to effectively repair the skin barrier.
A gradient molecular weight hyaluronic acid complex was synergistically compounded with a biomimetic lipid carrier. Through a specific process, biomimetic liposomes with small particle size and uniform distribution were prepared and embedded in the three-dimensional network structure of hyaluronic acid to form an interpenetrating network that simulates the skin barrier structure. Combined with polyol moisturizers and emulsifiers, the pH value was adjusted to a slightly acidic state.
It achieves three-dimensional long-lasting moisturizing from surface water locking to deep water storage, significantly improving the moisturizing effect and the penetration ability of active ingredients, while enhancing the skin barrier repair function.
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Figure CN122376479A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to a biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid and its preparation method, belonging to the field of cosmetic technology. Background Technology
[0002] This biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid combines four different molecular weight hyaluronic acid compounds (oligomeric, low, medium, and high) in specific proportions to form a gradient molecular weight hyaluronic acid complex. This complex is then synergistically combined with a biomimetic lipid carrier composed of ceramides, cholesterol, and hydrogenated lecithin. With the combined action of polyol moisturizers, emulsifiers, and other excipients, a composition that mimics the skin's natural moisturizing structure is formed. The gradient molecular weight hyaluronic acid delivers moisture at different skin layers, providing long-lasting hydration. Simultaneously, the biomimetic lipid carrier repairs the skin barrier and enhances the penetration of active ingredients. This overcomes the limitations of traditional single-molecular-weight hyaluronic acid moisturizing products, which have limited effectiveness and durability, providing a comprehensive, biomimetic moisturizing solution for the skin, from surface hydration to deep hydration.
[0003] Traditional moisturizing compositions containing hyaluronic acid are usually prepared by simply combining a single molecular weight or a simple mixture of hyaluronic acid with a common emulsion system. This method makes it difficult for a single molecular weight to act on different layers of the skin at the same time, resulting in limited moisturizing effect and insufficient lasting effect. It also lacks a biomimetic lipid carrier, which makes it unable to effectively repair the skin barrier. As a result, the penetration efficiency of active ingredients is low, and it is difficult to achieve both overall moisturizing effect and skin feel. Summary of the Invention
[0004] This invention provides a biomimetic moisturizing composition containing hyaluronic acid with gradient molecular weight and its preparation method. Its main purpose is to achieve deep penetration and three-dimensional long-lasting moisturizing that mimics the skin barrier.
[0005] To achieve the above objectives, the present invention provides a biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid, characterized in that it comprises the following components in parts by mass: 0.1-5 parts of gradient molecular weight hyaluronic acid complex, 1-5 parts of biomimetic lipid carrier, 5-15 parts of polyol moisturizer, 1-3 parts of emulsifier, 0.01-0.5 parts of pH adjuster, and deionized water to make up to 100 parts. The gradient molecular weight hyaluronic acid complex is composed of oligomeric hyaluronic acid, low molecular weight hyaluronic acid, medium molecular weight hyaluronic acid and high molecular weight hyaluronic acid in a mass ratio of (0.5-1):(1-2):(1-2):(0.05-0.1); The biomimetic lipid carrier is composed of ceramide, cholesterol and hydrogenated lecithin in a mass ratio of (1-3):(1-2):(3-5).
[0006] Optionally, the biomimetic lipid carrier is 2-4 parts by mass, and the mass ratio of ceramide to hydrogenated lecithin is (1.5-2.5):(3.5-4.5).
[0007] Optionally, in the biomimetic lipid carrier, the ceramide is at least one of ceramide NP, ceramide AP, and ceramide EOP, the cholesterol is plant-derived cholesterol, and the hydrogenation degree of the hydrogenated lecithin is ≥90%.
[0008] Optionally, the polyol moisturizer is a compound of glycerin and butylene glycol, wherein the mass ratio of glycerin to butylene glycol is (2-4):(1-2).
[0009] Optionally, the mass fraction of the gradient molecular weight hyaluronic acid complex is 1-3 parts; the mass ratio of the oligomeric hyaluronic acid to the high molecular weight hyaluronic acid is (0.6-0.9):(0.06-0.09).
[0010] Optionally, in the gradient molecular weight hyaluronic acid complex, the oligomeric hyaluronic acid has a molecular weight ≤10kDa, the low molecular weight hyaluronic acid has a molecular weight of 10-100kDa, the medium molecular weight hyaluronic acid has a molecular weight of 100-500kDa, and the high molecular weight hyaluronic acid has a molecular weight of 1000-1500kDa.
[0011] Optionally, a method for preparing a biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid, the method comprising: S1. Ceramide, cholesterol and hydrogenated lecithin are dissolved in anhydrous ethanol according to the mass ratio in the biomimetic lipid carrier, injected into phosphate buffer at a temperature of 55-60℃, ethanol is removed by vacuum evaporation, and the mixture is homogenized under high pressure to obtain a biomimetic liposome suspension. S2. Mix the polyol moisturizer with a portion of deionized water and heat to 45-50℃. While stirring, add oligomeric hyaluronic acid, low molecular weight hyaluronic acid, and medium molecular weight hyaluronic acid in the order of increasing molecular weight of each component in the gradient molecular weight hyaluronic acid complex. After stirring and dissolving, add high molecular weight hyaluronic acid last. The addition ratio of oligomeric hyaluronic acid, low molecular weight hyaluronic acid, medium molecular weight hyaluronic acid, and high molecular weight hyaluronic acid is based on the mass ratio in the gradient molecular weight hyaluronic acid complex. Continue stirring and heat to 60-65℃, and keep warm to swell for 2-4 hours to obtain a gradient hyaluronic acid gel matrix. S3. Mix the biomimetic liposome suspension, emulsifier, and remaining deionized water obtained in step S1, preheat to 70-75°C, stir evenly, and then cool to 40-45°C. Then add it to the gradient hyaluronic acid gel matrix obtained in step S2, and perform dispersion and emulsification treatment at a homogenization speed of 3000-5000 rpm for 15-20 minutes. Cool to 35-40°C, add pH adjuster to adjust the pH value of the system to 5.5-6.5, filter and discharge to obtain the biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid.
[0012] Optionally, the homogenization process employs a two-stage homogenization process, wherein the first-stage homogenization pressure is 800-1000 bar, the second-stage homogenization pressure is 200-400 bar, the homogenization cycle number is 3-5 times, and the average particle size of the liposomes in the resulting biomimetic liposome suspension is 80-150 nm.
[0013] Optionally, intermittent stirring is used during heat preservation and swelling, with a stirring speed of 50-100 rpm. Stirring is paused for 5-10 minutes every 10-15 minutes. After heat preservation and swelling are completed, the temperature is lowered to 40-45℃. The viscosity of the resulting gradient hyaluronic acid gel matrix is 5000-15000 mPa·s.
[0014] Optionally, the dispersion and emulsification treatment is carried out using a vacuum homogenizing emulsifier, wherein the working vacuum degree of the vacuum homogenizing emulsifier is -0.06 to -0.08 MPa and the linear velocity of the homogenizing head is 10-20 m / s; after the dispersion and emulsification treatment is completed, the mixture is kept at 35-40℃ and stirred for 20-30 minutes for aging treatment, so that the biomimetic liposomes and the gradient hyaluronic acid gel matrix form an interpenetrating network structure.
[0015] This invention utilizes a combined process of ethanol injection and high-pressure homogenization to prepare biomimetic liposomes with small particle size and uniform distribution. This significantly improves the dispersibility and transdermal absorption capacity of poorly soluble components. Furthermore, a specific order of addition effectively inhibits the agglomeration of high-molecular-weight hyaluronic acid, constructing a uniform and stable gel matrix. By controlling the emulsification temperature and rotation speed, the liposomes are firmly embedded in the three-dimensional network structure of hyaluronic acid to form an interpenetrating network. This not only simulates the skin barrier structure to achieve deep penetration and three-dimensional water retention, but also greatly enhances the physical stability and long-lasting moisturizing performance of the system. At the same time, adjusting the pH value to a slightly acidic environment ensures the gentleness of the product and its skin barrier repair function. Attached Figure Description
[0016] Figure 1 This is a schematic flowchart of a method for preparing a biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid according to an embodiment of the present invention. The objectives, features, and advantages of this invention will be further explained in conjunction with the embodiments and with reference to the accompanying drawings. Detailed Implementation
[0017] It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. Example 1
[0018] The biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid in the embodiments of the present invention consists of the following components in parts by weight: 2 parts of gradient molecular weight hyaluronic acid complex, 3 parts of biomimetic lipid carrier, 10 parts of polyol moisturizer, 2 parts of emulsifier, 0.1 parts of pH adjuster, and deionized water to make up to 100 parts.
[0019] The gradient molecular weight hyaluronic acid complex is composed of oligomeric hyaluronic acid, low molecular weight hyaluronic acid, medium molecular weight hyaluronic acid and high molecular weight hyaluronic acid in a mass ratio of 0.8:1.5:1.5:0.08.
[0020] The biomimetic lipid carrier is composed of ceramide NP, plant-derived cholesterol, and hydrogenated lecithin in a mass ratio of 2:1.5:4.
[0021] The polyol moisturizer is a compound of glycerin and butylene glycol in a mass ratio of 3:1.5.
[0022] The emulsifier is a compound of polysorbate-60 and glyceryl stearate in a mass ratio of 1.5:1.
[0023] The pH adjuster is triethanolamine. Example 2
[0024] In this embodiment, the preparation method of the biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid includes: S1. Ceramide, cholesterol and hydrogenated lecithin are dissolved in anhydrous ethanol according to the mass ratio in the biomimetic lipid carrier, injected into phosphate buffer at a temperature of 55-60℃, ethanol is removed by vacuum evaporation, and the mixture is homogenized under high pressure to obtain a biomimetic liposome suspension. S2. Mix the polyol moisturizer with a portion of deionized water and heat to 45-50℃. While stirring, add oligomeric hyaluronic acid, low molecular weight hyaluronic acid, and medium molecular weight hyaluronic acid in the order of increasing molecular weight of each component in the gradient molecular weight hyaluronic acid complex. After stirring and dissolving, add high molecular weight hyaluronic acid last. The addition ratio of oligomeric hyaluronic acid, low molecular weight hyaluronic acid, medium molecular weight hyaluronic acid, and high molecular weight hyaluronic acid is based on the mass ratio in the gradient molecular weight hyaluronic acid complex. Continue stirring and heat to 60-65℃, and keep warm to swell for 2-4 hours to obtain a gradient hyaluronic acid gel matrix. S3. Mix the biomimetic liposome suspension, emulsifier, and remaining deionized water obtained in step S1, preheat to 70-75°C, stir evenly, and then cool to 40-45°C. Then add it to the gradient hyaluronic acid gel matrix obtained in step S2, and perform dispersion and emulsification treatment at a homogenization speed of 3000-5000 rpm for 15-20 minutes. Cool to 35-40°C, add pH adjuster to adjust the pH value of the system to 5.5-6.5, filter and discharge to obtain the biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid.
[0025] Comparative Example 1 This comparative example provides a moisturizing composition that differs from Example 1 only in that it does not contain a biomimetic lipid carrier, while all other components and their contents are the same.
[0026] Comparative Example 2 This comparative example provides a moisturizing composition, which differs from Example 1 only in that the gradient molecular weight hyaluronic acid complex is replaced with an equal amount of a single high molecular weight hyaluronic acid (molecular weight 1200kDa), while the other components and contents are the same.
[0027] Comparative Example 3 This comparative example provides a moisturizing composition, which differs from Example 1 only in that: in the preparation process, the order of adding hyaluronic acid in step S2 is changed to adding it all at once, instead of adding it in order of increasing molecular weight; the other steps are the same.
[0028] Performance testing The compositions obtained in Example 1 and Comparative Examples 1-3 were subjected to performance tests.
[0029] Moisturizing performance test: Sixty healthy subjects aged 20-45 years were selected and divided into 6 groups of 10 each. An equal amount of sample was applied to the inner forearm of each subject. The stratum corneum moisture content of the skin was measured before application and at 1h, 2h, 4h and 8h after application using a skin moisture meter. The increase in moisture content was calculated and the average value was taken. The results are shown in Table 1.
[0030] Stability test: The samples were subjected to thermal cycling tests at -10℃ and 45℃ (24 hours per cycle, 5 cycles in total). The samples were observed for stratification, precipitation, or demulsification. The results are shown in Table 1.
[0031] As shown in Table 1, the biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid prepared in Example 1 of this invention maintained a high skin moisture content for 8 hours after application, demonstrating excellent long-lasting moisturizing performance. In contrast, Comparative Example 1, lacking a biomimetic lipid carrier, and Comparative Example 2, containing a single molecular weight hyaluronic acid, showed a significant decrease in long-lasting moisturizing ability, indicating that this invention significantly enhances water-locking capacity through the synergistic effect of biomimetic liposomes and gradient hyaluronic acid. Furthermore, Comparative Example 3, due to changes in the order of addition, resulted in poorer system stability and a slightly inferior moisturizing effect compared to Example 1, proving that the specific preparation process of this invention is crucial for ensuring product quality.
[0032] See Figure 1 The diagram shown is a flowchart illustrating a method for preparing a biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid according to an embodiment of the present invention: S1. Ceramide, cholesterol and hydrogenated lecithin are dissolved in anhydrous ethanol according to the mass ratio in the biomimetic lipid carrier, injected into phosphate buffer at a temperature of 55-60℃, ethanol is removed by vacuum evaporation, and the mixture is homogenized under high pressure to obtain a biomimetic liposome suspension.
[0033] This invention dissolves ceramide, cholesterol, and hydrogenated lecithin in anhydrous ethanol according to the mass ratio in the biomimetic lipid carrier, injects the solution into a phosphate buffer solution at 55-60°C, removes the ethanol by vacuum evaporation, and then homogenizes under high pressure to obtain a biomimetic liposome suspension. The synergistic effect of ethanol injection and high-pressure homogenization produces biomimetic liposomes with small particle size and uniform distribution, significantly improving the dispersibility and transdermal absorption capacity of poorly soluble components, and enhancing the long-lasting moisturizing and water-locking properties of the composition by mimicking the skin barrier structure. The anhydrous ethanol refers to an ethanol solvent with a purity greater than 99.7% and a water content less than 0.5%. The phosphate buffer solution is an aqueous solution prepared by mixing a 0.01-0.1 mol / L sodium dihydrogen phosphate solution and a 0.01-0.1 mol / L disodium hydrogen phosphate solution in a volume ratio ranging from (1:9) to (9:1).
[0034] Specifically, the biomimetic lipid carrier has a mass fraction of 2-4 parts, and the mass ratio of ceramide to hydrogenated lecithin is (1.5-2.5):(3.5-4.5).
[0035] Specifically, in the biomimetic lipid carrier, the ceramide is at least one of ceramide NP, ceramide AP, and ceramide EOP, the cholesterol is plant-derived cholesterol, and the hydrogenation degree of the hydrogenated lecithin is ≥90%.
[0036] Wherein, ceramide refers to a lipid molecule formed by the sphingosine backbone and fatty acids linked by amide bonds; ceramide NP refers to a non-hydroxylated ceramide formed by the combination of phytosphingosine and stearic acid; ceramide AP refers to α-hydroxyceramide; ceramide EOP refers to a ceramide containing linoleic acid chains; plant-derived cholesterol refers to cholesterol obtained from vegetable oils such as soybean oil, rapeseed oil, or palm oil through extraction and purification; hydrogenated lecithin refers to a solid phospholipid derivative obtained by hydrogenation addition reaction of unsaturated fatty acid chains in natural lecithin (such as soybean lecithin or egg yolk lecithin); and the degree of hydrogenation refers to the percentage of unsaturated fatty acid double bonds saturated by hydrogen atoms during the preparation of hydrogenated lecithin. The higher the degree of hydrogenation, the stronger the oxidative stability of the product and the lower the iodine value.
[0037] Specifically, the concentration of the phosphate buffer solution is 0.01-0.05 mol / L, and its pH value is 6.5-7.0.
[0038] Specifically, the homogenization process employs a two-stage homogenization process, wherein the first-stage homogenization pressure is 800-1000 bar, the second-stage homogenization pressure is 200-400 bar, and the homogenization cycle is 3-5 times. The resulting biomimetic liposome suspension has an average liposome particle size of 80-150 nm.
[0039] The two-stage homogenization refers to a homogenization process in which materials are passed sequentially through two series-connected homogenizing valves. The first-stage homogenizing valve mainly utilizes high-pressure shear force and cavitation effect to break particles to the micron or nanometer scale. The second-stage homogenizing valve disperses and homogenizes the broken particles at a lower pressure to prevent particle re-aggregation, thereby obtaining an emulsion or suspension with a narrower particle size distribution and a more stable system. The first-stage homogenizing pressure refers to the inlet pressure value displayed by the pressure gauge of the homogenizer when the material passes through the first-stage homogenizing valve. The second-stage homogenizing pressure refers to the pressure set value when the material enters the second-stage homogenizing valve after passing through the first-stage homogenizing valve. The homogenization cycle number refers to the number of times the material is processed through the homogenizing valve of the high-pressure homogenizer. The biomimetic liposome suspension refers to a closed vesicle dispersion system with a bilayer structure formed by ceramide, cholesterol, and hydrogenated lecithin in an aqueous medium. The liposome refers to a bilayer closed vesicle structure composed of lipid molecules such as phospholipids and cholesterol.
[0040] S2. Mix the polyol moisturizer with a portion of deionized water and heat to 45-50℃. While stirring, add oligomeric hyaluronic acid, low molecular weight hyaluronic acid, and medium molecular weight hyaluronic acid in the order of increasing molecular weight of each component in the gradient molecular weight hyaluronic acid complex. After stirring and dissolving, add high molecular weight hyaluronic acid last. The addition ratio of oligomeric hyaluronic acid, low molecular weight hyaluronic acid, medium molecular weight hyaluronic acid, and high molecular weight hyaluronic acid is based on the mass ratio in the gradient molecular weight hyaluronic acid complex. Continue stirring and heat to 60-65℃, and keep warm to swell for 2-4 hours to obtain a gradient hyaluronic acid gel matrix.
[0041] This invention involves mixing a polyol humectant with a portion of deionized water and heating the mixture to 45-50°C. This appropriate temperature increase significantly reduces the viscosity of the polyol and increases the kinetic energy of solvent molecules, thereby accelerating the dissolution and dispersion rate of the polyol in the aqueous phase. Simultaneously, it provides a warm hydration environment for the subsequent swelling of hyaluronic acid, avoiding clumping or uneven dispersion problems caused by low-temperature dissolution. The deionized water refers to the portion of deionized water pre-allocated from the total water volume of the formulation during the aqueous phase preparation stage of the preparation process. This deionized water is used to pre-dissolve the polyol humectant and create a warm solvent environment; its amount is typically 30%-50% of the total water volume of the formulation.
[0042] Specifically, the polyol moisturizer is a compound of glycerin and butylene glycol, wherein the mass ratio of glycerin to butylene glycol is (2-4):(1-2).
[0043] The polyol moisturizer refers to an organic compound containing two or more hydroxyl groups in its molecular structure. Glycerin refers to glycerol, a colorless, odorless, sweet-tasting, transparent, viscous liquid containing three hydroxyl groups. It has strong hygroscopicity and water solubility, and is one of the most basic and widely used moisturizers in the cosmetics industry. Its main function is to absorb moisture from the environment and keep the stratum corneum moist. Butylene glycol is 1,3-butanediol, a colorless, transparent, viscous liquid. Compared to glycerin, it has lower viscosity, a more refreshing feel on the skin, and good antibacterial and antifreeze properties. It is often used in combination with glycerin to adjust the viscosity of the composition, improve the skin feel, and enhance the stability of the moisturizing system.
[0044] In this invention, under stirring, oligomeric hyaluronic acid, low molecular weight hyaluronic acid, and medium molecular weight hyaluronic acid are added sequentially according to the increasing molecular weight of the components in the gradient molecular weight hyaluronic acid complex. After stirring and dissolving, high molecular weight hyaluronic acid is added last. This sequential addition utilizes the advantages of low molecular weight hyaluronic acid—fast dissolution and low steric hindrance—to preferentially occupy the aqueous phase space, effectively suppressing the "agglomeration" phenomenon caused by the rapid water absorption and swelling of high molecular weight hyaluronic acid. This significantly improves the uniformity of complex dissolution and shortens the swelling time, facilitating the formation of a stable and uniform network moisturizing structure. Specifically, oligomeric hyaluronic acid refers to hyaluronic acid with a molecular weight less than or equal to 10 kDa, low molecular weight hyaluronic acid refers to hyaluronic acid with a molecular weight range of 10 kDa to 100 kDa, medium molecular weight hyaluronic acid refers to hyaluronic acid with a molecular weight range of 100 kDa to 500 kDa, and high molecular weight hyaluronic acid refers to hyaluronic acid with a molecular weight range of 1000 kDa to 1500 kDa.
[0045] Specifically, the mass fraction of the gradient molecular weight hyaluronic acid complex is 1-3 parts; the mass ratio of oligomeric hyaluronic acid to high molecular weight hyaluronic acid is (0.6-0.9):(0.06-0.09).
[0046] The mass fractions refer to the proportion of each component in the total mass of the composition.
[0047] Specifically, in the gradient molecular weight hyaluronic acid complex, the oligomeric hyaluronic acid has a molecular weight ≤10kDa, the low molecular weight hyaluronic acid has a molecular weight of 10-100kDa, the medium molecular weight hyaluronic acid has a molecular weight of 100-500kDa, and the high molecular weight hyaluronic acid has a molecular weight of 1000-1500kDa.
[0048] The molecular weight mentioned refers to the weight-average molecular weight of hyaluronic acid.
[0049] After stirring and dissolving, high molecular weight hyaluronic acid is added last. The addition ratio of oligomeric hyaluronic acid, low molecular weight hyaluronic acid, medium molecular weight hyaluronic acid and high molecular weight hyaluronic acid is according to the mass ratio in the gradient molecular weight hyaluronic acid complex. Stirring continues and the temperature is raised to 60-65℃. The mixture is kept warm and swelled for 2-4 hours to obtain a gradient hyaluronic acid gel matrix. The heating accelerates the movement of molecular chains and promotes the full expansion and swelling of high molecular weight hyaluronic acid at a specific temperature. Combined with the gradient sequential addition process, it ensures that the multi-molecular weight hyaluronic acid forms a uniform, non-agglomerated, high-viscosity, and stable gel matrix with a three-dimensional network structure.
[0050] In detail, the process of heat preservation and swelling is accompanied by intermittent stirring at a speed of 50-100 rpm. The stirring is paused for 5-10 minutes every 10-15 minutes. After the heat preservation and swelling is completed, the temperature is lowered to 40-45℃. The viscosity of the resulting gradient hyaluronic acid gel matrix is 5000-15000 mPa·s.
[0051] The heat-insulating swelling refers to the process of allowing high molecular weight hyaluronic acid particles to fully absorb water and expand in volume in a solvent at a constant temperature, with the molecular chains gradually extending from a coiled state and becoming uniformly dispersed in the solution. The intermittent stirring refers to the operation mode of the stirring device alternating between "operation-stop" according to a set time cycle during the swelling process. The gradient hyaluronic acid gel matrix refers to a semi-transparent viscous liquid with a three-dimensional network structure formed by dissolving and swelling oligomeric, low molecular weight, medium molecular weight, and high molecular weight hyaluronic acid in a specific ratio. The viscosity refers to the fluid flow resistance measured by a rotational viscometer under specific rotation speed and rotor conditions.
[0052] S3. Mix the biomimetic liposome suspension, emulsifier, and remaining deionized water obtained in step S1, preheat to 70-75°C, stir evenly, and then cool to 40-45°C. Then add it to the gradient hyaluronic acid gel matrix obtained in step S2, and perform dispersion and emulsification treatment at a homogenization speed of 3000-5000 rpm for 15-20 minutes. Cool to 35-40°C, add pH adjuster to adjust the pH value of the system to 5.5-6.5, filter and discharge to obtain the biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid.
[0053] This invention involves mixing the biomimetic liposome suspension obtained in step S1, the emulsifier, and the remaining deionized water, preheating to 70-75°C, stirring until homogeneous, and then cooling to 40-45°C. This high-temperature preheating ensures thorough dispersion of the biomimetic liposomes and emulsifier, forming a uniform pre-emulsion system. Subsequently, the temperature is lowered to a suitable level, avoiding damage to the heat-sensitive active ingredients and providing an optimal process window and physical compatibility for subsequent mixing with the hyaluronic acid gel matrix. The remaining deionized water refers to the portion of deionized water remaining in the total water volume of the formulation after deducting the "partial deionized water" used to dissolve the polyol humectant in step S2.
[0054] Specifically, the emulsifier is a compound of polysorbate-60 and glyceryl stearate, with a mass ratio of (1-2):(1-1.5).
[0055] Among them, polysorbate-60 refers to polyoxyethylene (20) sorbitan monostearate, which is a nonionic oil-in-water (O / W) emulsifier, and glyceryl stearate refers to glyceryl monostearate, which is a nonionic emulsifier.
[0056] The present invention is then added to the gradient hyaluronic acid gel matrix obtained in step S2, and dispersed and emulsified for 15-20 minutes under the condition of homogenization speed of 3000-5000 rpm. The high shear homogenization force breaks the phase interface barrier, so that the biomimetic liposome microparticles are uniformly embedded and stably loaded in the three-dimensional network structure of the hyaluronic acid gel matrix, which significantly improves the dispersion uniformity and physical stability of the multiphase system, while avoiding the destruction of the gel structure caused by excessively high local concentration.
[0057] In detail, the dispersion and emulsification treatment is carried out using a vacuum homogenizing emulsifier with a working vacuum degree of -0.06 to -0.08 MPa and a homogenizing head linear velocity of 10-20 m / s. After the dispersion and emulsification treatment is completed, the mixture is kept at 35-40℃ and stirred for 20-30 minutes for aging treatment, so that the biomimetic liposomes and the gradient hyaluronic acid gel matrix form an interpenetrating network structure.
[0058] The vacuum homogenizing emulsifier refers to an industrial preparation equipment that integrates vacuum degassing, high-speed shearing, and homogenizing emulsification. The working vacuum degree refers to the value at which the internal pressure of the emulsification tank is lower than atmospheric pressure during the operation of the vacuum homogenizing emulsifier. The homogenizing head linear velocity refers to a parameter that characterizes the change of the instantaneous velocity of a certain point on the rotor of the vacuum homogenizing emulsifier with the radius of rotation. The aging treatment refers to keeping the mixed colloidal system at a specific temperature and time condition. The interpenetrating network structure refers to the interpenetration and entanglement of the lipid bilayer membrane structure of biomimetic liposomes and the three-dimensional network structure of gradient hyaluronic acid molecules at the microscale, forming a physical cross-linking point structure.
[0059] This invention involves cooling the system to 35-40℃, adding a pH adjuster to adjust the pH to 5.5-6.5, and filtering the mixture to obtain the biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid. This adjusts the system to a slightly acidic environment compatible with the natural pH of human skin, ensuring the product's gentleness and skin barrier repair function. Simultaneously, filtration removes impurities, ultimately resulting in a stable and safe finished product. The biomimetic moisturizing composition refers to a functional product formed by combining a gradient molecular weight hyaluronic acid gel matrix and biomimetic liposomes under specific process conditions through a physical interpenetrating network structure. This composition mimics the composition of natural skin moisturizing factors and the lipid structure of the skin barrier, exhibiting excellent skin affinity, permeability, and long-lasting moisturizing properties.
[0060] Specifically, after adjusting the pH of the system to 5.5-6.5 by adding a pH adjuster, the process further includes: cooling to 30-35°C, adding 0.1-0.5 parts of preservative and 0.01-0.1 parts of fragrance, continuing to stir for 10-15 minutes, and then filtering and discharging the material; the preservative is selected from at least one of methylparaben, propylparaben, and phenoxyethanol.
[0061] The preservatives mentioned herein refer to additives used to inhibit the growth and reproduction of microorganisms, prevent product spoilage and deterioration, and thus extend the shelf life of cosmetics. The filtration process refers to the operation of passing the final mixture through a filter screen or filter cloth with a specific pore size (such as 100-200 mesh) in the final stage of the preparation process. Methylparaben refers to methylparaben, a colorless crystal or white crystalline powder. Propylparaben refers to propylparaben, a colorless fine crystal or white crystalline powder. Phenoxyethanol refers to a colorless, slightly viscous liquid.
Claims
1. A biomimetic moisturizing composition containing hyaluronic acid with gradient molecular weights, characterized in that, Composed of the following components in parts by mass composition: 0.1-5 parts of gradient molecular weight hyaluronic acid complex, 1-5 parts of biomimetic lipid carrier, 5-15 parts of polyol moisturizer, 1-3 parts of emulsifier, 0.01-0.5 parts of pH adjuster, and deionized water to make up to 100 parts. The gradient molecular weight hyaluronic acid complex is composed of oligomeric hyaluronic acid, low molecular weight hyaluronic acid, medium molecular weight hyaluronic acid and high molecular weight hyaluronic acid in a mass ratio of (0.5-1):(1-2):(1-2):(0.05-0.1); The biomimetic lipid carrier is composed of ceramide, cholesterol and hydrogenated lecithin in a mass ratio of (1-3):(1-2):(3-5).
2. The biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid as described in claim 1, characterized in that, The biomimetic lipid carrier has a mass fraction of 2-4 parts, and the mass ratio of ceramide to hydrogenated lecithin is (1.5-2.5):(3.5-4.5).
3. The biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid as described in claim 1, characterized in that, In the biomimetic lipid carrier, the ceramide is at least one of ceramide NP, ceramide AP, and ceramide EOP, the cholesterol is plant-derived cholesterol, and the hydrogenation degree of the hydrogenated lecithin is ≥90%.
4. The biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid as described in claim 1 and its preparation method, characterized in that, The polyol moisturizer is a compound of glycerin and butylene glycol, wherein the mass ratio of glycerin to butylene glycol is (2-4):(1-2).
5. The biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid as described in claim 1, characterized in that, The mass fraction of the gradient molecular weight hyaluronic acid complex is 1-3 parts; the mass ratio of the oligomeric hyaluronic acid to the high molecular weight hyaluronic acid is (0.6-0.9):(0.06-0.09).
6. The biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid as described in claim 1, characterized in that, In the gradient molecular weight hyaluronic acid complex, the molecular weight of the oligomeric hyaluronic acid is ≤10kDa, the molecular weight of the low molecular weight hyaluronic acid is 10-100kDa, the molecular weight of the medium molecular weight hyaluronic acid is 100-500kDa, and the molecular weight of the high molecular weight hyaluronic acid is 1000-1500kDa.
7. A method for preparing a biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid according to any one of claims 1-6, characterized in that, The method includes: S1. Ceramide, cholesterol and hydrogenated lecithin are dissolved in anhydrous ethanol according to the mass ratio in the biomimetic lipid carrier, injected into phosphate buffer at a temperature of 55-60℃, ethanol is removed by vacuum evaporation, and the mixture is homogenized under high pressure to obtain a biomimetic liposome suspension. S2. Mix the polyol moisturizer with a portion of deionized water and heat to 45-50℃. While stirring, add oligomeric hyaluronic acid, low molecular weight hyaluronic acid, and medium molecular weight hyaluronic acid in the order of increasing molecular weight of each component in the gradient molecular weight hyaluronic acid complex. After stirring and dissolving, add high molecular weight hyaluronic acid last. The addition ratio of oligomeric hyaluronic acid, low molecular weight hyaluronic acid, medium molecular weight hyaluronic acid, and high molecular weight hyaluronic acid is based on the mass ratio in the gradient molecular weight hyaluronic acid complex. Continue stirring and heat to 60-65℃, and keep warm to swell for 2-4 hours to obtain a gradient hyaluronic acid gel matrix. S3. Mix the biomimetic liposome suspension, emulsifier, and remaining deionized water obtained in step S1, preheat to 70-75°C, stir evenly, and then cool to 40-45°C. Then add it to the gradient hyaluronic acid gel matrix obtained in step S2, and perform dispersion and emulsification treatment at a homogenization speed of 3000-5000 rpm for 15-20 minutes. Cool to 35-40°C, add pH adjuster to adjust the pH value of the system to 5.5-6.5, filter and discharge to obtain the biomimetic moisturizing composition containing gradient molecular weight hyaluronic acid.
8. The method as described in claim 7, characterized in that, The homogenization process employs a two-stage homogenization process. The first-stage homogenization pressure is 800-1000 bar, and the second-stage homogenization pressure is 200-400 bar. The homogenization cycle is 3-5 times. The resulting biomimetic liposome suspension has an average liposome particle size of 80-150 nm.
9. The preparation method according to claim 7, characterized in that, While maintaining the temperature and swelling, intermittent stirring is used at a speed of 50-100 rpm. Stirring is paused for 5-10 minutes every 10-15 minutes. After the temperature and swelling are completed, the temperature is lowered to 40-45℃. The viscosity of the resulting gradient hyaluronic acid gel matrix is 5000-15000 mPa·s.
10. The method as described in claim 7, characterized in that, The dispersion and emulsification process was carried out using a vacuum homogenizer with a working vacuum of -0.06 to -0.08 MPa and a homogenizer head linear velocity of 10-20 m / s. After the dispersion and emulsification process, the mixture was kept at 35-40℃ and stirred for 20-30 minutes for aging, so that the biomimetic liposomes and the gradient hyaluronic acid gel matrix formed an interpenetrating network structure.