A synergistic oil control composition based on active ingredients and a method for its preparation

Abstract

The present application relates to a kind of synergistic oil control composition based on active ingredient and its preparation method, the synergistic oil control composition based on active ingredient, including the following mass fraction of ingredients: PCA zinc 0.1-1 part, octanoyl glycine 0.1-1 part, rosemary extract 0.1-2 parts, hydrolyzed red algae extract 0.1-2 parts, olive leaf extract 0.1-2 parts, Ulmus pumila L. extract 0.1-2 parts, white willow bark extract 0.1-2 parts, modified silicon dioxide 0.5-3 parts, betaine 0.1-1 part, carboxyl modified chitosan hydrogel 10-30 parts, skin conditioner 0.5-3 parts, auxiliary agent 4-12 parts;Wherein, the modified silicon dioxide is that hydroxylated silicon dioxide, kh570 is blended and then added to n-hexyl acrylate, dimethylaminoethyl methacrylate is blended and reacted to obtain.The present application has good oil control effect and slow-release performance, and has good application prospect.

Description

Technical Field

[0001] This invention relates to the field of skincare technology, and in particular to a synergistic oil-control composition based on active ingredients and its preparation method. Background Technology

[0002] Oil-controlling compositions are products designed for oily, combination, and acne-prone skin, covering categories such as cleansers, toners, serums, gels, lotions, and masks. Their core function is to absorb surface oil and regulate sebum secretion.

[0003] The working principle of the oil-control composition includes: inhibiting sebum secretion, reducing triglyceride synthesis, and reducing oil production from the source; physically absorbing oil, quickly absorbing free oil on the skin surface after application, blurring enlarged pores, and immediately eliminating shine; unclogging pores, dissolving sebum plugs, improving blackheads and closed comedones, and preventing acne caused by oil blockage.

[0004] Common types of oil-control products on the market include: oil-control toners, which are high-water-phase formulas containing polyols and plant extracts for oil control, are refreshing and lightweight, and suitable for daily secondary cleansing; oil-control serums, which contain high concentrations of active ingredients such as zinc PCA and niacinamide, and are highly targeted; oil-control hydrogels, which use hydrogels such as polysaccharides and carbomer as carriers to slowly release oil-control ingredients while suspending powder, providing both immediate matte finish and long-lasting oil control, leaving skin feeling moisturized and non-comedogenic, and suitable for oily and sensitive skin; and oil-control lotions, which contain a small amount of light oils and oil-control powders, suitable for very dry and oily skin, etc.

[0005] However, currently, common oil-control compositions still have some problems, including: insufficient oil control effect, rapid facial oiliness and shine, obvious oiliness in the T-zone, visual greasiness, pores filled with oil, appearing large, dull and yellow, skin tone turning yellow and dirty after oil oxidation, and foundation easily becoming patchy, fading, and clogging pores; insufficient slow-release effect, significantly shortening the oil control time, severe oil rebound, rapid one-time loss of active ingredients, unable to continuously act on sebaceous glands, providing a brief refreshing feeling after application, but sebum secretion increases shortly afterward, failing to achieve the core demand for long-lasting oil control; and insufficient stability, causing obvious appearance defects, significantly reduced efficacy, failure of the core oil control selling point, and direct abandonment by consumers.

[0006] In conclusion, it is necessary to develop a new technical solution to address the shortcomings of existing technologies. Summary of the Invention

[0007] This invention provides a synergistic oil-controlling composition based on active ingredients and its preparation method. The modified silica of the synergistic oil-controlling composition based on active ingredients introduces active groups, which work synergistically with the other components to improve the various properties of the composition.

[0008] The purpose of this invention is to provide a synergistic oil-controlling composition based on active ingredients, wherein the synergistic oil-controlling composition based on active ingredients comprises the following components in parts by weight: PCA zinc 0.1-1 part Capryloyl glycine 0.1-1 part Rosemary extract 0.1-2 parts 0.1-2 parts of hydrolyzed red algae extract Olive leaf extract 0.1-2 parts Spiraea elm extract 0.1-2 parts 0.1-2 parts of white willow bark extract 0.5-3 parts modified silica Betaine 0.1-1 part 10-30 parts of carboxyl-modified chitosan hydrogel Skin conditioning agent 0.5-3 parts 4-12 parts of auxiliary agent; The modified silica is obtained by blending hydroxylated silica and KH570, followed by blending n-hexyl acrylate and dimethylaminoethyl methacrylate.

[0009] Furthermore, the skin conditioning agent is selected from one or more of allantoin, maltitol, nicotinamide, amino acids, dipotassium glycyrrhizate, sodium hyaluronate, β-glucan, hydrolyzed collagen, panthenol, and polyglutamic acid.

[0010] Furthermore, the additive is selected from one or more of the following: humectants, thickeners, preservatives, chelating agents, and multifunctional additives.

[0011] Another object of the present invention is to provide a method for preparing the synergistic oil-controlling composition based on the active ingredient, the method comprising the following steps: S1. Hydroxylated silicon dioxide is obtained by hydroxylating silicon dioxide; S2. The hydroxylated silica and KH570 are mixed and heated and stirred to react, yielding an intermediate product. S3. The intermediate product, n-hexyl acrylate, dimethylaminoethyl methacrylate, and initiator are mixed and heated and stirred to react, thereby obtaining modified silica. S4. Mix the components other than the skin conditioning agent and the auxiliary agent evenly, remove the air bubbles under negative pressure, add the remaining components, mix evenly, remove the air bubbles under negative pressure, and obtain the synergistic oil-control composition based on active ingredients.

[0012] Furthermore, in step S1, the hydroxylation temperature is 70-90°C.

[0013] Further, in step S2, the mass ratio of the hydroxylated silicon dioxide to KH570 is (1-2):(0.5-3).

[0014] Furthermore, in step S2, the heating temperature is 50-80℃.

[0015] Further, in step S3, the mass ratio of the intermediate product, n-hexyl acrylate, and dimethylaminoethyl methacrylate is (1-3):(0.4-1.5):(0.4-1.5).

[0016] Furthermore, in step S3, the heating temperature is 60-90℃.

[0017] The present invention has the following beneficial effects: This invention provides a synergistic oil-controlling composition based on active ingredients and its preparation method. The modified silica is obtained by first blending hydroxylated silica and KH570 to produce double bonds on the surface of silica, and then adding n-hexyl acrylate and dimethylaminoethyl methacrylate for blending and polymerization.

[0018] The modified silica of this invention incorporates hexyl and amino groups. Hexyl groups are lipophilic, allowing them to adsorb oil and reduce facial oil adhesion, thus controlling oil production. Amino groups are hydrophilic, improving the compatibility of the modified silica with other components, ensuring uniform distribution, reducing agglomeration, and preventing performance degradation caused by agglomeration. Silica itself has a porous structure, which also adsorbs facial oil, further contributing to oil control. Furthermore, the carboxyl-modified chitosan hydrogel contains dense three-dimensional pores, encapsulating the components and preventing instantaneous dissolution upon skin contact. Instead, it slowly penetrates and releases the components. Moreover, the carboxyl groups in the carboxyl-modified chitosan hydrogel can form electrostatic adsorption with components containing cationic or positively charged groups (such as zinc PCA and betaine), further reducing the release rate and prolonging the duration of action.

[0019] The protonated amino groups on the surface of modified silica are positively charged, forming weak electrostatic associations with the negatively charged carboxyl groups on the carboxyl-modified chitosan hydrogel. This allows the modified silica to be uniformly anchored in the three-dimensional network of the carboxyl-modified chitosan hydrogel, preventing the modified silica from settling and agglomerating, and improving the stability of the formulation during storage.

[0020] Modified silica is responsible for "rapid oil absorption," instantly eliminating shine by quickly absorbing excess oil from the skin's surface. Meanwhile, carboxyl-modified chitosan hydrogel is responsible for "oil locking," forming a breathable, continuous hydrating film on the skin's surface to fix the absorbed oil and prevent its diffusion and shine. The two work synergistically to solve both immediate shine and reduce rebound oil production. The synergistic effect of each component enhances the overall performance of the composition. Detailed Implementation

[0021] To more clearly illustrate the technical solution of the present invention, the following embodiments are provided. Unless otherwise stated, the raw materials, reactions, and post-processing methods appearing in the embodiments are all commercially available raw materials and technical methods well known to those skilled in the art.

[0022] The terms "preferred," "more preferably," and "more suitable" used in this invention refer to embodiments of the invention that provide certain beneficial effects under certain circumstances. However, other embodiments may also be preferred under the same or other circumstances. Furthermore, the description of one or more preferred embodiments does not imply that other embodiments are unavailable, nor is it intended to exclude other embodiments from the scope of this invention.

[0023] It should be understood that, except in any operational instance or otherwise indicated, the amounts or all figures representing ingredients used, for example, in the specification and claims, should be understood to be modified by the term "about" in all cases. Therefore, unless otherwise stated, the numerical parameters set forth in the following specification and appended claims are approximate values ​​varying according to the desired performance to be obtained according to the invention.

[0024] The embodiments of the present invention use the following raw materials: Zinc PCA: Purchased from Wuhan Huaxiang Kejie Biotechnology Co., Ltd.

[0025] Rosemary extract: purchased from Guangzhou Puyifeng Biotechnology Co., Ltd.

[0026] Hydrolyzed red algae extract: purchased from Jiangsu Jufeng Chemical Technology Co., Ltd.

[0027] Olive leaf extract: purchased from Xi'an Tianfeng Biotechnology Co., Ltd.

[0028] Spiraea japonica extract: purchased from Xi'an Shilin Biotechnology Co., Ltd.

[0029] White willow bark extract: purchased from Xi'an Tianfeng Biotechnology Co., Ltd.

[0030] Silica: Particle size 30-80nm.

[0031] Carboxyl-modified chitosan hydrogel: Model COOH-Chitosan, purchased from Shenzhen Meiluo Technology Co., Ltd.

[0032] Chitosan hydrogel: purchased from Shenzhen Meiluo Technology Co., Ltd.

[0033] Skin conditioning agent: β-glucan (purchased from Hubei Xinyuhong Biomedical Technology Co., Ltd.) and niacinamide are mixed in a 1:1 mass ratio.

[0034] Additives: Moisturizer (glycerin), moisturizer (propylene glycol), and thickener (sodium polyacrylate, purchased from Shandong Fangchang Biotechnology Co., Ltd.) are mixed in a mass ratio of 4:4:1.

[0035] The components and mass fractions of the active ingredient-based synergistic oil-controlling compositions in Examples 1-3 are shown in Table 1.

[0036] Table 1. Components and mass fractions of the synergistic oil-controlling compositions based on active ingredients in Examples 1-3 Examples 1-3 A method for preparing a synergistic oil-controlling composition based on active ingredients, the method comprising the following steps: S1. Immerse silica in a 2 mol / L hydrochloric acid solution, heat to 75°C and stir for 2 hours, filter, wash and dry to obtain hydroxylated silica; S2. Using ethanol and water in a volume ratio of 1:1 as solvents, the hydroxylated silica and KH570 were mixed in a mass ratio of 1:0.5, heated to 50°C and stirred for 24 hours, filtered, washed and dried to obtain the intermediate product. S3. Under a nitrogen atmosphere, using dimethyl sulfoxide as a solvent, the intermediate product, n-hexyl acrylate, dimethylaminoethyl methacrylate, and initiator azobisisobutyronitrile are mixed in a mass ratio of 2:0.5:0.5:0.02, heated to 80°C and stirred for 10 hours. The mixture is then filtered, washed, and dried to obtain modified silica. S4. Mix the components other than the skin conditioning agent and the auxiliary agent evenly, remove the air bubbles under negative pressure, add the remaining components, mix evenly, remove the air bubbles under negative pressure, and obtain the synergistic oil-control composition based on active ingredients.

[0037] Comparative Example 1 The difference between Comparative Example 1 and Example 1 is that the mass of n-hexyl acrylate in step S3 is replaced with methyl methacrylate, while the remaining components and preparation methods are the same as in Example 1.

[0038] Comparative Example 2 The difference between Comparative Example 2 and Example 1 is that the same mass of dimethylaminoethyl methacrylate in step S3 is replaced with methyl methacrylate, while the remaining components and preparation methods are the same as in Example 1.

[0039] Comparative Example 3 The difference between Comparative Example 3 and Example 1 is that the carboxyl-modified chitosan hydrogel was replaced with chitosan hydrogel by the same mass, while the other components and preparation methods were the same as in Example 1.

[0040] Test Example 1 The oil control performance of the compositions of Examples 1-3 and Comparative Examples 1-3 was tested.

[0041] Test method: Sixty volunteers aged 25-40 with oily skin were selected and divided into 6 groups of 10 each. Each group used the compositions prepared in Examples 1-3 and Comparative Examples 1-3 respectively. After cleansing, each volunteer applied 0.5g of the composition evenly to their face. Then, the initial sebum secretion and the sebum secretion after 5h, 8h and 12h were measured using a skin tester. The average value of the results for each group was taken.

[0042] The test results are shown in Table 2.

[0043] Table 2 Test Results As can be seen from Table 2, the results of Examples 1-3 are better than those of Comparative Examples 1-3. This is because the modified silica of Comparative Example 1 did not introduce hexyl groups, which reduced its oil absorption capacity and thus reduced the oil control performance of the composition; the modified silica of Comparative Example 2 did not introduce amino groups, which reduced the compatibility of the components and thus reduced the oil control effect of the composition; the chitosan hydrogel of Comparative Example 3 did not introduce carboxyl groups, which weakened the sustained-release effect of the composition and accelerated the release of the components, resulting in a shorter action time of the composition and thus reduced the oil control effect of the composition.

[0044] Test Example 2 Stability tests were conducted on the compositions of Examples 1-3 and Comparative Examples 1-3.

[0045] Test method: Low-temperature stability test: The compositions of Examples 1-3 and Comparative Examples 1-3 were bottled and sealed, and placed in an environment at 15°C for 24 hours of freeze-thaw cycle. Then they were taken out and brought back to room temperature, and the phenomenon was observed. This freeze-thaw cycle was repeated five times. If there is no obvious layering or precipitation in the composition, it is judged to be qualified for low-temperature stability.

[0046] High-temperature stability test: The compositions of Examples 1-3 and Comparative Examples 1-3 were bottled and sealed, and placed in an environment of 40°C for 24 hours. Then they were taken out and allowed to return to room temperature. The phenomenon was observed. This high-temperature cycle was repeated five times. If the composition did not show obvious discoloration, layering or precipitation, it was judged to be qualified for high-temperature stability.

[0047] The test results are shown in Table 3.

[0048] Table 3 Stability Test Results As can be seen from Table 3, the results of Examples 1-3 are better than those of Comparative Examples 2-3. This is because the modified silica of Comparative Example 2 did not introduce amino groups, which reduced the compatibility of the components, making them prone to aggregation and uneven dispersion, resulting in a decrease in the stability of the composition. In contrast, the chitosan hydrogel of Comparative Example 3 did not introduce carboxyl groups, which led to a decrease in stability.

[0049] 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 invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, it is intended that all variations falling within the meaning and scope of equivalents of the claims be included within the present invention.

[0050] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A synergistic oil-controlling composition based on active ingredients, characterized in that, The synergistic oil-controlling composition based on active ingredients comprises the following components in parts by weight: PCA zinc 0.1-1 part Capryloyl glycine 0.1-1 part Rosemary extract 0.1-2 parts 0.1-2 parts of hydrolyzed red algae extract Olive leaf extract 0.1-2 parts Spiraea elm extract 0.1-2 parts 0.1-2 parts of white willow bark extract 0.5-3 parts modified silica Betaine 0.1-1 part 10-30 parts of carboxyl-modified chitosan hydrogel Skin conditioning agent 0.5-3 parts 4-12 parts of auxiliary agent; The modified silica is obtained by blending hydroxylated silica and KH570, followed by blending n-hexyl acrylate and dimethylaminoethyl methacrylate.

2. The synergistic oil-controlling composition based on active ingredients according to claim 1, characterized in that, The skin conditioning agent is selected from one or more of allantoin, maltitol, nicotinamide, amino acids, dipotassium glycyrrhizate, sodium hyaluronate, β-glucan, hydrolyzed collagen, panthenol, and polyglutamic acid.

3. The synergistic oil-controlling composition based on active ingredients according to claim 1, characterized in that, The additives are selected from one or more of the following: humectants, thickeners, preservatives, chelating agents, and multifunctional additives.

4. The method for preparing the synergistic oil-controlling composition based on active ingredients according to any one of claims 1-3, characterized in that, The preparation method of the synergistic oil-controlling composition based on active ingredients includes the following steps: S1. Hydroxylated silicon dioxide is obtained by hydroxylating silicon dioxide; S2. The hydroxylated silica and KH570 are mixed and heated and stirred to react, and an intermediate product is obtained. S3. The intermediate product, n-hexyl acrylate, dimethylaminoethyl methacrylate, and initiator are mixed and heated and stirred to react, thereby obtaining modified silica. S4. Mix the components other than the skin conditioning agent and the auxiliary agent evenly, remove the air bubbles under negative pressure, add the remaining components, mix evenly, remove the air bubbles under negative pressure, and obtain the synergistic oil-control composition based on active ingredients.

5. The method for preparing the synergistic oil-controlling composition based on active ingredients according to claim 4, characterized in that, In step S1, the hydroxylation temperature is 70-90°C.

6. The method for preparing the synergistic oil-controlling composition based on active ingredients according to claim 4, characterized in that, In step S2, the mass ratio of hydroxylated silicon dioxide to KH570 is (1-2):(0.5-3).

7. The method for preparing the synergistic oil-controlling composition based on active ingredients according to claim 4, characterized in that, In step S2, the heating temperature is 50-80℃.

8. The method for preparing the synergistic oil-controlling composition based on active ingredients according to claim 4, characterized in that, In step S3, the mass ratio of the intermediate product, n-hexyl acrylate, and dimethylaminoethyl methacrylate is (1-3):(0.4-1.5):(0.4-1.5).

9. The method for preparing the synergistic oil-controlling composition based on active ingredients according to claim 4, characterized in that, In step S3, the heating temperature is 60-90℃.

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