Silk fibroin-containing essence mask and preparation method thereof

Abstract

The application discloses a silk fibroin-containing essence mask and a preparation method thereof, and belongs to the technical field of skin care products.The essence mask contains glycerol, 1,2-pentanediol, 1,2-hexanediol, p-hydroxyacetophenone, silk fibroin, tetrahydro methyl pyrimidine carboxylic acid, hydroxyethyl cellulose and water according to percentage by weight.The application effectively improves the moisturizing and repairing performance of the mask through synergistic effect of specific components, and solves the problems of easy inactivation and poor stability of silk fibroin in the prior art by synergistically protecting the activity of silk fibroin with p-hydroxyacetophenone.The preparation method is simple in process and is low-temperature operation throughout, and can maximize the efficacy of active ingredients.The obtained mask is refreshing, mild and non-irritating, is suitable for sensitive skin people, and has a good application prospect.

Description

Technical Field

[0001] This invention belongs to the field of cosmetic technology, and in particular relates to an essence mask containing silk fibroin and its preparation method. Background Technology

[0002] Facial masks are among the most widely used skincare products in daily skincare routines. They work by concentrating essential ingredients onto the facial skin to achieve various skincare benefits such as moisturizing, repairing, whitening, and anti-aging. Among these, moisturizing and repairing are the most fundamental and core functions of facial masks, and also one of the key demands of consumers when purchasing facial mask products.

[0003] Silk fibroin (also known as silk heart protein) is a natural high-molecular-weight fibrous protein extracted from silkworm silk. It possesses excellent biocompatibility, transdermal absorption, and biodegradability, along with superior moisturizing, repairing, and antioxidant effects. It can promote skin cell proliferation and repair, and improve skin barrier function, thus being widely used in skincare products. However, existing silk fibroin-containing mask formulations still have several drawbacks: First, silk fibroin is prone to denaturation and degradation in aqueous systems, resulting in low retention of active ingredients and poor long-term product stability; second, the formulation system lacks sufficient moisturizing ability, failing to achieve long-lasting hydration, leading to dryness and tightness after application; third, irritating preservatives are often added to enhance preservative effects, easily causing skin sensitivity, redness, and other adverse reactions, limiting its suitability for certain groups; and fourth, the transdermal absorption rate of active ingredients is low, failing to fully utilize the repairing effects of silk fibroin.

[0004] Therefore, there is an urgent need to develop an essence mask product that combines high moisturizing properties, high activity stability, low irritation, and can fully exert the repairing effects of silk fibroin. Summary of the Invention

[0005] To address the aforementioned technical problems, this invention proposes an essence mask containing silk fibroin and its preparation method. This mask has excellent immediate and long-lasting moisturizing effects, high retention rate of silk fibroin activity, good system stability, and is non-irritating. It can effectively repair the skin barrier and is suitable for people with all skin types.

[0006] To achieve the above objectives, the present invention provides the following technical solution: A silk fibroin-containing essence mask, excluding the mask sheet, comprises the following components by weight percentage: Glycerin: 1%~10%, 1,2-pentanediol: 0.05%~5%, 1,2-hexanediol: 0.05%~3%, p-hydroxyacetophenone: 0.01%~3%, silk fibroin: 0.01%~3%, tetrahydromethylpyrimidine carboxylic acid: 0.01%~3%, hydroxyethyl cellulose: 0.01%~3%, balance: water.

[0007] This invention's formula uses water as a solvent to construct the basic system, supplemented with glycerin, 1,2-pentanediol, and 1,2-hexanediol as polyol moisturizers, providing deep hydration while also offering preservative and enhanced efficacy. In this system, silk fibroin acts as the core active ingredient, playing a repairing role, while p-hydroxyacetophenone not only acts as an antioxidant but also provides crucial synergistic protection with silk fibroin, effectively preventing the degradation and inactivation of active ingredients. Simultaneously, the formula introduces tetrahydromethylpyrimidine carboxylic acid to synergize with silk fibroin, further enhancing the skin's moisturizing and barrier repair capabilities; hydroxyethyl cellulose acts as a thickener to adjust the system's viscosity, ensuring that each active ingredient is evenly dispersed and stably adheres to the mask sheet, ultimately forming a gentle, stable, and highly effective essence mask system.

[0008] Optionally, the silk fibroin-containing essence mask comprises the following components by weight percentage: Glycerin: 3%~8%, 1,2-pentanediol: 0.1%~3%, 1,2-hexanediol: 0.1%~2%, p-hydroxyacetophenone: 0.05%~2%, silk fibroin: 0.1%~2%, tetrahydromethylpyrimidine carboxylic acid: 0.1%~2%, hydroxyethyl cellulose: 0.1%~2%, balance: water.

[0009] Furthermore, by weight percentage, the essence mask containing silk fibroin comprises the following components: Glycerin: 5%, 1,2-pentanediol: 1%, 1,2-hexanediol: 0.5%, p-hydroxyacetophenone: 0.5%, silk fibroin: 1%, tetrahydromethylpyrimidine carboxylic acid: 1%, hydroxyethyl cellulose: 0.5%, water: 90.5%.

[0010] Furthermore, by weight percentage, the essence mask containing silk fibroin comprises the following components: Glycerin: 3%, 1,2-pentanediol: 0.1%, 1,2-hexanediol: 0.1%, p-hydroxyacetophenone: 0.05%, silk fibroin: 0.1%, tetrahydromethylpyrimidine carboxylic acid: 0.1%, hydroxyethyl cellulose: 0.1%, water: 96.55%.

[0011] Furthermore, by weight percentage, the essence mask containing silk fibroin comprises the following components: Glycerin: 8%, 1,2-pentanediol: 3%, 1,2-hexanediol: 2%, p-hydroxyacetophenone: 2%, silk fibroin: 2%, tetrahydromethylpyrimidine carboxylic acid: 2%, hydroxyethyl cellulose: 2%, water: 79%.

[0012] A method for preparing the above-mentioned silk fibroin-containing essence mask includes the following steps: (1) Aqueous premixing: Water, glycerol, 1,2-pentanediol, 1,2-hexanediol and p-hydroxyacetophenone were added to the reaction vessel according to the weight percentage, stirred evenly, and then heated to obtain an aqueous premix; (2) Preparation of thickening system: Hydroxyethyl cellulose is slowly added to the above aqueous premixed solution, and stirred at a constant temperature until the hydroxyethyl cellulose is completely dissolved to obtain a uniform thickening system; (3) Addition of active ingredients: Reduce the temperature of the reaction vessel to 25℃~30℃, add the formula amount of silk fibroin and tetrahydromethylpyrimidine carboxylic acid, stir evenly, keep warm and stir until all components are completely dissolved and dispersed; (4) Homogenization and sterilization: The mixture obtained in step (3) is homogenized and then filtered and sterilized to obtain the essence mask stock solution; (5) Mask preparation: Inject the sterilized essence mask stock solution into a packaging container containing the mask sheet, seal the packaging, and the finished essence mask is obtained.

[0013] The preparation method of this invention first involves an aqueous premixing step, where heating promotes the complete dissolution and uniform dispersion of glycerol, 1,2-pentanediol, 1,2-hexanediol, and p-hydroxyacetophenone in water, constructing a stable basic liquid phase system. Subsequently, hydroxyethyl cellulose is slowly added to this premix under incubation conditions, allowing it to completely dissolve and form a homogeneous thickening system, providing a suitable viscosity environment for the subsequent suspension and stability of the active ingredients. After the system temperature drops to a mild range of 25℃~30℃, heat-sensitive silk fibroin and tetrahydromethylpyrimidine carboxylic acid are added. This low-temperature operation effectively avoids the denaturation and inactivation of the core active ingredients while ensuring the uniform dispersion of each component in the thickening system. Next, homogenization further refines the system, improving the fineness and stability of the essence. Finally, it is sterilized by filtration through a microporous membrane, ensuring product sterility while maximizing the retention of active ingredients. Finally, the high-quality essence mask stock solution is injected into a container containing the mask sheet and sealed, thus completing the preparation of the finished product. The entire process is interconnected, taking into account the safety, stability and efficacy of the product.

[0014] Optionally, in step (1), the heating conditions are: heating to 40℃~50℃ and stirring for 10min~15min.

[0015] Optionally, in step (2), the time for heat preservation and stirring (corresponding to 40℃~50℃ in step (1)) is 20min~30min.

[0016] Optionally, in step (3), the time for heat preservation and stirring is 15 min to 20 min.

[0017] Optionally, in step (4), the homogenization speed of the homogenization process is 3000 r / min to 5000 r / min, and the homogenization time is 5 min to 10 min.

[0018] Optionally, in step (4), the filtration sterilization is performed using a 0.22 μm microporous membrane.

[0019] Optionally, in step (5), the mask fabric is one of Tencel mask fabric, silk mask fabric or cotton velvet mask fabric.

[0020] Compared with the prior art, the present invention has the following advantages and technical effects: 1. In the essence mask formula system of the present invention, glycerin is compounded with 1,2-pentanediol and 1,2-hexanediol to form a polyol moisturizing system, which can not only achieve excellent immediate moisturizing effect, but also lock in skin moisture for a long time, avoiding dryness and tightness of the skin after applying the mask. At the same time, the polyol system can synergistically enhance the preservative ability of the system, eliminating the need to add traditional irritating preservatives, reducing the irritation of the product, and making it suitable for people with sensitive skin.

[0021] 2. In this invention, the combination of p-hydroxyacetophenone and polyol not only enhances the preservative stability of the system, but also synergistically protects the activity of silk fibroin, preventing denaturation and degradation of silk fibroin during storage, thus significantly improving the storage stability of the product. After 12 months of storage at room temperature, the silk fibroin activity retention rate can reach up to 95% or more.

[0022] 3. In this invention, tetrahydromethylpyrimidine carboxylic acid (ectoin) is combined with silk fibroin to achieve synergistic effects. Tetrahydromethylpyrimidine carboxylic acid can enhance the skin barrier function, promote the transdermal absorption of silk fibroin, and enhance the repair and antioxidant effects of silk fibroin. At the same time, it can further enhance the moisturizing ability of the system, achieving a skin care effect of 1+1>2.

[0023] 4. The preparation method of the present invention is simple, mild, and uses low temperature treatment throughout, which avoids the destruction of silk fibroin activity by high temperature and preserves the activity of the active ingredients to the greatest extent. At the same time, the homogenization and sterilization treatment ensures the hygiene and safety of the product, making it suitable for large-scale industrial production. Detailed Implementation

[0024] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as a limitation of the present invention, but rather as a more detailed description of certain aspects, features, and embodiments of the present invention.

[0025] It should be understood that the terminology used in this invention is merely for describing particular embodiments and is not intended to limit the invention. Furthermore, with respect to numerical ranges in this invention, it should be understood that each intermediate value between the upper and lower limits of the range is also specifically disclosed. Every smaller range between any stated value or intermediate value within a stated range, and any other stated value or intermediate value within said range, is also included in this invention. The upper and lower limits of these smaller ranges may be independently included or excluded from the range.

[0026] Unless otherwise stated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. While only preferred methods and materials have been described herein, any methods and materials similar or equivalent to those described herein may be used in the implementation or testing of this invention. All references to this specification are incorporated by way of citation to disclose and describe methods and / or materials associated with those references. In the event of any conflict with any incorporated reference, the content of this specification shall prevail.

[0027] Various modifications and variations can be made to the specific embodiments described in this specification without departing from the scope or spirit of the invention, as will be apparent to those skilled in the art. Other embodiments derived from this specification will also be readily apparent to those skilled in the art. This specification and embodiments are merely exemplary.

[0028] The terms “include,” “including,” “have,” “contain,” etc., used in this article are all open-ended terms, meaning that they include but are not limited to.

[0029] This invention discloses an essence mask containing silk fibroin, which comprises the following components by weight percentage: Glycerin: 1%~10%, 1,2-pentanediol: 0.05%~5%, 1,2-hexanediol: 0.05%~3%, p-hydroxyacetophenone: 0.01%~3%, silk fibroin: 0.01%~3%, tetrahydromethylpyrimidine carboxylic acid: 0.01%~3%, hydroxyethyl cellulose: 0.01%~3%, water: make up to 100%.

[0030] In some alternative embodiments, the essence mask containing silk fibroin comprises, by weight percentage, the following components: Glycerin: 3%~8%, 1,2-pentanediol: 0.1%~3%, 1,2-hexanediol: 0.1%~2%, p-hydroxyacetophenone: 0.05%~2%, silk fibroin: 0.1%~2%, tetrahydromethylpyrimidine carboxylic acid: 0.1%~2%, hydroxyethyl cellulose: 0.1%~2%, water: make up to 100%.

[0031] In some alternative embodiments, the silk fibroin-containing essence mask comprises, by weight percentage, the following components: Glycerin: 5%, 1,2-pentanediol: 1%, 1,2-hexanediol: 0.5%, p-hydroxyacetophenone: 0.5%, silk fibroin: 1%, tetrahydromethylpyrimidine carboxylic acid: 1%, hydroxyethyl cellulose: 0.5%, water: make up to 100%.

[0032] This invention discloses a method for preparing the above-mentioned essence mask containing silk fibroin, comprising the following steps: (1) Aqueous premixing: Add the prescribed amounts of water, glycerol, 1,2-pentanediol, 1,2-hexanediol and p-hydroxyacetophenone to the reaction vessel, stir evenly, heat to 40℃~50℃, keep warm and stir for 10min~15min to obtain the aqueous premix; (2) Preparation of thickening system: The prescribed amount of hydroxyethyl cellulose is slowly added to the above aqueous premixed solution, and stirred for 20 min to 30 min until the hydroxyethyl cellulose is completely dissolved to obtain a uniform thickening system; (3) Addition of active ingredients: Reduce the temperature of the reaction vessel to 25℃~30℃, add the formula amount of silk fibroin and tetrahydromethylpyrimidine carboxylic acid, stir evenly, keep warm and stir for 15min~20min until all components are completely dissolved and dispersed; (4) Homogenization and sterilization: The above mixture is homogenized at a speed of 3000 r / min to 5000 r / min for 5 min to 10 min, and then filtered and sterilized to obtain the essence mask stock solution. (5) Mask preparation: Inject the sterilized essence mask stock solution into a packaging container containing the mask sheet, seal the packaging, and the finished essence mask is obtained.

[0033] In some alternative embodiments, the filtration sterilization in step (4) is performed using a 0.22 μm microporous membrane.

[0034] In some alternative embodiments, the mask fabric in step (5) is one of Tencel mask fabric, silk mask fabric or cotton velvet mask fabric.

[0035] This invention also discloses the application of the above-mentioned silk fibroin-containing essence mask in the preparation of moisturizing and repairing skin care products.

[0036] All raw materials used in this invention were purchased from the market.

[0037] The technical solution of the present invention will be further illustrated by the following embodiments.

[0038] Example 1 A silk fibroin-containing essence mask, comprising the following components by weight percentage: Glycerin: 5%, 1,2-pentanediol: 1%, 1,2-hexanediol: 0.5%, p-hydroxyacetophenone: 0.5%, silk fibroin: 1%, tetrahydromethylpyrimidine carboxylic acid: 1%, hydroxyethyl cellulose: 0.5%, water: 90.5%.

[0039] The preparation method of this silk fibroin-containing essence mask includes the following steps: (1) Aqueous premixing: Add the prescribed amounts of water, glycerol, 1,2-pentanediol, 1,2-hexanediol and p-hydroxyacetophenone to the reaction vessel, stir evenly, heat to 45°C, keep warm and stir for 12 min to obtain the aqueous premix; (2) Preparation of thickening system: The prescribed amount of hydroxyethyl cellulose is slowly added to the above aqueous premixed solution, and stirred for 25 min until the hydroxyethyl cellulose is completely dissolved to obtain a uniform thickening system; (3) Addition of active ingredients: Reduce the temperature of the reaction vessel to 28°C, add the formulated amount of silk fibroin and tetrahydromethylpyrimidine carboxylic acid, stir evenly, keep warm and stir for 18 minutes until all components are completely dissolved and dispersed; (4) Homogenization and sterilization: The above mixture is homogenized at a speed of 4000 r / min for 8 min. Then, it is filtered and sterilized using a 0.22 μm microporous membrane to obtain the essence mask stock solution. (5) Mask preparation: The sterilized essence mask stock solution is injected into an aluminum foil bag containing Tencel mask cloth, sealed and packaged to obtain the finished essence mask.

[0040] Example 2 A silk fibroin-containing essence mask, comprising the following components by weight percentage: Glycerin: 3%, 1,2-pentanediol: 0.1%, 1,2-hexanediol: 0.1%, p-hydroxyacetophenone: 0.05%, silk fibroin: 0.1%, tetrahydromethylpyrimidine carboxylic acid: 0.1%, hydroxyethyl cellulose: 0.1%, water: 96.45%.

[0041] The preparation method is the same as in Example 1.

[0042] Example 3 A silk fibroin-containing essence mask, comprising the following components by weight percentage: Glycerin: 8%, 1,2-pentanediol: 3%, 1,2-hexanediol: 2%, p-hydroxyacetophenone: 2%, silk fibroin: 2%, tetrahydromethylpyrimidine carboxylic acid: 2%, hydroxyethyl cellulose: 2%, water: 79%.

[0043] The preparation method is the same as in Example 1.

[0044] Comparative Example 1 The difference between this comparative example and Example 1 is that tetrahydromethylpyrimidine carboxylic acid is not added to the formulation, while the other components and preparation methods, except for water, are the same as in Example 1.

[0045] Comparative Example 2 The difference between this comparative example and Example 1 is that p-hydroxyacetophenone is not added to the formulation, while the other components and preparation methods, except for water, are the same as in Example 1.

[0046] Performance testing I. Moisturizing Performance Test One hundred and ten healthy volunteers, aged 20-45 years, were randomly divided into 11 groups of 10 each. Each group used one of the masks described in Examples 1-3, Comparative Examples 1-2, or two commercially available silk fibroin-containing mask products (Control 1 and Control 2). Before the test, all volunteers washed their faces and sat quietly for 30 minutes in a constant temperature and humidity environment (temperature 22℃±2℃, relative humidity 50%±5%). The initial skin moisture content was measured using a skin moisture meter. The masks were then applied for 15 minutes. After removing the masks, the skin moisture content was measured at 1 hour, 4 hours, and 8 hours. The skin moisture enhancement rate was calculated, and the results are shown in the table below. Table 1 As can be seen from the results in the table above, the facial mask products of Examples 1-3 of the present invention are significantly better than the comparative examples and commercially available control products in terms of both immediate and long-lasting moisturizing effects. Among them, Example 3 has the best moisturizing effect, with a skin moisture increase rate of 38.5% after 8 hours, indicating that the formulation system of the present invention has excellent long-lasting moisturizing ability.

[0047] II. Silk fibroin activity retention rate test The facial mask products of Examples 1-3 and Comparative Examples 1-2 were placed in a constant temperature and humidity chamber and stored for 12 months at a temperature of 25°C and a relative humidity of 60%. The activity content of silk fibroin before and after storage was tested by ELISA, and the activity retention rate was calculated. The results are shown in the table below: Table 2 As shown in the table above, the mask products of Examples 1-3 of this invention can retain more than 93% of the silk fibroin activity after 12 months of storage, which is significantly better than Comparative Example 2. This indicates that the p-hydroxyacetophenone and polyol compound system can effectively protect the silk fibroin activity and improve the storage stability of the product.

[0048] III. Stimulation Testing Thirty volunteers with sensitive skin, aged 20-40 years, were randomly divided into three groups of 10 each. Each group used the mask products described in Examples 1-3 once daily for seven consecutive days. Skin reactions such as redness, itching, and stinging were observed. The results are shown in Table 3. Table 3 As shown in the table above, the mask product of the present invention is non-irritating and can be safely used by people with sensitive skin, making it suitable for a wide range of people.

[0049] The above are merely preferred embodiments of this application, but the scope of protection of this application is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in this application should be included within the scope of protection of this application. Therefore, the scope of protection of this application should be determined by the scope of the claims.

Claims

1. A silk fibroin-containing essence mask, characterized in that, excluding the mask sheet, By weight percentage, it includes the following components: Glycerin: 1%~10%, 1,2-pentanediol: 0.05%~5%, 1,2-hexanediol: 0.05%~3%, p-hydroxyacetophenone: 0.01%~3%, silk fibroin: 0.01%~3%, tetrahydromethylpyrimidine carboxylic acid: 0.01%~3%, hydroxyethyl cellulose: 0.01%~3%, balance: water.

2. The essence mask containing silk fibroin according to claim 1, characterized in that, By weight percentage, the essence mask containing silk fibroin comprises the following components: Glycerin: 3%~8%, 1,2-pentanediol: 0.1%~3%, 1,2-hexanediol: 0.1%~2%, p-hydroxyacetophenone: 0.05%~2%, silk fibroin: 0.1%~2%, tetrahydromethylpyrimidine carboxylic acid: 0.1%~2%, hydroxyethyl cellulose: 0.1%~2%, balance: water.

3. The essence mask containing silk fibroin according to claim 2, characterized in that, By weight percentage, the essence mask containing silk fibroin comprises the following components: Glycerin: 5%, 1,2-pentanediol: 1%, 1,2-hexanediol: 0.5%, p-hydroxyacetophenone: 0.5%, silk fibroin: 1%, tetrahydromethylpyrimidine carboxylic acid: 1%, hydroxyethyl cellulose: 0.5%, water: 90.5%.

4. The essence mask containing silk fibroin according to claim 2, characterized in that, By weight percentage, the essence mask containing silk fibroin comprises the following components: Glycerin: 8%, 1,2-pentanediol: 3%, 1,2-hexanediol: 2%, p-hydroxyacetophenone: 2%, silk fibroin: 2%, tetrahydromethylpyrimidine carboxylic acid: 2%, hydroxyethyl cellulose: 2%, water: 79%.

5. A method for preparing an essence mask containing silk fibroin as described in any one of claims 1-4, characterized in that, Includes the following steps: (1) Add water, glycerol, 1,2-pentanediol, 1,2-hexanediol and p-hydroxyacetophenone to the reaction vessel according to the weight percentage, stir evenly, and then heat to obtain an aqueous premix; (2) Slowly add hydroxyethyl cellulose to the aqueous premix, keep warm and stir until the hydroxyethyl cellulose is completely dissolved to obtain a uniform thickening system; (3) Reduce the temperature of the reactor to 25℃~30℃, add the formulated amount of silk fibroin and tetrahydromethylpyrimidine carboxylic acid, stir evenly, and keep warm while stirring until all components are completely dissolved and dispersed; (4) Homogenize, filter and sterilize the mixture obtained in step (3) to obtain the essence mask stock solution; (5) Inject the essence mask stock solution into the packaging container containing the mask sheet, seal the packaging, and you will get the finished essence mask.

6. The method for preparing the essence mask containing silk fibroin according to claim 5, characterized in that, In step (1), the heating conditions are: heating to 40℃~50℃ and stirring for 10min~15min.

7. The method for preparing the essence mask containing silk fibroin according to claim 5, characterized in that, In step (2), the time for heat preservation and stirring is 20 min to 30 min.

8. The method for preparing the essence mask containing silk fibroin according to claim 5, characterized in that, In step (3), the time for heat preservation and stirring is 15 min to 20 min.

9. The method for preparing the essence mask containing silk fibroin according to claim 5, characterized in that, In step (4), the homogenization speed during the homogenization process is 3000 r / min to 5000 r / min, and the homogenization time is 5 min to 10 min.

10. The method for preparing the essence mask containing silk fibroin according to claim 5, characterized in that, In step (5), the mask fabric is one of Tencel mask fabric, silk mask fabric or cotton velvet mask fabric.

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