Cosmetic formula preparation process taking silicon-based composite material as carrier

Abstract

The invention relates to the technical field of cosmetic preparation, in particular to a cosmetic formula preparation process taking a silicon-based composite material as a carrier, which comprises the following steps of: homogenizing and mixing cyclopentasiloxane, phenyltrimethylsiloxane and nanospheres to form a phase A; heating and dissolving water, butanediol and sodium chloride into a phase B; adding a W / Si type emulsifier into the phase A, adding the phase B while stirring, keeping the temperature, and performing high-shear homogenization to form an emulsified body; then stirring and cooling the emulsified body, sequentially adding a xanthan gum solution for thickening and essence after cooling, homogenizing, degassing and filling to obtain a finished product. The cosmetic formula prepared by the invention shows remarkable advantages in the aspects of physical stability and active matter controlled release performance.

Description

Technical Field

[0001] This invention relates to the field of cosmetic preparation technology, and in particular to a cosmetic formulation preparation process using silicon-based composite materials as a carrier. Background Technology

[0002] Cosmetics, as daily chemical products used to improve skin condition and enhance appearance, depend not only on the active ingredients themselves but also on the carrier system and its delivery efficiency. An ideal carrier should possess good stability, biocompatibility, high loading capacity for active ingredients, and controllable release properties to ensure precise and long-lasting application of the active ingredients to the target skin area and improve the final product's feel. Currently, commonly used carriers in cosmetics include liposomes, microemulsions, polymer microspheres, and natural or synthetic esters.

[0003] Patent CN115282068A discloses an organic gel carrier, its preparation method, and cosmetics. This organic gel carrier is formed from components such as hydroxystearic acid, fatty acids, fatty acid esters, higher fatty alcohols, and surfactants, exhibiting good biocompatibility and stability against acids, alkalis, and electrolytes. However, this organic gel carrier primarily relies on the self-assembly structure of fatty acids and their derivatives. Its mechanical strength and thermal stability are significantly affected by environmental temperature and other components in the formulation. Long-term storage or extreme conditions may lead to structural softening or precipitation, affecting product stability and appearance. Furthermore, its loading of active ingredients mainly relies on physical encapsulation or dissolution, limiting its loading efficiency for hydrophilic components with significant polarity differences. Additionally, the organic gel system itself may result in a greasy or heavy skin feel, impacting the user experience.

[0004] Chinese patent application CN101791278A discloses a cosmetic composition comprising an organosilicon compound, a hydrophobic film-forming polymer, a pigment, and a volatile carrier. This invention provides a cosmetic composition for treating keratin fibers, particularly human keratin fibers such as hair. However, silicone-based materials (such as silicone oil) are typically inert continuous phases or solvents, with limited capacity for physical adsorption and loading of active ingredients (especially water-soluble or macromolecular actives). Summary of the Invention

[0005] To address the problems mentioned in the background section, this invention provides a cosmetic formulation preparation process using silicon-based composite materials as a carrier.

[0006] To achieve the above objectives, the present invention adopts the following technical solution: A cosmetic formulation preparation process using silicon-based composite materials as a carrier includes the following steps: S1. Cyclopentadimethylsiloxane, phenyltrimethylsiloxane and nanospheres are mixed and homogeneously dispersed to obtain phase A; S2. Mix water, butanediol and sodium chloride, heat and stir to dissolve, and obtain phase B; S3. Add the W / Si type emulsifier to phase A, add phase B while stirring, maintain the temperature and perform high shear homogenization to form an emulsion; S4. Stir and cool the emulsion. After cooling, add xanthan gum solution to thicken it. Continue cooling and add fragrance. Homogenize, degas and fill the final product.

[0007] Further, in step S1, the mass ratio of cyclopentadimethylsiloxane, phenyltrimethylsiloxane to nanospheres is (8-12):(2-5):1, for example 8:2:1, 9:3:1, 10:4:1, 12:5:1; the rotation speed for homogeneous dispersion is 2500-3000 rpm, and the time is 15-20 min.

[0008] Further, in step S2, the mass ratio of water, butanediol, and sodium chloride is (82-96):(7-12):1, for example, 82:7:1, 85:8:1, 89:8:1, 90:9.5:1, 96:12:1; the target heating temperature is 75-80℃, the stirring speed is 100-300rpm, and the W / Si type emulsifier is polydimethylsiloxane (PEG-10), with an addition amount of 1.0-2.5% of the total mass of phase A and phase B.

[0009] Furthermore, in step S3, the stirring speed is 1400-1600 rpm, and the high-shear homogenization is carried out at 75-80℃ for 3-5 minutes.

[0010] Further, in step S4, when the emulsion is stirred and cooled to 45-50°C, a xanthan gum solution is added. The xanthan gum solution has a mass fraction of 0.5-2%, and its addition amount is 1-5% of the total mass of the emulsion. Then, when the temperature is further cooled to below 40°C, a fragrance is added. The xanthan gum solution is a homogeneous solution prepared by slowly adding xanthan gum powder to deionized water under stirring and allowing it to swell fully. The amount of fragrance added is 0.1-0.5% of the total mass of the emulsion.

[0011] Furthermore, in step S5, homogenization is carried out at a speed of 500-800 rpm for 2-3 min; degassing is carried out under a vacuum of -0.06 to -0.09 MPa for 5-15 min.

[0012] Furthermore, the nanospheres in step S1 are prepared by the following steps: A1. Add ferulic acid to a phosphate buffer solution with a pH of 8.5-9, then add horseradish peroxidase and hydrogen peroxide to carry out a polymerization reaction. After the reaction is completed, centrifuge the reaction solution, collect the solid precipitate, wash it several times with deionized water, and dry it to obtain polyferric acid solid powder. A2. Disperse the polyferric acid solid obtained in step A1 in an aqueous acetic acid solution to prepare solution A. Add carboxymethyl chitosan to the aqueous acetic acid solution to prepare solution B. Add zinc acetate to deionized water to prepare solution C. Add solution B dropwise to solution A, and then add solution C to carry out the cross-linking reaction. After the cross-linking reaction is completed, centrifuge the mixed system to collect the nanosphere precipitate, wash it with deionized water to remove unreacted substances, and dry it to obtain nanosphere powder.

[0013] Furthermore, in step A1, the amounts of materials used for each 0.1-0.2 mol / L phosphate buffer solution are: ferulic acid 1.94-3.88 g; horseradish peroxidase with an enzyme activity of 50-200 U; and 30% hydrogen peroxide aqueous solution 0.57-1.8 g.

[0014] Further, in step A2, solution A is a dispersion formed by dissolving solid polyferric acid in a 1-2% (v / v) aqueous acetic acid solution, with a concentration of 1.0-2.0 mg / mL; Solution B is a solution formed by dissolving carboxymethyl chitosan in a 1% (v / v) aqueous acetic acid solution, with a concentration of 0.5-1.5 mg / mL; Solution C is a solution formed by dissolving zinc acetate in deionized water, with a concentration of 1-5 mg / mL.

[0015] Furthermore, the polymerization reaction in step A1 is carried out at a temperature of 25-30°C for 2-7 hours.

[0016] Furthermore, in step A2, the dropping rate of solution B is 0.8-1.2 mL / min, the temperature of the cross-linking reaction is 30-35℃, the reaction time is 1-5 h, and the dropping and cross-linking reaction processes are carried out under magnetic stirring or mechanical stirring at a speed of 300-500 rpm.

[0017] The beneficial effects of this invention are: 1. The nanospheres prepared in this invention use enzymatically polymerized polyferric acid as a hydrophobic core and a gel network composed of carboxymethyl chitosan cross-linked with zinc ions as a hydrophilic shell, providing a suitable microenvironment for active substances of different polarities. The hydrophobic core helps to encapsulate lipid-soluble components, while the hydrophilic shell is beneficial for binding water-soluble substances, thereby potentially broadening the loading range of the formulation. Simultaneously, the ionically cross-linked shell can, to some extent, shield and protect the active ingredient in the core, reducing its impact from oxidation, light, and other factors during storage, thus helping to maintain the stability of the active ingredient.

[0018] 2. The ion-crosslinked gel network of the nanosphere shell has certain environmental response characteristics. When applied to the skin surface, external moisture and the weakly acidic skin microenvironment may cause the crosslinked network to swell, thereby regulating the release behavior of the internal active ingredients. This may change the release of active ingredients from simple diffusion to a more gradual and sustained process, helping to avoid rapid loss, thus potentially prolonging its duration of action and improving utilization efficiency.

[0019] 3. When using the product, the volatile silicone oil in the formula evaporates quickly, bringing a refreshing skin feel, while the biocompatible polymer components of the nanosphere shell may form a thin, breathable film on the skin surface, which helps to achieve the desired efficacy while also providing a good sensory experience. Attached Figure Description

[0020] Figure 1 This is a scanning electron microscope image of nanospheres prepared according to one embodiment of the present invention. Detailed Implementation

[0021] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0022] In this preparation example and examples, ferulic acid was purchased from Aladdin Reagent (Shanghai) Co., Ltd. (item number F110166, purity ≥98%); horseradish peroxidase (HRP) was purchased from Sigma-Aldrich (Shanghai) Trading Co., Ltd. (item number P8250, type II, enzyme activity approximately 250-330 U / mg, determined using pyrogallol as substrate); carboxymethyl chitosan was purchased from Shanghai Maclean Biochemical Technology Co., Ltd. (item number C817440, degree of substitution ≥80%, viscosity (1% aqueous solution, 25℃) 10-100 mPa·s); zinc acetate, glacial acetic acid, disodium hydrogen phosphate, sodium dihydrogen phosphate, and other chemical reagents were all analytical grade and purchased from Sinopharm Chemical Reagent Co., Ltd.

[0023] Preparation Example 1 Nanospheres are prepared by the following steps: A1. Add 3.0 g of ferulic acid to 1.0 L of 0.15 mol / L phosphate buffer with pH 8.8, stir to dissolve, then add horseradish peroxidase (enzyme activity added amount of 150 U) and 1.2 g of 30% hydrogen peroxide aqueous solution. Stir at 300 rpm for 5 h at 28 °C. After the reaction is completed, centrifuge the reaction solution at 8000 rpm for 15 min, collect the precipitate, wash three times with deionized water, freeze dry to obtain brown polyferulic acid solid powder. A2. Disperse polyferric acid solid powder in a 1.5% (v / v) aqueous acetic acid solution to prepare a dispersion with a concentration of 1.5 mg / mL, as solution A. Dissolve carboxymethyl chitosan in a 1% (v / v) aqueous acetic acid solution to prepare a solution with a concentration of 1.0 mg / mL, as solution B. Dissolve zinc acetate in deionized water to prepare a solution with a concentration of 3 mg / mL, as solution C. Under magnetic stirring at 400 rpm, slowly add 100 mL of solution B to 100 mL of solution A at a rate of 1.0 mL / min. After the addition is complete, continue stirring for 30 min. Then, add 30 mL of solution C while stirring, and continue stirring and reacting at 33 °C for 3 h. After the reaction is complete, centrifuge the mixture at 10000 rpm for 20 min, collect the precipitate, wash it three times with deionized water, and dry it to constant weight to obtain nanosphere powder.

[0024] Preparation Example 2 Nanospheres are prepared by the following steps: A1. In 1.0 L of 0.1 mol / L phosphate buffer with pH 9.0, add 1.94 g of ferulic acid and stir to dissolve. Then add horseradish peroxidase (enzyme activity added at 50 U) and 0.57 g of 30% hydrogen peroxide aqueous solution. Stir at 250 rpm for 7 h at 25 °C. After the reaction is completed, centrifuge the reaction solution at 8000 rpm for 15 min, collect the precipitate, wash it three times with deionized water, and dry it to constant weight to obtain polyferric acid solid powder. A2. Prepare solution A (polyferric ferulic acid solid in 2% acetic acid aqueous solution, concentration 1.0 mg / mL), solution B (carboxymethyl chitosan in 1% acetic acid aqueous solution, concentration 0.5 mg / mL), and solution C (zinc acetate aqueous solution, concentration 1 mg / mL). Under mechanical stirring at 500 rpm, solution B is added dropwise to an equal volume of solution A at a rate of 0.8 mL / min, followed by solution C. The mixture is reacted at 30 °C for 5 h. After the reaction is complete, the mixture is centrifuged at 10000 rpm for 20 min, the precipitate is collected, washed three times with deionized water, and dried to constant weight to obtain nanosphere powder.

[0025] Preparation Example 3 Nanospheres are prepared by the following steps: A1. Add 3.88 g of ferulic acid to 1.0 L of 0.2 mol / L phosphate buffer with pH 8.5, stir to dissolve, then add horseradish peroxidase (enzyme activity added amount of 200 U) and 1.8 g of 30% hydrogen peroxide aqueous solution. Stir at 350 rpm for 2 h at 30 °C. After the reaction is completed, centrifuge the reaction solution at 8000 rpm for 15 min, collect the precipitate, wash it three times with deionized water, and dry it to constant weight to obtain polyferric acid solid powder. A2. Prepare solutions A (polyferric ferulic acid solid in 1% acetic acid aqueous solution, concentration 2.0 mg / mL), B (carboxymethyl chitosan in 1% acetic acid aqueous solution, concentration 1.5 mg / mL), and C (zinc acetate aqueous solution, concentration 5 mg / mL). Under magnetic stirring at 300 rpm, add solution B dropwise to an equal volume of solution A at a rate of 1.2 mL / min, followed by solution C. React at 35 °C for 1 h. After the reaction is complete, centrifuge the mixture at 10000 rpm for 20 min, collect the precipitate, wash it three times with deionized water, and dry it to constant weight to obtain nanosphere powder.

[0026] Example 1 A cosmetic formulation preparation process using silicon-based composite materials as a carrier includes the following steps: S1. Weigh 10.0 g of cyclopentadimethylsiloxane, 4.0 g of phenyltrimethylsiloxane and 1.0 g of nanosphere powder prepared in Preparation Example 1, place them in a mixing container, and homogeneously disperse them at a speed of 2800 rpm for 18 min to make them evenly mixed, so as to obtain phase A. S2. Weigh 89.0g of deionized water, 8.0g of butanediol and 1.0g of sodium chloride, place them in another container, heat to 78℃, and stir at 200rpm until completely dissolved to obtain phase B; S3. Add 1.8g of polydimethylsiloxane to phase A. While stirring at 1500rpm, slowly add phase B, which is preheated to 78℃, to phase A. After the addition is complete, keep the temperature at 78℃ and homogenize at 15000rpm for 4min to obtain an emulsion. S4. Allow the emulsion to cool naturally under stirring. When the temperature drops to 48°C, add 6.7g of xanthan gum solution with a mass fraction of 1.5% and continue stirring until it thickens and becomes uniform. Then, continue cooling to 38°C and add 0.3g of flavoring. Stir until uniform and homogenize the final product at 600 rpm for 2.5 min. Then, degas under a vacuum of -0.08 MPa for 10 min and aseptically fill to obtain the finished product.

[0027] Example 2 A cosmetic formulation preparation process using silicon-based composite materials as a carrier includes the following steps: S1. Weigh 8.0 g of cyclopentadimethylsiloxane, 2.0 g of phenyltrimethylsiloxane and 1.0 g of nanosphere powder prepared in Preparation Example 2, and homogeneously disperse them at 2500 rpm for 20 min to obtain phase A; S2. Weigh 82.0g of deionized water, 7.0g of butanediol and 1.0g of sodium chloride, heat to 75℃ and stir at 100rpm to dissolve to obtain phase B; S3. Add 1.0 g of polydimethylsiloxane to phase A. While stirring at 1400 rpm, slowly add phase B, which has been preheated to 75°C. After adding the materials, perform high-shear homogenization (15000 rpm) at 75°C for 5 min to obtain an emulsion. S4. When the emulsion is cooled to 50°C, add 4.0 g of xanthan gum solution with a mass fraction of 0.5%. Continue cooling to 35°C, add 0.2 g of fragrance, stir evenly, homogenize the final product at 500 rpm for 3 min, degas at -0.06 MPa vacuum for 15 min, and aseptically fill to obtain the finished product.

[0028] Example 3 A cosmetic formulation preparation process using silicon-based composite materials as a carrier includes the following steps: S1. Weigh 12.0 g of cyclopentadimethylsiloxane, 5.0 g of phenyltrimethylsiloxane, and 1.0 g of the nanosphere powder known in Example 1, and homogeneously disperse them at 3000 rpm for 15 min to obtain phase A; S2. Weigh 96.0g of deionized water, 12.0g of butanediol and 1.0g of sodium chloride, heat to 80℃ and stir at 300rpm to dissolve to obtain phase B; S3. Add 2.7g of polydimethylsiloxane to phase A. While stirring at 1600rpm, add phase B, which is preheated to 80℃, quickly and smoothly. After adding the materials, perform high-shear homogenization (15000rpm) at 80℃ for 3min to obtain an emulsion. S4. When the emulsion is cooled to 45°C, add 11.6g of xanthan gum solution with a mass fraction of 2.0%. Continue cooling to 40°C, add 0.6g of fragrance, stir evenly, homogenize the final product at 800rpm for 2min, degas at -0.09MPa vacuum for 5min, and aseptically fill to obtain the finished product.

[0029] Example 4 This embodiment is basically the same as Embodiment 1, except that: The amount of cyclopentamethoxysiloxane in S1 is 9.0g, and the amount of phenyltrimethylsiloxane is 3.0g; The amount of deionized water used in S2 is 86.0g, and the amount of butanediol used is 9.0g; The amount of polydimethylsiloxane used in S3 is 1.5g; S4 contains 8.3g of xanthan gum solution with a mass fraction of 1.2% and 0.25g of fragrance.

[0030] Example 5 This embodiment is basically the same as Example 2, except that the nanosphere powder prepared in Preparation Example 1 is used. In S1, the amount of cyclopentamethoxysiloxane was 11.0 g, the amount of phenyltrimethylsiloxane was 4.5 g, the homogenization speed was 2900 rpm, and the time was 16 min. In S2, the amount of deionized water is 93.0g, the amount of butanediol is 10.0g, the heating temperature is 79℃, and the stirring speed is 250rpm; In S3, the amount of polydimethylsiloxane used is 2.2g, the stirring speed is 1550rpm, and the homogenization time is 3.5min; When S4 is cooled to 49°C, add 5.6g of xanthan gum solution with a mass fraction of 1.8% and when cooled to 39°C, add 0.4g of fragrance.

[0031] Example 6 This embodiment is basically the same as Example 3, except that the nanosphere powder prepared in Preparation Example 2 is used. In S1, the homogenization speed is 2750 rpm and the time is 19 min; The amount of butanediol used in S2 is 11.0g, the heating temperature is 76℃, and the stirring speed is 180rpm; In S3, the amount of polydimethylsiloxane used is 1.9g, the stirring speed is 1520rpm, and the homogenization time is 4.2min; When S4 is cooled to 46°C, add 10.0g of xanthan gum solution with a mass fraction of 0.8% and when cooled to 37°C, add 0.35g of fragrance.

[0032] Comparative Example 1 The difference between this comparative example and Example 1 is that the nanosphere powder obtained in Preparation Example 1 is not used in step S1, but instead an equal mass (1.0 g) of unmodified carboxymethyl chitosan powder. The other steps and parameters are the same as in Example 1.

[0033] Comparative Example 2 The difference between this comparative example and Example 1 is that in step S3, polydimethylsiloxane emulsifier is not used, but instead an equal mass (1.8 g) of conventional water-in-oil emulsifier, sorbitan monooleate (Span 80). The other steps and parameters are the same as in Example 1.

[0034] Comparative Example 3 The difference between this comparative example and Example 1 is that the addition of xanthan gum solution in step S4 is omitted, while the other steps and parameters are the same as in Example 1.

[0035] Comparative Example 4 This comparative example is essentially the same as Preparation Example 1 in preparing nanospheres, but in step A2, solution C (zinc acetate solution) is not added, i.e., no ionic crosslinking reaction is performed. The mixture of solutions A and B is directly centrifuged, washed, and dried to obtain uncrosslinked composite powder. The subsequent cosmetic formulation process is exactly the same as in Example 1, using this uncrosslinked composite powder to replace the original nanosphere powder.

[0036] Take 10 mL of each sample from Examples 1-6 and Comparative Examples 1-4 into centrifuge tubes and centrifuge at 3000 rpm for 30 min. Observe whether layering, precipitation, or demulsification occurs to evaluate centrifugation stability. Store each sample in a 40℃ incubator for 4 weeks. Take samples at weeks 0 and 4 to measure viscosity and calculate viscosity change rate. Viscosity change rate (%) = [(η t -η0) / η0] ×100%, where η0 is the initial viscosity, i.e., the sample viscosity measured before the start of the test (week 0), η t for t The viscosity at a specific time point, i.e., the viscosity of the sample measured at a specific time point after treatment under specific conditions (4 weeks after high-temperature storage), is used to evaluate high-temperature stability. The results are shown in Table 1: Table 1. Stability test results of the examples and comparative examples The same process as in Preparation Example 1 was used, but in step A1, 3.0 g of ferulic acid and 0.05 g of Nile red were pre-dissolved together in phosphate buffer before enzymatic polymerization. Subsequent steps remained unchanged. After centrifugation, washing, and drying, Nile red-loaded nanosphere powder was obtained, denoted as N1. The uncrosslinked loaded nanospheres prepared in Comparative Example 4 were taken, denoted as N2, i.e., without the addition of zinc acetate for crosslinking. Another control group was set up, containing only free Nile red, denoted as F1. A phosphate buffer (PBS) with a pH of 5.5 was prepared to simulate the weakly acidic environment of the skin surface, containing 0.5% (w / v) polysorbate 80 (Tween 80) to maintain the leak conditions as the release medium.

[0037] Weigh out equal amounts of N1, N2, and F1 (containing an equal amount of Nile Red). Disperse the first two separately and uniformly in cyclopentamethoxysilane to simulate its state in phase A of the formulation. Dissolve the free Nile Red directly in an equal amount of cyclopentamethoxysilane.

[0038] The above dispersions were quantitatively transferred to pretreated dialysis bags, and both ends were tied tightly. The dialysis bags were immersed in Erlenmeyer flasks containing 50 mL of release medium. The Erlenmeyer flasks were placed in a 37°C constant-temperature shaking incubator and slowly shaken at 100 rpm to simulate body temperature and slight friction. At predetermined time points (1, 2, 8, 24, and 72 h), 2 mL samples were taken from the release medium, and an equal volume of fresh release medium was immediately added. The fluorescence intensity of the samples was measured (excitation wavelength: 552 nm; emission wavelength: 636 nm). The cumulative release rate (Q,%) was calculated as follows: Among them, C n The concentration measured at the nth time point, V is the total volume of the released medium (50 mL), v i M0 represents the volume of each sample taken (2 mL), and M0 represents the total amount of Nile Red in the sample.

[0039] The results are shown in Table 2: Table 2. Results of Nile Red Simulated In Vitro Release Experiment As shown in Table 1, Examples 1-6 all exhibited good centrifugal stability, with no stratification or precipitation. This indicates that cosmetic formulations using silicon-based composite materials as a carrier and adding specific nanosphere powder can maintain a stable emulsion structure under centrifugation. This may be because the nanosphere powder plays a good dispersing and stabilizing role in the system, interacting with the silicon-based material and other components to form a stable system, preventing oil-water separation and particle aggregation.

[0040] Comparative Example 1 uses unmodified carboxymethyl chitosan powder instead of nanosphere powder. The carboxymethyl chitosan powder may not be able to interact effectively with other components in the system and cannot form a stable emulsion structure, resulting in oil-water separation and particle aggregation.

[0041] Comparative Example 2 replaced the polydimethylsiloxane emulsifier with the conventional water-in-oil emulsifier sorbitan monooleate (Span 80), demonstrating that different emulsifiers have a significant impact on the stability of the system. Polydimethylsiloxane may be more suitable for this system, as it can better stabilize the emulsion, while Span 80 cannot achieve the same effect, resulting in slight stratification and particle aggregation.

[0042] In Comparative Example 3, the lack of xanthan gum affected the viscosity and structural stability of the system, making it unable to effectively prevent oil-water separation and particle aggregation.

[0043] The uncrosslinked composite powder obtained in Comparative Example 4, without ionic crosslinking, exhibited a weaker ability to stabilize the emulsion compared to the crosslinked nanosphere powder. Ionic crosslinking may enhance the structural stability of the nanospheres and their interaction with other components in the system, thereby improving the stability of the emulsion.

[0044] Examples 1-6 show relatively small viscosity change rates, with both positive and negative directions, indicating that the viscosity of these samples did not change significantly after 4 weeks of high-temperature storage. This suggests that cosmetic formulations using silicon-based composite materials as a carrier and adding specific nanosphere powder exhibit good high-temperature stability. The nanosphere powder may help maintain the viscosity stability of the system. The differences in viscosity change rates among the different examples may be related to factors such as the preparation process of the nanosphere powder, the amount added, and the proportion of other components in the system. Comparative Examples 1-4 show larger viscosity change rates, all of which are negative, indicating that the viscosity of these samples decreased significantly after high-temperature storage.

[0045] Table 2 shows that the cumulative release rate of Nile Red in group N1 gradually increased over time, but the overall release rate was relatively slow, reaching 68.9% at 72 hours. This indicates that the ion-crosslinked nanosphere powder has a good encapsulation effect and can control the release rate of Nile Red. Ion crosslinking may make the nanosphere structure more compact, requiring a longer time for Nile Red to diffuse out of the nanospheres, thus achieving a sustained-release effect.

[0046] The cumulative release rate of Nile Red in group N2 was significantly higher than that in group N1, reaching 94.7% after 72 hours. This indicates that the uncrosslinked nanosphere powder has a poor encapsulation effect on Nile Red, allowing it to be released more quickly from the nanospheres. The relatively loose structure of the uncrosslinked nanospheres also facilitates the diffusion of Nile Red into the release medium.

[0047] The F1 group exhibited the highest cumulative release rate of Nile Red, reaching 75.3% at 1 hour and almost completely released at 72 hours. Free Nile Red was not confined by any encapsulation structure, thus enabling it to rapidly dissolve and diffuse into the release medium.

[0048] In summary, the cosmetic formulation prepared by this invention, which constructs a composite carrier with cross-linked nanospheres as the core, silicon-based materials as the continuous phase, and supplemented by a specific emulsification and thickening system, exhibits significant advantages in terms of physical stability and controlled release performance of active ingredients.

[0049] In the description of this specification, the reference to terms such as "embodiment," "various embodiments," etc., indicates that a specific feature, structure, material, or characteristic described in connection with that embodiment or preparation example is included in at least one embodiment of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments.

[0050] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A cosmetic formulation preparation process using silicon-based composite materials as a carrier, characterized in that, Includes the following steps: S1. Cyclopentadimethylsiloxane, phenyltrimethylsiloxane and nanospheres are mixed and homogeneously dispersed to obtain phase A; S2. Mix water, butanediol and sodium chloride, heat and stir to dissolve, and obtain phase B; S3. Add the W / Si type emulsifier to phase A, add phase B while stirring, maintain the temperature and perform high shear homogenization to form an emulsion; S4. Stir and cool the emulsion. After cooling, add xanthan gum solution to thicken it. Continue cooling and add flavoring. Homogenize, degas and fill to obtain the finished product.

2. The preparation process according to claim 1, characterized in that, In step S1, the mass ratio of cyclopentadimethylsiloxane, phenyltrimethylsiloxane and nanospheres is (8-12):(2-5):1; the rotation speed for homogeneous dispersion is 2500-3000 rpm and the time is 15-20 min.

3. The preparation process according to claim 1, characterized in that, In step S2, the mass ratio of water, butanediol, and sodium chloride is (82-96):(7-12):1; the target heating temperature is 75-80℃, and the stirring speed is 100-300rpm.

4. The preparation process according to claim 1, characterized in that, In step S3, the stirring speed is 1400-1600 rpm, and the high-shear homogenization is carried out at 75-80℃ for 3-5 minutes.

5. The preparation process according to claim 1, characterized in that, In step S4, when the emulsion is stirred and cooled to 45-50°C, xanthan gum solution is added. The mass fraction of xanthan gum solution is 0.5-2%, and the amount added is 1-5% of the total mass of the emulsion. Then, when the emulsion is cooled to below 40°C, flavoring is added.

6. The preparation process according to claim 1, characterized in that, The nanospheres in step S1 are prepared by the following steps: A1. Add ferulic acid to a phosphate buffer solution with a pH of 8.5-9, then add horseradish peroxidase and hydrogen peroxide to carry out a polymerization reaction to obtain polyferric acid solid. A2. Disperse the polyferric acid solid obtained in step A1 in an aqueous acetic acid solution to prepare solution A. Add carboxymethyl chitosan to the aqueous acetic acid solution to prepare solution B. Add zinc acetate to deionized water to prepare solution C. Add solution B dropwise to solution A, and then add solution C to carry out the cross-linking reaction. After drying, nanospheres are obtained.

7. The preparation process according to claim 6, characterized in that, In step A1, the amounts of materials used for each 0.1-0.2 mol / L phosphate buffer solution are: ferulic acid 1.94-3.88 g; horseradish peroxidase with an enzyme activity of 50-200 U; and 30% hydrogen peroxide aqueous solution 0.57-1.8 g.

8. The preparation process according to claim 6, characterized in that, In step A2, solution A is a dispersion formed by dissolving solid polyferric acid in a 1-2% (v / v) aqueous acetic acid solution, with a concentration of 1.0-2.0 mg / mL. Solution B is a solution formed by dissolving carboxymethyl chitosan in a 1% (v / v) aqueous acetic acid solution, with a concentration of 0.5-1.5 mg / mL; Solution C is a solution formed by dissolving zinc acetate in deionized water, with a concentration of 1-5 mg / mL.

9. The preparation process according to claim 6, characterized in that, The polymerization reaction in step A1 is carried out at a temperature of 25-30℃ for 2-7 hours.

10. The preparation process according to claim 6, characterized in that, In step A2, the dropping rate of solution B is 0.8-1.2 mL / min, the temperature of the cross-linking reaction is 30-35℃, and the reaction time is 1-5 h.

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