An anti-wrinkle composition containing recombinant collagen and preparation method thereof

Abstract

The present invention provides an anti-wrinkle composition containing recombinant collagen, the anti-wrinkle composition containing recombinant collagen includes the following components by mass fraction: 5-10% recombinant human collagen, 0.5-1% organic-inorganic-modified titanium dioxide, 1-3% squalane, 1-2% sodium hyaluronate, 15-35% oil, 3-5% emulsifier, 3-5% adjuvant, and water balance; wherein the organic-inorganic-modified titanium dioxide is a titanium dioxide nanoparticle with a citric acid grafted outer layer and a silicon dioxide layer wrapped inner layer. The organic-inorganic-modified titanium dioxide of the present invention has good amphiphilicity, good compatibility with other components such as recombinant human collagen, squalane and sodium hyaluronate, can enhance the synergistic effect between components, and enhance the anti-wrinkle effect of the anti-wrinkle composition; at the same time, the organic-inorganic-modified titanium dioxide also has a good anti-ultraviolet effect, which can further enhance the anti-wrinkle effect of the anti-wrinkle composition.

Description

Technical Field

[0001] The invention relates to the field of cosmetics, and in particular to an anti-wrinkle composition containing recombinant collagen and a preparation method thereof. Background Art

[0002] With the development of society and the improvement of people's living standards, the demand for beauty and skin care is growing. Skin aging is part of the natural physiological process, but people are always looking for ways to slow down this process. Wrinkles are one of the obvious signs of skin aging, and their formation is a complex process involving multiple internal and external factors. With age, the skin gradually loses elasticity and moisture, and the reduction of collagen and elastin causes the skin to become thinner, thus forming wrinkles; in addition, ultraviolet radiation is an important factor leading to skin aging and wrinkle formation, which can destroy collagen and elastin in the skin, causing the skin to lose elasticity. Therefore, the development of effective anti-wrinkle products has become an important research direction in the cosmetics and skin care industry.

[0003] Among the many anti-wrinkle ingredients, recombinant collagen has attracted much attention due to its key role in maintaining skin elasticity and structure. Recombinant human collagen is produced through bioengineering technology and is highly similar to the body's own collagen. It has better biocompatibility and lower immunogenicity. It can promote the proliferation and differentiation of skin cells and enhance the skin's self-repair ability, thereby reducing the formation of wrinkles.

[0004] Most anti-wrinkle products on the market currently use recombinant collagen combined with other active ingredients such as sodium hyaluronate and squalane to achieve better anti-wrinkle effects. These ingredients help improve the skin's ability to retain moisture, thereby reducing the formation of wrinkles. However, due to the differences in the hydrophilicity and lipophilicity of these active ingredients, compatibility issues have become a challenge in product development. If not handled properly, it can easily lead to reduced product stability, precipitation, stratification and other phenomena, affecting the anti-wrinkle effect or the appearance and user experience of the product.

[0005] Based on this, it is urgent to propose a technical solution to solve the above-mentioned problems. Summary of the invention

[0006] Based on this, the present invention provides an anti-wrinkle composition containing recombinant collagen and a preparation method thereof, wherein the anti-wrinkle composition is prepared from recombinant human collagen, organic-inorganic-modified titanium dioxide, squalane and sodium hyaluronate, etc. The organic-inorganic-modified titanium dioxide is obtained by first inorganically treating the surface of nano-TiO2 with SiO2 and then organically coating it with citric acid, wherein the outer layer is grafted with citric acid and the inner layer is wrapped with a silicon dioxide layer, and the composition has good amphiphilicity, good compatibility with other components such as recombinant human collagen, squalane and sodium hyaluronate, and can enhance the synergistic effect between the components and enhance the anti-wrinkle effect of the anti-wrinkle composition.

[0007] One object of the present invention is to provide an anti-wrinkle composition containing recombinant collagen, wherein the anti-wrinkle composition containing recombinant collagen comprises the following components in mass fractions:

[0008] Recombinant human collagen 5-10%

[0009]

[0010] in,

[0011] The organic-inorganic-modified titanium dioxide is titanium dioxide nanoparticles with a citric acid grafted outer layer and a silicon dioxide layer wrapped inner layer.

[0012] Furthermore, the recombinant human collagen is selected from one or more of type 1 recombinant human collagen, type 3 recombinant human collagen or type 17 recombinant human collagen.

[0013] Furthermore, the oil is selected from one or more of jojoba oil, sweet almond oil, coconut oil or olive oil.

[0014] Furthermore, the emulsifier is selected from one or more of beeswax, carnauba wax or lecithin.

[0015] Furthermore, the auxiliary agent is selected from one or more of moisturizers, emollients, skin conditioners, antioxidants, thickeners, pH regulators, preservatives, antibacterial agents or fragrances.

[0016] Another object of the present invention is to provide a method for preparing the above anti-wrinkle composition containing recombinant collagen, comprising the following steps:

[0017] S1. Add titanium dioxide into water, stir and disperse, add sodium hexametaphosphate, disperse by ultrasonic to obtain titanium dioxide slurry, then add sodium silicate, adjust pH, heat and react to form an intermediate product;

[0018] S2, soaking the intermediate product in strong acid and hydrogen peroxide, heating for reaction, and obtaining a hydroxylated intermediate product;

[0019] S3, immersing the hydroxylated intermediate product in an aqueous solution of citric acid, heating and ultrasonically reacting the mixture to obtain an organic-inorganic-modified titanium dioxide;

[0020] S4, heating the water, adding the auxiliary agent, stirring and dissolving, and obtaining an aqueous phase;

[0021] S5, heating the oil and adding an emulsifier, stirring and dispersing, to obtain an oil phase;

[0022] S6. Under stirring, add the oil phase to the water phase and stir to form an emulsion; cool down, add recombinant human collagen, organic-inorganic-modified titanium dioxide, squalane and sodium hyaluronate, stir, adjust the pH, and obtain an anti-wrinkle composition containing recombinant collagen.

[0023] Furthermore, in step S1, the mass ratio of titanium dioxide to sodium silicate is 1:(0.25-1).

[0024] Furthermore, in step S1, the heating temperature is 80-100°C, and the reaction time is 4-6h.

[0025] Furthermore, in step S1, the pH is 8-10.

[0026] Furthermore, in step S2, the heating temperature is 80-100° C., and the reaction time is 1-3 h.

[0027] Furthermore, in step S3, the mass ratio of the hydroxylated intermediate product to citric acid is 1:(3-8).

[0028] Furthermore, in step S3, the heating temperature is 60-80° C., and the reaction time is 8-12 h.

[0029] Furthermore, in step S4, the heating temperature is 70-80°C.

[0030] Furthermore, in step S5, the heating temperature is 70-80°C.

[0031] Furthermore, in step S6, the cooling temperature is 30-40°C.

[0032] Furthermore, in step S6, the pH is 5-6.

[0033] The present invention has the following beneficial effects:

[0034] The invention provides an anti-wrinkle composition containing recombinant collagen and a preparation method thereof. The anti-wrinkle composition containing recombinant collagen is prepared from components such as recombinant human collagen, organic-inorganic-modified titanium dioxide, squalane and sodium hyaluronate. The present invention firstly uses sodium silicate to treat nano-TiO2, so that silicon is precipitated in the form of orthosilicic acid monomer or silicate polymer, and is firmly bonded to the hydroxyl group on the surface of the nano-TiO2 by chemical bonding to form a nucleation point, and then polycondenses to generate a silicon polymer, and finally forms a layer of continuous SiO2 solid film to form TiO2-SiO2 composite particles, thereby improving the dispersibility, hydrophilicity, light resistance, weather resistance, anti-powdering and stability of the nano-TiO2; at the same time, the present invention combines citric acid having carboxyl and hydroxyl groups with the hydroxylated composite particles to obtain organic-inorganic-modified titanium dioxide, and the modified titanium dioxide particles have good compatibility with other components such as recombinant human collagen, squalane and sodium hyaluronate, which not only enhances the stability of the composition, but also can adsorb and combine other active components through intermolecular forces, enhance the synergistic effect between the components, and is conducive to promoting the absorption and effectiveness of the active components, thereby enhancing the anti-wrinkle effect of the anti-wrinkle composition. In addition, the SiO2 film in the organic-inorganic-modified titanium dioxide can establish a barrier between the nano-TiO2 and the surrounding medium, reduce the transmittance of ultraviolet rays, reduce the damage of ultraviolet rays to the skin, and further enhance the anti-wrinkle effect of the anti-wrinkle composition. DETAILED DESCRIPTION

[0035] The following will be combined with the embodiments to clearly and completely describe the concept of the present invention and the technical effects produced, so as to fully understand the purpose, characteristics and effects of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, other embodiments obtained by those skilled in the art without creative work are all within the scope of protection of the present invention.

[0036] Unless otherwise stated, the raw materials, reactions and post-treatment methods mentioned in the examples are common raw materials on the market and technical methods well known to those skilled in the art.

[0037] The molecular weight of the type 1 recombinant human collagen in the examples and comparative examples of the present invention is 40w-200w, and is purchased from Hesheng Chuangyan.

[0038] The molecular weight of the type 3 recombinant human collagen in the examples and comparative examples of the present invention is 20w-300w, and is purchased from Hesheng Chuangyan.

[0039] The molecular weight of the type 17 recombinant human collagen in the examples and comparative examples of the present invention is 1000-20w, and is purchased from Shiguang Xinya.

[0040] The molecular weight of the sodium hyaluronate in the examples and comparative examples of the present invention is 1.5-3.9 million, and is purchased from Avituo (Shanghai) Pharmaceutical Technology Co., Ltd.

[0041] Example 1

[0042] An anti-wrinkle composition containing recombinant collagen, comprising the following components in mass fractions:

[0043]

[0044] in,

[0045] The organic-inorganic-modified titanium dioxide is titanium dioxide nanoparticles with a citric acid grafted outer layer and a silicon dioxide layer wrapped inner layer.

[0046] The method for preparing the anti-wrinkle composition containing recombinant collagen comprises the following steps:

[0047] S1. Add nano titanium dioxide into deionized water, stir and disperse to form a suspension, add sodium hexametaphosphate, and ultrasonically disperse for 10 minutes to obtain titanium dioxide slurry, then add sodium silicate (titanium dioxide: deionized water: sodium hexametaphosphate: sodium silicate = 100:500:0.25:25, m / m / m / m), adjust the pH to 9 with 1 mol / L sulfuric acid, react at 90°C for 5 hours, filter, wash, and dry to obtain an intermediate product;

[0048] S2, soaking the intermediate product in a mixed solution of concentrated sulfuric acid and hydrogen peroxide (concentrated sulfuric acid: hydrogen peroxide = 7:3, m / m, the concentration of the hydrogen peroxide is 30wt%), reacting at 80° C. for 1 h, filtering, washing, and drying to obtain a hydroxylated intermediate product;

[0049] S3, soaking the hydroxylated intermediate product in a 10 wt % citric acid aqueous solution (hydroxylated intermediate product: citric acid = 1:5, m / m), ultrasonically reacting for 10 h at 70° C., then filtering, washing, and drying to obtain organic-inorganic-modified titanium dioxide;

[0050] S4. According to the above mass fraction, deionized water is heated to 70°C, glycerol and potassium sorbate are added, and stirred at a speed of 200 r / min until completely dissolved to obtain an aqueous phase;

[0051] S5, heating the olive oil to 70°C, adding hydrogenated lecithin, and stirring at a speed of 100 r / min for 30 min to obtain an oil phase;

[0052] S6. Under the condition of a rotation speed of 100 r / min, the oil phase is added to the water phase, and stirring is continued for 30 minutes to form an emulsion; the emulsion is cooled to 30°C, and type 1 recombinant human collagen, type 3 recombinant human collagen, type 17 recombinant human collagen, organic-inorganic-modified titanium dioxide, squalane and sodium hyaluronate are added, and stirring is carried out for 30 minutes. The pH is adjusted to 6 with citric acid to obtain the anti-wrinkle composition containing recombinant collagen.

[0053] Example 2

[0054] An anti-wrinkle composition containing recombinant collagen, comprising the following components in mass fractions:

[0055]

[0056] in,

[0057] The organic-inorganic-modified titanium dioxide is titanium dioxide nanoparticles with a citric acid grafted outer layer and a silicon dioxide layer wrapped inner layer.

[0058] The preparation method of the above anti-wrinkle composition containing recombinant collagen is the same as that of Example 1.

[0059] Example 3

[0060] An anti-wrinkle composition containing recombinant collagen, comprising the following components in mass fractions:

[0061]

[0062] in,

[0063] The organic-inorganic-modified titanium dioxide is titanium dioxide nanoparticles with a citric acid grafted outer layer and a silicon dioxide layer wrapped inner layer.

[0064] The preparation method of the above anti-wrinkle composition containing recombinant collagen is the same as that of Example 1.

[0065] Comparative Example 1

[0066] An anti-wrinkle composition containing recombinant collagen. The difference between this comparative example and Example 1 is that step S1 is omitted, and in step S2, the mass of the intermediate product is replaced by titanium dioxide. Other ingredients and preparation methods are the same as those in Example 1.

[0067] Comparative Example 2

[0068] An anti-wrinkle composition containing recombinant collagen. The difference between this comparative example and Example 1 is that steps S2 and S3 are omitted, and in step S6, the mass of the organic-inorganic-modified titanium dioxide is replaced by the intermediate product. Other ingredients and preparation methods are the same as those in Example 1.

[0069] Test Case

[0070] The anti-wrinkle effects of Examples 1-3 and Comparative Examples 1-2 were tested.

[0071] Test method:

[0072] Subjects: 50 healthy female volunteers, aged 35-50 years old, with similar facial wrinkle levels. The subjects were randomly divided into 5 groups, 10 people in each group, and each group tried one sample. The subjects used the above samples for daily skin care, once in the morning and once in the evening, for 4 consecutive weeks. The number of wrinkles in the cheek wrinkle area of ​​the subjects and the degree of wrinkle area reduction were tested using the Antera 3D skin analyzer, and the average value of each group was taken.

[0073] The test results are shown in Table 1.

[0074] Table 1 Anti-wrinkle effect test results of Examples 1-3 and Comparative Examples 1-2

[0075]

[0076] From the above test results, it can be seen that after using the samples of Examples 1-3 of the present invention, the average reduction in the number of surface wrinkles, the average reduction in the area of ​​surface wrinkles, and the average reduction in the depth of surface wrinkles all have relatively excellent effects, indicating that the combination of the organic-inorganic-modified titanium dioxide of the present invention with recombinant human collagen, squalane, sodium hyaluronate and other ingredients can produce a synergistic effect and effectively improve the wrinkle removal effect of the product. In Comparative Example 1, nano-TiO2 was treated only with citric acid, and in Comparative Example 2, nano-TiO2 was treated only with SiO2, and their anti-wrinkle effects were worse than those of the present invention.

[0077] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Therefore, the embodiments should be considered exemplary and non-restrictive in all respects, and the scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims be included in the present invention.

[0078] In addition, it should be understood that although the present specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment may also be appropriately combined to form other implementation modes that can be understood by those skilled in the art.

Claims

1. An anti-wrinkle composition containing recombinant collagen, characterized in that: The anti-wrinkle composition containing recombinant collagen comprises the following components in mass fractions: in, The organic-inorganic-modified titanium dioxide is a titanium dioxide nanoparticle with a citric acid grafted outer layer and a silicon dioxide layer wrapped inner layer; The method for preparing the anti-wrinkle composition containing recombinant collagen comprises the following steps: S1. Add titanium dioxide into water, stir and disperse, add sodium hexametaphosphate, disperse by ultrasonic to obtain titanium dioxide slurry, then add sodium silicate, adjust pH, heat and react to form an intermediate product; S2, soaking the intermediate product in strong acid and hydrogen peroxide, heating for reaction, and obtaining a hydroxylated intermediate product; S3, immersing the hydroxylated intermediate product in an aqueous solution of citric acid, heating and ultrasonically reacting the mixture to obtain an organic-inorganic-modified titanium dioxide; S4, heating the water, adding the auxiliary agent, stirring and dissolving, and obtaining an aqueous phase; S5, heating the oil and adding an emulsifier, stirring and dispersing, to obtain an oil phase; S6. Under stirring, add the oil phase to the water phase and stir to form an emulsion; cool down, add recombinant human collagen, organic-inorganic-modified titanium dioxide, squalane and sodium hyaluronate, stir, adjust the pH, and obtain an anti-wrinkle composition containing recombinant collagen.

2. The anti-wrinkle composition containing recombinant collagen according to claim 1, characterized in that: The recombinant human collagen is selected from one or more of type 1 recombinant human collagen, type 3 recombinant human collagen or type 17 recombinant human collagen.

3. The anti-wrinkle composition containing recombinant collagen according to claim 1, characterized in that: The oil is selected from one or more of jojoba oil, sweet almond oil, coconut oil or olive oil.

4. The anti-wrinkle composition containing recombinant collagen according to claim 1, characterized in that: The emulsifier is selected from one or more of beeswax, carnauba wax or lecithin.

5. The anti-wrinkle composition containing recombinant collagen according to claim 1, characterized in that: The auxiliary agent is selected from one or more of moisturizers, emollients, skin conditioners, antioxidants, thickeners, pH regulators, preservatives, antibacterial agents or fragrances.

6. The anti-wrinkle composition containing recombinant collagen according to claim 1, characterized in that: In step S1, the mass ratio of titanium dioxide to sodium silicate is 1:(0.25-1).

7. The anti-wrinkle composition containing recombinant collagen according to claim 1, characterized in that: In step S1, the heating temperature is 80-100°C and the reaction time is 4-6h.

8. The anti-wrinkle composition containing recombinant collagen according to claim 1, characterized in that: In step S3, the mass ratio of the hydroxylated intermediate product to citric acid is 1:(3-8).

9. The anti-wrinkle composition containing recombinant collagen according to claim 1, characterized in that: In step S3, the heating temperature is 60-80° C. and the reaction time is 8-12 h.

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