Mask containing silk fibroin composite microspheres and preparation method thereof
By combining silk protein microspheres with Centella asiatica extract, yeast/zinc fermentation products, and silk amino acids, the problem of low mask penetration efficiency is solved, achieving multi-dimensional care effects of immediate soothing, moisturizing, and firming, and significantly improving skin condition.
Patent Information
- Application Number
- CN202511638986.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-10
- Publication Date
- 2026-01-16
AI Technical Summary
Existing facial mask products have low penetration efficiency and cannot effectively penetrate the skin, resulting in a rapid decline in the effect after the initial pseudo-plumping effect. They cannot achieve true bio-level firming, and most products have only one function, failing to address skin stress, damage, and aging issues simultaneously.
Using silk protein complex microspheres as a skin protectant, combined with Centella asiatica extract, yeast/zinc fermentation products and silk amino acids, transdermal absorption microspheres are formed through supramolecular self-assembly, which enhances the penetration efficiency of active ingredients and achieves moisturizing and firming effects in the deep layers of the skin.
It achieves multi-dimensional skin condition reversal in a short period of time, providing immediate soothing, moisturizing and firming effects, improving skin hydration and water barrier function, and significantly improving skin roughness and wrinkle depth.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application belongs to the technical field of cosmetic preparation, and particularly relates to a mask containing silk fibroin composite microspheres and a preparation method thereof. BACKGROUND
[0002] With the acceleration of modern life pace, the skin is continuously facing multiple challenges of environmental stress, digital blue light and internal emotional stress, resulting in problems such as damaged skin barrier, accelerated water loss and accelerated collagen degradation. However, a large number of mask products on the market have single efficacy positioning: or only focus on instant hydration while ignoring repair, or blindly pursue strong anti-wrinkle effect while the formula is highly irritating. For the skin in a stressed state, it is impossible to break the vicious cycle described above, and even the skin burden may be aggravated due to the irritation of the formula.
[0003] At the same time, the short application time of the mask puts high requirements on the penetration efficiency of active ingredients. Many products still use conventional formula bases, and a large amount of essence only stays on the surface of the stratum corneum. Key firming ingredients (such as peptides and collagen) cannot effectively penetrate the skin due to their large molecular weight or lack of penetration enhancement technology, resulting in rapid fading of the effect after "instant false fullness" and failure to achieve real biological firming.
[0004] Under this background, the market urgently needs an intensive care product that can provide instant repair and long-term improvement. The development of a mask that integrates soothing, moisturizing and firming into one is based on deep insight into the chain reaction of skin stress, damage and aging. It aims to reverse the skin state in multiple dimensions in a short time through precise formula design and advanced carrier technology, and meet the urgent needs of consumers for high-performance and one-stop skin care solutions. SUMMARY
[0005] In view of the deficiencies in the prior art, the purpose of the present application is to provide a mask containing silk fibroin composite microspheres and integrating soothing, moisturizing and firming effects.
[0006] To achieve this purpose, the present application adopts the following technical solutions:
[0007] The present application provides a mask containing silk fibroin composite microspheres, which comprises a skin protectant, a skin conditioner, a moisturizing agent and a thickening agent, wherein the skin protectant comprises: a silk fibroin composite microsphere aqueous solution, a centella asiatica extract, a yeast / zinc fermentation product and a silk amino acid.
[0008] The primary role of the silk fibroin composite microspheres in the present application is to reduce the skin barrier resistance, opening a channel for the transdermal absorption of other active ingredients, greatly improving the transdermal penetration efficiency of effective ingredients, and ensuring that effective ingredients can reach the target action layer in sufficient and deep manner, rather than just staying on the surface.
[0009] The skin protectant in the mask formula of the present application, with the assistance of silk fibroin composite microspheres, can act on stressed nerve receptors and inflammatory targets more quickly, immediately inhibit the release of inflammatory factors, and quickly relieve redness, burning, itching, and other discomfort. This step creates a stable, low-irritation skin environment for moisturizing and firming effects, avoiding the risk of intolerance that may be caused by directly using potent ingredients in a stressed state of the skin.
[0010] In the present application, the Centella asiatica extract, yeast / zinc fermentation product, and silk amino acids penetrate deeper into the skin with the assistance of silk fibroin composite microspheres, achieving hydration from the inside out. They not only quickly replenish the water content of the stratum corneum, but also promote the synthesis of natural moisturizing factor (NMF) and the repair of intercellular lipids, thereby strengthening the skin's own water-locking barrier. This deep moisturization provides a necessary hydration environment for the healthy growth of collagen, and more effectively enhances the effects of firming ingredients.
[0011] The effective ingredients such as Centella asiatica extract, yeast / zinc fermentation product, silk amino acids, and sodium hyaluronate can effectively inhibit excessive muscle contraction, stimulate fibroblasts to regenerate collagen and elastin, and structurally reverse relaxation to reshape the skin's firm, elastic, and supple young quality.
[0012] The yeast / zinc fermentation product is rich in small molecule amino acids, polypeptides, nucleotides, vitamins, and other natural active ingredients, making it a very good comprehensive skin conditioner.
[0013] Silk amino acids, with the INCI name SILK AMINO ACIDS and CAS 96690-41-4, are a mixture of amino acids extracted from natural silk. These amino acids have high physiological activity and human compatibility. Silk amino acids are a highly active cosmetic and skincare raw material that has the effects of moisturizing, nourishing the skin, inhibiting melanin formation, promoting skin tissue regeneration, preventing cracking and chemical damage, and so on.
[0014] As a preferred technical scheme of the present application, the facial mask comprises, by mass percentage, 1.5% to 10% (for example, 1.5%, 2%, 2.5%, 3%, 5%, 6%, 7%, 8%, 9% or 10%, etc.) of a skin protectant, 0.5% to 5% (for example, 0.5%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5% or 5%, etc.) of a skin conditioning agent, 5% to 10% (for example, 5%, 6%, 7%, 8%, 9% or 10%, etc.) of a humectant, 0.05% to 0.5% (for example, 0.05%, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45% or 0.5%, etc.) of a thickening agent, and 0.05% to 0.2% (for example, 0.05%, 0.1%, 0.12%, 0.15%, 0.16%, 0.18% or 0.2%, etc.) of a pH adjuster; and the balance is water.
[0015] Preferably, the facial mask comprises, by mass percentage, 1% to 2% (for example, 1%, 1.2%, 1.5%, 1.6%, 1.7%, 1.8% or 2%, etc.) of a silk fibroin composite microsphere aqueous solution, 0.2% to 1% (for example, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9% or 1%, etc.) of a centella asiatica extract, 0.1% to 0.5% (for example, 0.1%, 0.2%, 0.3%, 0.4% or 0.5%, etc.) of a yeast / zinc fermentation product, and 0.05% to 0.2% (for example, 0.05%, 0.1%, 0.12%, 0.15%, 0.16%, 0.18% or 0.2%, etc.) of a silk amino acid.
[0016] As a preferred technical scheme of the present application, the silk fibroin composite microspheres are prepared by the following method: silk fibroin and polydeoxyribonucleic acid (PDRN) are mutually penetrated, entangled and folded and compressed under the action of polylysine to obtain the silk fibroin composite microspheres.
[0017] It is found by molecular docking calculation simulation that there is a supramolecular interaction between PDRN and silk fibroin, and the interaction is used to make silk fibroin and PDRN self-assemble through intermolecular forces. In addition, the nucleic acid substance property of PDRN that is beneficial to folding is also used to automatically compress to obtain a complex aggregate with clear structure and specific function. The obtained silk fibroin composite microspheres can penetrate the cell membrane, enter the cell, and achieve the effect of transdermal absorption.
[0018] Preferably, the average particle size of the silk core protein composite microspheres is 50 nm to 500 nm, for example, it can be 50 nm, 100 nm, 150 nm, 200 nm, 250 nm, 300 nm, 320 nm, 330 nm, 340 nm, 350 nm, 360 nm, 380 nm, 400 nm, 420 nm, 450 nm, 480 nm or 500 nm, etc.
[0019] As a preferred technical solution of the present invention, in the raw materials for preparing the silk core protein composite microspheres, the mass ratio of silk core protein to polylysine is 1:(0.006~0.2), for example, it can be 1:0.006, 1:0.01, 1:0.02, 1:0.05, 1:0.1, 1:0.15 or 1:0.2, etc.
[0020] Preferably, the mass ratio of the silk core protein to polydeoxyribonucleic acid is 1:(1~10), for example, it can be 1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9 or 1:10, etc.
[0021] Preferably, the mass ratio of polylysine to polydeoxyribonucleic acid is 1:(5~150), for example, it can be 1:5, 1:5, 1:10, 1:20, 1:50, 1:60, 1:80, 1:100, 1:120 or 1:150, etc.
[0022] Preferably, the mass percentage of fibroin in the aqueous solution of the fibroin composite microspheres is 1% to 5%, for example, it can be 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5% or 5%, etc.
[0023] Preferably, the mass percentage of polylysine in the aqueous solution of the silk core protein composite microspheres is 0.01% to 1%. Polylysine is used to provide a cationic environment, and its mass percentage can be 0.01%, 0.02%, 0.05%, 0.1%, 0.2%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, or 1%, etc.
[0024] Preferably, the mass percentage of PDRN in the aqueous solution of the silk core protein composite microspheres is 1% to 5%, for example, it can be 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5% or 5%, etc.
[0025] Preferably, the polylysine comprises basic polylysine and / or modified polylysine.
[0026] Preferably, the polylysine is a mixture of basic polylysine and modified polylysine in a mass ratio of 1:(0.5~0.8), such as 1:0.5, 1:0.55, 1:0.6, 1:0.65, 1:0.7, 1:0.75 or 1:0.8.
[0027] Among them, basic polylysine provides a cationic environment, which triggers the formation of complex microparticles. Using modified polylysine to partially replace basic polylysine further improves transdermal absorption.
[0028] Preferably, the preparation of the modified polylysine includes the following steps:
[0029] Add the carboxyl group of phospholipid polyethylene glycol to water and stir evenly. Add 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (EDC) and N-hydroxysuccinimide (NHS), stir at 25-30℃ for 5-10 min, and dropwise add to a buffer solution containing basic polylysine (the buffer solution is a phosphate buffer solution with a pH of 7.4). Stir at 25-30℃ for 20-24 h, purify, and freeze-dry to obtain modified polylysine.
[0030] As a preferred technical solution of the present invention, the aqueous solution of the silk core protein composite microspheres further contains a pH adjuster, and the pH of the aqueous solution of the silk core protein composite microspheres is 5.5-6.5, for example, it can be 5.5, 5.6, 5.8, 6.0, 6.2, 6.3 or 6.5, etc.
[0031] Preferably, the pH adjuster includes any one or a combination of at least two of citric acid, lactic acid, malic acid, tartaric acid or glycolic acid, with citric acid being the most preferred.
[0032] Preferably, the aqueous solution of the silk core protein composite microspheres further contains a thickener, and the content of the thickener in the aqueous solution of the silk core protein composite microspheres is 0.5% to 1%, for example, it can be 0.5%, 0.6%, 0.7%, 0.8%, 0.9% or 1%, etc.
[0033] Preferably, the thickener is hydroxyethyl cellulose.
[0034] In this invention, fibroin, PDRN, and polylysine can form the fibroin composite microspheres. Adding optional components such as thickeners and pH adjusters further facilitates storage and improves compatibility with other components. The amounts of thickener and pH adjuster used can be adjusted according to subsequent application requirements.
[0035] As a preferred embodiment of the present invention, the skin conditioning agent comprises any one or a combination of at least two of the following: polydimethylsiloxane, hydroxyethylpiperazine ethanesulfonic acid, panthenol, and tetrahydromethylpyrimidine carboxylic acid.
[0036] Preferably, the moisturizer comprises any one or a combination of at least two of 1,2-hexanediol, methyl propylene glycol, glycerin, methyl gluceth-20, and sodium hyaluronate.
[0037] Preferably, the thickener is an acrylate / C10-30 alkanol acrylate crosspolymer.
[0038] Preferably, the pH adjuster includes aminomethylpropanol, and the pH of the mask is 4.0 to 8.5.
[0039] As a preferred embodiment of the present invention, in the raw materials for preparing the facial mask, the mass percentage of polydimethylsiloxane is 0.1%~0.5% (e.g., 0.1%, 0.2%, 0.3%, 0.4%, or 0.5%), the mass percentage of hydroxyethylpiperazine ethanesulfonic acid is 0.1%~0.5% (e.g., 0.1%, 0.2%, 0.3%, 0.4%, or 0.5%), the mass percentage of panthenol is 0.1%~0.5% (e.g., 0.1%, 0.2%, 0.3%, 0.4%, or 0.5%), and the mass percentage of tetrahydromethylpyrimidine carboxylic acid is 0.05%~0.2% (e.g., 0.05%, 0.08%, 0.1%, 0.15%, or 0.2%).
[0040] Preferably, in the raw materials for preparing the facial mask, the mass percentage of 1,2-hexanediol is 0.5% to 1% (e.g., 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, or 1%), the mass percentage of methylpropanediol is 2% to 5% (e.g., 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, or 5%), and the mass percentage of glycerin is 2% to 5% (e.g., 2%, 2.5%, or 3%). The mass percentage of methyl gluceth-20 is 0.1% to 0.5% (e.g., 0.1%, 0.2%, 0.3%, 0.4%, or 0.5%), and the mass percentage of sodium hyaluronate is 0.005% to 0.02% (e.g., 0.005%, 0.008%, 0.01%, 0.012%, 0.015%, 0.018%, or 0.02%).
[0041] The facial mask described in this invention can be a facial mask sheet or a facial mask spreader. Preferably, the facial mask sheet comprises a facial mask fabric and a facial mask impregnated on the facial mask fabric.
[0042] In a second aspect, the present invention also provides a method for preparing a facial mask as described in the first aspect, the method comprising the following steps:
[0043] Mix the formulated amounts of silk protein composite microsphere aqueous solution, Centella asiatica extract, yeast / zinc fermentation product, silk amino acids, skin conditioning agent, moisturizer and thickener, and stir to obtain the face mask.
[0044] As a preferred embodiment of the present invention, the preparation method of the silk-core protein composite microsphere aqueous solution includes the following steps:
[0045] Add polydeoxyribonucleic acid to water and stir until homogeneous to obtain an aqueous solution of polydeoxyribonucleic acid;
[0046] Dilute the silk protein solution, mix it with an aqueous solution of polydeoxyribonucleic acid, add an aqueous solution of polylysine to obtain a composite solution system, and stir to mix.
[0047] Then add an optional pH adjuster and thickener, and stir to obtain the aqueous solution of the silk core protein composite microspheres.
[0048] As a preferred technical solution of the present invention, the methyl propylene glycol, glycerin, methyl gluceth-20, panthenol, acrylate / C10-30 alkanol acrylate crosspolymer and sodium hyaluronate in the facial mask are mixed and dissolved at 80℃~90℃ (for example, 80℃, 82℃, 84℃, 85℃, 86℃, 88℃ or 90℃, etc.).
[0049] Preferably, the aminomethylpropanol is mixed and dissolved at 70°C to 80°C (e.g., 70°C, 72°C, 74°C, 75°C, 76°C, 78°C, or 80°C).
[0050] Preferably, the aqueous solution of the silk protein composite microspheres, 1,2-hexanediol, Centella asiatica extract, yeast / zinc fermentation product, polydimethylsiloxane, hydroxyethylpiperazine ethanesulfonic acid, tetrahydromethylpyrimidine carboxylic acid, and silk amino acids are mixed and dissolved at 40°C to 45°C (e.g., 40°C, 41°C, 42°C, 43°C, 44°C, or 45°C).
[0051] The numerical range described in this invention includes not only the point values listed above, but also any point values within the numerical ranges not listed above. Due to space limitations and for the sake of brevity, this invention will not exhaustively list all the specific point values included in the range.
[0052] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0053] The moisturizing and firming mask provided by this invention contains four different skin protectants. Among them, Centella asiatica extract, yeast / zinc fermentation products and silk amino acids, with the assistance of silk protein composite microspheres, can penetrate to deeper layers of the skin. The resulting mask transcends the single and superficial care level of traditional masks. Through systematic formula architecture and carrier innovation, it breaks the vicious cycle of sensitivity, dryness and sagging, thereby achieving the care effects of moisturizing, firming and repairing.
[0054] This invention uses a moisture meter to measure the rate of change in skin moisture content and the TWEL value after 14 and 28 days of use of the mask. The experimental results show that after 14 days of use, the rate of change in skin moisture content is greater than 12%, reaching a maximum of 17.89%; after 28 days of use, the rate of change is greater than 16%, reaching a maximum of 26.55%. Simultaneously, the TWEL value is significantly lower between days 14 and 28. Furthermore, image analysis of the changes in average skin roughness and average wrinkle depth shows that the skin is significantly smoother after 28 days of use. Detailed Implementation
[0055] The technical solution of the present invention will be further illustrated below through specific embodiments. However, the following examples are merely simplified examples of the present invention and do not represent or limit the scope of protection of the present invention. The scope of protection of the present invention shall be determined by the claims.
[0056] In the following embodiments, the experimental materials and consumables were all purchased from conventional reagent manufacturers in the art; unless otherwise specified, the experimental methods and techniques used are conventional methods and techniques in the art.
[0057] Among them, silk heart protein can be purchased from Suzhou Suhao Biomaterials Co., Ltd.; PDRN can be purchased from Ruijiming Biotechnology Co., Ltd. or Shanghai Huiwen Biotechnology Co., Ltd.; polylysine can be purchased from Shandong Freda Biotechnology Co., Ltd. or Shanghai Maclean Biochemical Technology Co., Ltd.; Centella Asiatica extract can be purchased from Microcare Biotechnology (Yantai) Co., Ltd.; yeast / zinc fermentation products can be purchased from Angel Yeast Co., Ltd.; silk amino acids can be purchased from Beijing Aosimei Biotechnology Co., Ltd., under the product name Sishuyuan; polydimethylsiloxane can be purchased from Guangzhou Hengtai Chemical Co., Ltd.; 1,2-hexanediol can be purchased from Microcare Emollient HXD(P) Toll Chemical; glycerol can be purchased from Procter & Gamble International Operations SA Singapore Branch; methyl glucetol polyether-20 can be purchased from Ningbo Dongfang Yongning Chemical Technology Co., Ltd.; sodium hyaluronate can be purchased from Shandong Focus Freda Biotechnology Co., Ltd.; acrylates / C10-30 alkanol acrylate crosspolymers can be purchased from Lubrizol Advanced Materials, Inc.
[0058] All other materials not mentioned can be purchased from conventional manufacturers in this field.
[0059] The aqueous solution of the silk core protein composite microspheres described in this invention can be prepared according to the following method:
[0060] (1) Dissolve 1 g of PDRN (DNA content ≥70%, purchased from Ruijiming Biotechnology Co., Ltd.) in 50 g of water and stir until homogeneous to obtain PDRN solution; dissolve 1 g of silk protein (purchased from Suzhou Suhao Biomaterials Co., Ltd.) in 25 g of water and stir until homogeneous; then dissolve 0.05 g of polylysine (purchased from Shandong Freda Biotechnology Co., Ltd.) in 25 g of water and stir.
[0061] (2) Mix the silk core protein solution prepared in step (1) with the PDRN solution and stir for 60 min at a stirring speed of 600 rpm. Then, add the polylysine solution and stir at 600 rpm for 30 min.
[0062] (3) Add 0.5% by mass of hydroxyethyl cellulose (purchased from Beijing Kangtailong Technology Development Co., Ltd., molecular weight and viscosity 3400~5000 mPa.s), and then use citric acid to adjust the pH of the solution to about 6 to obtain an aqueous solution containing the silk core protein composite microspheres, wherein the particle size of the silk core protein composite microspheres is <500 nm.
[0063] Example 1
[0064] This embodiment provides a face mask, the raw materials for which the face mask is prepared are shown in Table 1, including:
[0065] Table 1
[0066] The preparation method is as follows:
[0067] (1) Add water, methyl propylene glycol, glycerin, methyl glucetol polyether-20, panthenol, acrylate / C10-30 alkanol acrylate crosspolymer and sodium hyaluronate to an emulsifying pot, turn on the homogenizer, homogenize for 5 minutes, stir and heat to 85°C, keep warm for 20 minutes to ensure complete dissolution, and start cooling.
[0068] (2) Cool down to 75°C, add aminomethylpropanol and stir well, then continue to cool down;
[0069] (3) Cool down to 45°C, add the following ingredients: silk protein composite microsphere aqueous solution, 1,2-hexanediol, Centella asiatica extract, yeast / zinc fermentation product, polydimethylsiloxane, hydroxyethylpiperazine ethane sulfonic acid, tetrahydromethylpyrimidine carboxylic acid and silk amino acids, and stir evenly.
[0070] (4) Cool down to 38°C, stop stirring, and obtain the face mask.
[0071] Example 2
[0072] This embodiment provides a face mask, the difference between the raw materials used in the preparation of the face mask and those in Embodiment 1 is as follows:
[0073] The content of the silk heart protein composite microsphere aqueous solution is 0.5%; the content of Centella Asiatica extract is 1.5%; the content of yeast / zinc fermentation product is 1%; and the content of silk amino acids is 0.05%.
[0074] Example 3
[0075] This embodiment provides a face mask, the difference between the raw materials used in the preparation of the face mask and those in Embodiment 1 is as follows:
[0076] The content of the silk heart protein composite microsphere aqueous solution is 2.5%; the content of Centella Asiatica extract is 0.1%; the content of yeast / zinc fermentation product is 0.5%; and the content of silk amino acids is 0.01%.
[0077] Example 4
[0078] This embodiment provides a face mask, which differs from Embodiment 1 in that the skin conditioning agent in the face mask is a single polydimethylsiloxane; its content is increased to 0.9%.
[0079] Example 5
[0080] This embodiment provides a face mask, which differs from Embodiment 1 in that the skin conditioning agent in the face mask is a single hydroxyethylpiperazine ethanesulfonic acid; its content is increased to 1.9%.
[0081] Example 6
[0082] This embodiment provides a face mask, which differs from Embodiment 1 in that the moisturizer in the face mask is a single methylpropanediol; its content is increased to 6.81%.
[0083] Comparative Example 1
[0084] This comparative example provides a face mask that differs from Example 1 in that the face mask does not contain an aqueous solution of silk protein composite microspheres, and the missing mass fraction is made up by silk amino acids.
[0085] Comparative Example 2
[0086] This comparative example provides a face mask that differs from Example 1 in that the face mask does not contain Centella Asiatica extract, and the missing mass fraction is made up by silk amino acids.
[0087] Comparative Example 3
[0088] This comparative example provides a face mask that differs from Example 1 in that the face mask replaces Centella asiatica extract with meadowfoam (LIMNANTHES ALBA) seed oil (purchased from Elementis Specialties, Inc.), and the missing mass fraction is made up by silk amino acids.
[0089] Comparative Example 4
[0090] This comparative example provides a face mask that differs from Example 1 in that the face mask does not contain yeast / zinc fermentation products, and the missing mass fraction is made up by silk amino acids.
[0091] Comparative Example 5
[0092] This comparative example provides a face mask that differs from Example 1 in that the face mask does not contain silk amino acids, and the missing mass fraction is made up by an aqueous solution of silk protein composite microspheres.
[0093] Comparative Example 6
[0094] This comparative example provides a face mask that differs from Example 1 in that the face mask replaces the aqueous solution of silk core protein composite microspheres with an equal amount of silk core protein and PDRN.
[0095] Test Example 1
[0096] Human skin patch experiment
[0097] Participants: 30 in total, 0 males and 30 females, aged 18-40 years, meeting the criteria for voluntary inclusion.
[0098] Patch method: Using a qualified patch tester, approximately 0.025 g of the test substance (Examples 1-6 and Comparative Examples 1-6) was applied to the patch tester using a closed patch test method. The patch was then applied to the back of the subject with special adhesive tape. The test substance was removed after 24 hours. Skin reactions were observed at 0.5 hours, 24 hours, and 48 hours after removal. The results were recorded according to the skin reaction grading standards in the "Cosmetic Hygiene Standard".
[0099] The results of the human skin patch test showed that none of the 30 subjects experienced symptoms such as erythema, edematous erythema, significant redness or swelling, or papules; indicating that the masks provided in the examples and comparative examples are safe to use.
[0100] Test Example 2
[0101] Skin moisture content and skin moisture loss (TEWL) test
[0102] Because water differs significantly from other substances in dielectric constant, a moisture content testing probe can reflect water content by measuring changes in the capacitance of the stratum corneum. This invention uses a moisture meter to measure the moisture content of the stratum corneum on the right cheek of a subject, taking three measurements and averaging them. A before-and-after comparison is used to evaluate the moisturizing efficacy of the product.
[0103] TEWL (Temperature-to-Waist-Length) value is an important indicator of skin barrier health. A lower TEWL value indicates better skin barrier function, and vice versa. A higher TEWL value also indicates a greater reduction in skin moisture loss and better skin barrier repair.
[0104] Based on Fick's law of diffusion, the transdermal moisture loss meter reflects transdermal moisture loss by calculating the amount of water diffused per unit time and per unit area. This study measured transdermal moisture loss on the right side of the subject's face, taking three measurements and averaging them. A before-and-after comparison was used to evaluate the product's repair efficacy.
[0105] Testing Method: Volunteers aged 20-45 years were selected and randomly assigned to groups, with at least 30 participants per sample. Two samples were tested on each participant's left and right sides of the face. No products (including cosmetics, topical medications, and oral supplements) were used on the test areas for 15 days prior to the test. Before the test, participants were required to wash their faces and, 2 hours later, sit quietly in a climate-controlled room (22±1℃, 50% relative humidity) for at least 20 minutes, maintaining a relaxed state.
[0106] Moisture content data (D0) was recorded the day before the test. Volunteers used the product once every two days after cleansing. Moisture content data (D14, D28) was recorded after the test and its rate of change was calculated. At the same time, its TEWL value (D14, D28) was also recorded.
[0107] The results are shown in Table 2:
[0108] Table 2
[0109] As can be seen from the table above, the components of the mask described in this invention are rationally combined and have a synergistic effect, enhancing the internal cellular water cycle, strengthening the surface water-locking barrier, repairing the stratum corneum barrier, reducing transepidermal water loss, and improving the water-locking capacity of the stratum corneum.
[0110] Meanwhile, a comparison of Example 1 with Comparative Examples 1 and 6 shows that the silk-core protein composite microspheres in this invention have an irreplaceable effect in improving the transdermal absorption efficiency of the mask. If the silk-core protein composite microspheres are not present, the skin moisturizing effect is significantly reduced.
[0111] A comparison of Example 1 and Comparative Examples 2-5 shows that the silk protein composite microspheres in this invention, combined with Centella asiatica extract, yeast / zinc fermentation products, and silk amino acids, work synergistically to achieve the best moisturizing and water-locking effect; if any of the components is missing or replaced, the water-locking effect is significantly reduced.
[0112] Test Example 3
[0113] Anti-aging and anti-wrinkle test
[0114] Sixty volunteers were randomly selected and divided into two groups, using Example 1 and Comparative Example 1 respectively. The test sites were both cheeks and the corners of the eyes. The product was used once every two days after cleansing.
[0115] One day before and 28 days after using the mask, the changes in average skin roughness and average wrinkle depth were measured using the EVA FACE rapid optical imaging system. The average values were calculated and are shown in Table 3.
[0116] Table 3
[0117] As can be seen from the rate of change, using Example 1 of the present invention significantly improves the skin roughness and skin wrinkle depth values compared to Comparative Example 1.
[0118] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.
Claims
1. A facial mask containing silk-core protein composite microspheres, wherein the raw materials for preparing the facial mask include skin protectants, skin conditioning agents, moisturizers, and thickeners, characterized in that, The skin protectants in the mask include: a water solution of silk protein complex microspheres, centella asiatica extract, yeast / zinc fermentation products, and silk amino acids.
2. The facial mask according to claim 1, characterized in that, The mask comprises, by weight percentage: 1.5%~3% skin protectant, 0.5%~5% skin conditioning agent, 5%~10% moisturizer, 0.05%~0.5% thickener, and 0.05%~0.2% pH adjuster, with the remainder being water; Preferably, the mask comprises, by weight percentage: 1%~2% aqueous solution of silk protein composite microspheres, 0.2%~1% Centella asiatica extract, 0.1%~0.5% yeast / zinc fermentation product and 0.05%~0.2% silk amino acids.
3. The facial mask according to claim 1 or 2, characterized in that, The aqueous solution of the silk-core protein composite microspheres contains silk-core protein composite microspheres, which are prepared by the following method: silk-core protein and polydeoxyribonucleic acid are interpenetrated, entangled, folded and compressed under the action of polylysine to obtain the silk-core protein composite microspheres; Preferably, the average particle size of the silk-core protein composite microspheres is 50 nm to 500 nm; Preferably, the polylysine comprises basic polylysine and / or modified polylysine.
4. The facial mask according to claim 3, characterized in that, In the raw materials for preparing the silk core protein composite microspheres, the mass ratio of silk core protein to polylysine is 1:(0.006~0.2), the mass ratio of silk core protein to polydeoxyribonucleic acid is 1:(1~10), and the mass ratio of polylysine to polydeoxyribonucleic acid is 1:(5~150). Preferably, the mass percentage of silk core protein in the aqueous solution of the silk core protein composite microspheres is 1% to 5%; Preferably, the mass percentage of polylysine in the aqueous solution of the silk-core protein composite microspheres is 0.01%~1%; Preferably, the mass percentage of PDRN in the aqueous solution of the silk core protein composite microspheres is 1% to 5%.
5. The facial mask according to claim 1, characterized in that, The skin conditioning agent includes any one or a combination of at least two of the following: polydimethylsiloxane, hydroxyethylpiperazine ethane sulfonic acid, panthenol, and tetrahydromethylpyrimidine carboxylic acid; Preferably, the moisturizer comprises any one or a combination of at least two of the following: 1,2-hexanediol, methylpropanediol, glycerin, methyl gluceth-20, and sodium hyaluronate; Preferably, the thickener is an acrylate / C10-30 alkanol acrylate crosslinked polymer; Preferably, the pH adjuster includes aminomethylpropanol, and the pH of the mask is 4.0 to 8.
5.
6. The facial mask according to claim 5, characterized in that, In the raw materials for preparing the facial mask, the mass percentage of polydimethylsiloxane is 0.1%~0.5%, the mass percentage of hydroxyethylpiperazine ethanesulfonic acid is 0.1%~0.5%, the mass percentage of panthenol is 0.1%~0.5%, and the mass percentage of tetrahydromethylpyrimidine carboxylic acid is 0.05%~0.2%. Preferably, in the raw materials for preparing the facial mask, the mass percentage of 1,2-hexanediol is 0.5%~1%, the mass percentage of methyl propylene glycol is 2%~5%, the mass percentage of glycerin is 2%~5%, the mass percentage of methyl glucetol polyether-20 is 0.1%~0.5%, and the mass percentage of sodium hyaluronate is 0.005%~0.02%.
7. The facial mask according to claim 1, characterized in that, The mask is a sheet mask; Preferably, the mask patch includes a mask sheet and a mask soaked in the mask sheet.
8. A method for preparing a facial mask as described in any one of claims 1 to 7, characterized in that, The preparation method includes the following steps: Mix the formulated amounts of silk protein composite microsphere aqueous solution, Centella asiatica extract, yeast / zinc fermentation product, silk amino acids, skin conditioning agent, moisturizer and thickener, and stir to obtain the face mask.
9. The preparation method according to claim 8, characterized in that, The preparation method of the aqueous solution of the silk core protein composite microspheres includes the following steps: Add polydeoxyribonucleic acid to water and stir until homogeneous to obtain an aqueous solution of polydeoxyribonucleic acid; Dilute the silk protein solution, mix it with an aqueous solution of polydeoxyribonucleic acid, add an aqueous solution of polylysine to obtain a composite solution system, and stir to mix. Then add an optional pH adjuster and thickener, and stir to obtain the aqueous solution of the silk core protein composite microspheres.
10. The preparation method according to claim 8, characterized in that, The mask contains methyl propylene glycol, glycerin, methyl gluceth-20, panthenol, acrylate / C10-30 alkanol acrylate crosspolymer, and sodium hyaluronate, which are mixed and dissolved at 80°C to 90°C. Preferably, the aminomethylpropanol is mixed and dissolved at 70°C to 80°C; Preferably, the aqueous solution of the silk protein composite microspheres, 1,2-hexanediol, Centella asiatica extract, yeast / zinc fermentation product, polydimethylsiloxane, hydroxyethylpiperazine ethanesulfonic acid, tetrahydromethylpyrimidine carboxylic acid, and silk amino acids are mixed and dissolved at 40°C to 45°C.