A gankeng active ingredient composite mask substrate and a preparation method thereof

Abstract

The present application relates to the field of cosmetic technology, and particularly relates to a combined mask substrate of active ingredients of Bombyx Batryticatus and a preparation method thereof. The mask substrate comprises the following components in mass fractions: 1-8 parts of active peptide extract of Bombyx Batryticatus, 5-20 parts of polyvinyl alcohol, 2-10 parts of sodium alginate, 1-6 parts of carboxymethyl chitosan, 5-15 parts of glycerol, 0.1-1 part of sodium hyaluronate, 0.5-3 parts of gluconolactone, 0.5-3 parts of calcium citrate, and 40-80 parts of water. The mask substrate can realize integrated construction of active peptide of Bombyx Batryticatus and gel network, has good rehydration performance, and can delay the release rate of active peptide. The raw materials are stable in source, the preparation process is mature, the safety is good, and the present application is suitable for popularization and application in the field of cosmetics.

Description

Technical Field

[0001] This invention relates to the field of cosmetic technology, and in particular to a composite facial mask matrix containing active ingredients from silkworm pupae and its preparation method. Background Technology

[0002] Silkworm larvae, also known as "stiff silkworms," ​​are the dried, stiffened bodies of silkworm larvae infected with Beauveria bassiana. They are a traditional Chinese medicine. Silkworm larvae are rich in proteins, polypeptides, polysaccharides, and various enzymes, offering skincare benefits such as promoting skin cell regeneration, regulating sebum production, improving skin microcirculation, and scavenging free radicals. Among these, silkworm larvae's active peptides have attracted attention in the cosmetics industry due to their small molecular weight and relatively easy transdermal absorption.

[0003] Currently, when applying the active ingredients of silkworm pupae to facial mask products, the method of extraction followed by direct addition is commonly used. A common practice is to treat silkworm pupae with enzymes to obtain an active peptide enrichment, which is then mixed evenly with a pre-prepared mask base (such as a hydrogel solution or essence) before being packaged. In terms of product form, common forms include liquid essence soaked in non-woven fabric, and freeze-dried masks where the mask liquid is freeze-dried.

[0004] However, each of the aforementioned existing product formats has its own shortcomings. For liquid masks, the stability of active peptides is limited when stored in an aqueous environment for extended periods, making them prone to oxidation or degradation, leading to a decrease in efficacy within their shelf life. Furthermore, to ensure a certain shelf life, liquid products typically require the addition of various preservatives and stabilizers, which may increase the risk of irritation for some users with sensitive skin. For freeze-dried masks, rehydration is necessary before use, but existing freeze-dried masks mostly use non-woven fabric as a carrier to absorb the freeze-dried essence. After rehydration, the active ingredients dissolve rapidly with the water, limiting their retention time and sustained effectiveness on the skin surface.

[0005] Furthermore, in terms of mask base selection, commonly used hydrogel bases have limited ability to retain active ingredients. During application, active ingredients rapidly diffuse with the migration of water within the gel, resulting in the release of a large amount of active substances in a short period, making it difficult to maintain an effective concentration on the skin surface for a prolonged time. These issues restrict the full realization of the efficacy of silkworm pupae active peptides in mask products. Summary of the Invention

[0006] The purpose of this invention is to address the problems existing in the prior art by providing a composite mask matrix of active ingredients from silkworm pupae and its preparation method.

[0007] To achieve the above objectives, the present invention provides a composite mask matrix containing active ingredients of silkworm pupae, comprising the following components in parts by weight: 1-8 parts of active peptide extract of silkworm pupae, 5-20 parts of polyvinyl alcohol, 2-10 parts of sodium alginate, 1-6 parts of carboxymethyl chitosan, 5-15 parts of glycerin, 0.1-1 part of sodium hyaluronate, 0.5-3 parts of gluconolactone, 0.5-3 parts of calcium citrate, and 40-80 parts of water.

[0008] In some optional embodiments, the preparation method of the *Bombyx mori* active peptide extract includes: The silkworm, water, and complex protease were mixed and enzymatically hydrolyzed. After enzyme inactivation, the hydrolysate was obtained. The enzymatic hydrolysate was sequentially passed through an ultrafiltration membrane and a nanofiltration membrane for membrane separation. The nanofiltration retentate was collected and dried to obtain the active peptide extract of *Bombyx mori*.

[0009] In some optional embodiments, the silkworms are pretreated before use. The pretreatment includes: washing, sterilizing, drying, crushing, and sieving the silkworms in sequence. The sterilization temperature is 115-125℃, and the time is 3-7 seconds; the drying temperature is -40 to -50℃, the vacuum degree is 5-15 Pa, and the moisture content is ≤8%; the sieve mesh size is 50-150 mesh.

[0010] In an optional embodiment, the mixing includes: mixing silkworm pupae with water, then adjusting the pH to the desired range with a sodium hydroxide solution with a concentration of 0.05-0.15 mol / L, and then adding a complex protease for enzymatic hydrolysis.

[0011] In some optional embodiments, the mass ratio of the silkworm pupae to water is 1:(10-20); the amount of the compound protease added accounts for 0.5-2.5% of the mass of the silkworm pupae; the compound protease includes neutral protease and papain, with a mass ratio of (1-2):1; the enzymatic hydrolysis is performed at a pH of 6.5-8.0, a temperature of 35-55℃, and a time of 2-6 hours; the enzyme inactivation temperature is 80-100℃, and the time is 10-20 minutes.

[0012] In some optional embodiments, the enzymatic hydrolysate is centrifuged at 3500-4500 r / min for 15-25 min, the supernatant is collected, and the supernatant is sequentially passed through an ultrafiltration membrane and a nanofiltration membrane for membrane separation. The ultrafiltration membrane has a molecular weight cutoff of 80-120 kDa; the nanofiltration membrane has a molecular weight cutoff of 1-3 kDa.

[0013] In some alternative embodiments, the drying temperature is -40 to -50°C, the vacuum degree is 5-15 Pa, and the time is 12-36 h.

[0014] In some alternative embodiments, the polyvinyl alcohol has a degree of alcoholysis of 87-89% and a degree of polymerization of 1700-2400.

[0015] In some alternative embodiments, the carboxymethyl chitosan has a degree of substitution of 0.8-1.2 and a molecular weight of 50-200 kDa.

[0016] In some alternative embodiments, the sodium hyaluronate has a molecular weight of 50-150 kDa.

[0017] This invention also provides a method for preparing a composite mask matrix containing active ingredients from silkworm pupae, comprising the following steps: S1. Mix polyvinyl alcohol, sodium alginate, carboxymethyl chitosan, glycerin, sodium hyaluronate, silkworm active peptide extract and water to obtain a drug-loaded mixture; S2. Mix the drug-loaded mixture with gluconolactone and calcium citrate, and then gel the mixture to obtain a gel product; S3. The gel product is freeze-dried and freeze-dried sequentially to obtain the composite mask matrix of the active ingredients of silkworm.

[0018] In some optional embodiments, in S1, the mixing includes: adding polyvinyl alcohol to water and stirring to dissolve it in a water bath at 80-95°C to obtain a polyvinyl alcohol solution; adding sodium alginate and carboxymethyl chitosan to water and stirring to dissolve them in a water bath at 40-60°C to obtain a polysaccharide solution; mixing the polyvinyl alcohol solution and the polysaccharide solution, adding glycerol and sodium hyaluronate, and stirring until homogeneous to obtain a mixed solution; dissolving the active peptide extract of *Bombyx mori* in water, adding it to the mixed solution, and stirring until homogeneous to obtain a drug-loaded mixture.

[0019] In some optional embodiments, in S2, gluconolactone and calcium citrate are added to the drug-loaded mixture, stirred evenly, and then injected into a mold for gelation. The gelation temperature is 20-30°C, and the time is 24-48 hours. During this process, gluconolactone slowly hydrolyzes to generate gluconic acid, lowering the pH of the system; under acidic conditions, calcium citrate gradually dissolves and continuously and uniformly releases calcium ions; calcium ions undergo ionic cross-linking reactions with guluronic acid units on the sodium alginate molecular chain to form a three-dimensional calcium alginate network; polyvinyl alcohol molecular chains form physically cross-linked regions through hydrogen bonding, and carboxymethyl chitosan molecular chains participate in network construction through electrostatic attraction and hydrogen bonding. Together, the three form an interpenetrating polymer network structure.

[0020] In some optional embodiments, in S3, the freezing temperature is -20 to -40°C, and the time is 12-24 hours; the cooling rate of the freeze-drying is 0.5-2°C / min; the vacuum degree of the freeze-drying is 5-20 Pa, and the time is 24-48 hours.

[0021] Compared with the prior art, the present invention has the following beneficial effects: (1) In this invention, polyvinyl alcohol, sodium alginate, and carboxymethyl chitosan are used as gel backbone materials. The three materials form an interpenetrating polymer network structure through synergistic effects of hydrogen bonding, electrostatics, and ionic crosslinking. The active peptide extract of silkworm pupae is introduced simultaneously during the formation of this network and loaded into the network through hydrogen bonding, electrostatic adsorption, and physical encapsulation. This integrated construction method enables multiple intermolecular interactions between the active ingredients and the gel network.

[0022] (2) This invention uses gluconolactone and calcium citrate as the crosslinking system. Gluconolactone slowly hydrolyzes to generate gluconic acid, causing the pH of the system to gradually decrease; calcium citrate continuously and uniformly releases calcium ions under acidic conditions; the calcium ions undergo an ionic crosslinking reaction with the guluronic acid units on the sodium alginate molecular chain to form a three-dimensional calcium alginate network. This crosslinking system avoids the problems of excessively rapid local crosslinking and uneven crosslinking that are easily caused by directly adding soluble calcium salts.

[0023] (3) The present invention uses a freeze-drying process to process the gel product. During the freezing process, the water in the system forms ice crystals. After freeze-drying, the ice crystals sublimate and form a three-dimensional porous network structure in the matrix, so that the freeze-dried mask matrix has good rehydration properties.

[0024] (4) In this invention, the active peptide extract of silkworm is loaded into an interpenetrating polymer network through multiple intermolecular interactions. This network structure has a certain physical barrier effect on the diffusion of active peptides, which is beneficial to delaying the release rate of active peptides.

[0025] (5) All components of this invention are raw materials commonly used in the cosmetics industry or permitted for use in the food industry, and do not contain toxic or harmful substances. No organic solvents need to be added during the preparation process, and the safety is good. In addition, the dissolution, mixing, gelation, freeze-drying and other operations in the preparation process of this invention are all mature unit operations, which are easy to scale up for industrial production. Attached Figure Description

[0026] Figure 1 This is a comparison chart of the cumulative release rate of silkworm active peptides in the mask matrix obtained in Examples 1-3 and Comparative Examples 1-3 of the present invention. Detailed Implementation

[0027] The following embodiments are provided to better understand the present invention and are not limited to the described embodiments. They do not constitute a limitation on the content and scope of protection of the present invention. Any product that is the same as or similar to the present invention, derived by any person under the guidance of the present invention or by combining the features of the present invention with other prior art, falls within the protection scope of the present invention.

[0028] For experiments not specifically described in the examples, the procedures or conditions should be followed according to the conventional experimental procedures described in the literature in this field. Reagents or instruments whose manufacturers are not specified are all commercially available products.

[0029] In the following embodiments and comparative examples of the present invention, the silkworms were provided by Sichuan Derenyuan Agricultural Technology Co., Ltd., and were high-quality silkworms ("Lezhi silkworms") obtained by standardized and large-scale artificial inoculation with Beauveria bassiana, which met the "three no's and one complete" (no sulfur processing, no aflatoxin pollution, no pollution and full traceability) quality certification.

[0030] In the following examples and comparative examples of the present invention, neutral protease (enzyme activity ≥100000U / g) and papain (enzyme activity ≥50000U / g) were purchased from Novozymes.

[0031] In the following examples and comparative examples of the present invention, the degree of alcoholysis of polyvinyl alcohol is 88% and the degree of polymerization is 2000; the viscosity of sodium alginate is 200-400 mPa·s; the degree of substitution of carboxymethyl chitosan is 1.0 and the molecular weight is 100 kDa; and the molecular weight of sodium hyaluronate is 80 kDa.

[0032] Example 1 This embodiment provides a method for preparing a composite mask matrix containing active ingredients from silkworm pupae, comprising the following steps: The silkworm pupae were thoroughly cleaned with deionized water. They were then sterilized at 121°C for 5 seconds using a high-temperature instantaneous sterilizer. Next, the pupae were placed in a vacuum freeze dryer and dried at -45°C and a vacuum of 10 Pa until the moisture content was ≤8%. The dried pupae were then pulverized using a pulverizer and passed through a 100-mesh sieve to obtain silkworm pupae powder.

[0033] Take 100g of silkworm powder and add 1500g of deionized water, stirring to disperse. Adjust the pH to 7.5 with 0.1mol / L sodium hydroxide solution. Add 1.5g of complex protease (1.0g neutral protease + 0.5g papain), and incubate at 45℃ in a water bath for 4 hours. After enzymatic hydrolysis, heat to 90℃ to inactivate the enzyme for 15 minutes. Centrifuge the hydrolysate at 4000r / min for 20 minutes and collect the supernatant.

[0034] The supernatant was first ultrafiltered through an ultrafiltration membrane with a molecular weight cutoff of 100 kDa, and the permeate was collected. Then, the permeate was concentrated by nanofiltration through a nanofiltration membrane with a molecular weight cutoff of 2 kDa, and the retentate was collected. The retentate was freeze-dried at -45°C and a vacuum of 10 Pa for 24 h to obtain the active peptide extract of *Bombyx mori*.

[0035] Weigh each component according to the following mass proportions: 4 parts of silkworm active peptide extract, 12 parts of polyvinyl alcohol, 5 parts of sodium alginate, 3 parts of carboxymethyl chitosan, 8 parts of glycerin, 0.5 parts of sodium hyaluronate, 1.5 parts of gluconolactone, 1.2 parts of calcium citrate, and 64.8 parts of deionized water.

[0036] 12 parts of polyvinyl alcohol were added to 40 parts of deionized water and stirred in a 90°C water bath for 2 hours to obtain a polyvinyl alcohol solution. 5 parts of sodium alginate and 3 parts of carboxymethyl chitosan were added to 20 parts of deionized water and stirred in a 50°C water bath for 1 hour to obtain a polysaccharide solution. The polyvinyl alcohol solution and polysaccharide solution were mixed, and 8 parts of glycerol and 0.5 parts of sodium hyaluronate were added and stirred until homogeneous to obtain a mixed solution. 4 parts of *Bombyx mori* active peptide extract were dissolved in 4.8 parts of deionized water and added to the mixed solution, and stirred until homogeneous to obtain a drug-loaded mixture.

[0037] Add 1.5 parts gluconolactone and 1.2 parts calcium citrate to the drug-loaded mixture, stir well, and then pour into a polytetrafluoroethylene mold (2 mm thick). Allow it to stand at 25°C for 24 hours to gel, and obtain the gel product.

[0038] The gel product was frozen at -30℃ for 18 hours, and then freeze-dried under a vacuum of 10 Pa for 36 hours at a cooling rate of 1℃ / min to obtain the composite mask matrix of silkworm active ingredients.

[0039] Example 2 This embodiment provides a method for preparing a composite mask matrix containing active ingredients from silkworm pupae, comprising the following steps: The active peptide extract of *Bombyx mori* was prepared using the same method as in Example 1.

[0040] Weigh each component according to the following mass proportions: 6 parts of silkworm active peptide extract, 10 parts of polyvinyl alcohol, 8 parts of sodium alginate, 4 parts of carboxymethyl chitosan, 10 parts of glycerin, 0.8 parts of sodium hyaluronate, 2 parts of gluconolactone, 1.6 parts of calcium citrate, and 57.6 parts of deionized water.

[0041] 10 parts of polyvinyl alcohol were added to 35 parts of deionized water and stirred in an 85°C water bath for 2 hours to obtain a polyvinyl alcohol solution. 8 parts of sodium alginate and 4 parts of carboxymethyl chitosan were added to 20 parts of deionized water and stirred in a 55°C water bath for 1 hour to obtain a polysaccharide solution. The polyvinyl alcohol solution and polysaccharide solution were mixed, and 10 parts of glycerol and 0.8 parts of sodium hyaluronate were added, and the mixture was stirred until homogeneous to obtain a mixed solution. 6 parts of *Bombyx mori* active peptide extract were dissolved in 2.6 parts of deionized water and added to the mixed solution, and the mixture was stirred until homogeneous to obtain a drug-loaded mixture.

[0042] Add 2 parts gluconolactone and 1.6 parts calcium citrate to the drug-loaded mixture, stir well, and then pour into a polytetrafluoroethylene mold (2 mm thick). Allow it to stand at 25°C for 30 h to gel, and obtain the gel product.

[0043] The gel product was frozen at -35℃ for 20 hours, and then freeze-dried under a vacuum of 10 Pa for 40 hours at a cooling rate of 1℃ / min to obtain the composite mask matrix of silkworm active ingredients.

[0044] Example 3 This embodiment provides a method for preparing a composite mask matrix containing active ingredients from silkworm pupae, comprising the following steps: The active peptide extract of *Bombyx mori* was prepared using the same method as in Example 1.

[0045] Weigh each component according to the following mass proportions: 2 parts of silkworm active peptide extract, 15 parts of polyvinyl alcohol, 3 parts of sodium alginate, 2 parts of carboxymethyl chitosan, 6 parts of glycerin, 0.3 parts of sodium hyaluronate, 1 part of gluconolactone, 0.8 parts of calcium citrate, and 69.9 parts of deionized water.

[0046] 15 parts of polyvinyl alcohol were added to 45 parts of deionized water and stirred in a 90°C water bath for 2 hours to obtain a polyvinyl alcohol solution. 3 parts of sodium alginate and 2 parts of carboxymethyl chitosan were added to 20 parts of deionized water and stirred in a 50°C water bath for 1 hour to obtain a polysaccharide solution. The polyvinyl alcohol solution and polysaccharide solution were mixed, and 6 parts of glycerol and 0.3 parts of sodium hyaluronate were added and stirred until homogeneous to obtain a mixed solution. 2 parts of *Bombyx mori* active peptide extract were dissolved in 4.9 parts of deionized water and added to the mixed solution, and stirred until homogeneous to obtain a drug-loaded mixture.

[0047] Add 1 part gluconolactone and 0.8 parts calcium citrate to the drug-loaded mixture, stir well, and then pour into a polytetrafluoroethylene mold (2 mm thick). Allow it to stand at 25°C for 24 hours to gel, and obtain the gel product.

[0048] The gel product was frozen at -30℃ for 18 hours, and then freeze-dried under a vacuum of 10 Pa for 36 hours at a cooling rate of 1℃ / min to obtain the composite mask matrix of silkworm active ingredients.

[0049] Comparative Example 1 This comparative example provides a method for preparing a mask matrix, including the following steps: Weigh each component according to the following mass proportions: 12 parts polyvinyl alcohol, 5 parts sodium alginate, 3 parts carboxymethyl chitosan, 8 parts glycerol, 0.5 parts sodium hyaluronate, 1.5 parts gluconolactone, 1.2 parts calcium citrate, and 68.8 parts deionized water.

[0050] 12 parts of polyvinyl alcohol were added to 45 parts of deionized water and stirred in a 90°C water bath for 2 hours to obtain a polyvinyl alcohol solution. 5 parts of sodium alginate and 3 parts of carboxymethyl chitosan were added to 23.8 parts of deionized water and stirred in a 50°C water bath for 1 hour to obtain a polysaccharide solution. The polyvinyl alcohol solution and the polysaccharide solution were mixed, and 8 parts of glycerol and 0.5 parts of sodium hyaluronate were added. The mixture was stirred until homogeneous to obtain a mixed solution.

[0051] Add 1.5 parts gluconolactone and 1.2 parts calcium citrate to the mixed solution, stir well, and then pour into a polytetrafluoroethylene mold (2 mm thick). Allow to stand at 25°C for 24 h to gel, and obtain the gel product.

[0052] The gel product was frozen at -30℃ for 18 h, and then freeze-dried under a vacuum of 10 Pa for 36 h at a cooling rate of 1℃ / min to obtain the hydrogel matrix.

[0053] Four parts of the *Bombyx mori* active peptide extract obtained in Example 1 were dissolved in 50 parts of deionized water, and the hydrogel matrix was immersed in the solution for 24 hours. After removal, the surface was rinsed three times with deionized water, and then freeze-dried again at -30°C for 24 hours to obtain the mask matrix.

[0054] Comparative Example 2 This comparative example provides a method for preparing a mask matrix, including the following steps: The active peptide extract of *Bombyx mori* was prepared using the same method as in Example 1.

[0055] Weigh each component according to the following mass proportions: 4 parts of silkworm active peptide extract, 20 parts of polyvinyl alcohol, 8 parts of glycerin, 0.5 parts of sodium hyaluronate, and 67.5 parts of deionized water.

[0056] Add 20 parts of polyvinyl alcohol to 60 parts of deionized water and stir in a 90°C water bath for 2 hours to obtain a polyvinyl alcohol solution. Add 8 parts of glycerin and 0.5 parts of sodium hyaluronate and stir until homogeneous to obtain a mixed solution. Dissolve 4 parts of silkworm pupae active peptide extract in 7.5 parts of deionized water, add to the mixed solution, and stir until homogeneous to obtain a drug-loaded mixture.

[0057] The drug-loaded mixture was injected into a polytetrafluoroethylene mold (2 mm thick), frozen at -30°C for 18 h, and then freeze-dried under a vacuum of 10 Pa for 36 h at a cooling rate of 1°C / min to obtain the mask matrix.

[0058] Comparative Example 3 This comparative example uses the gel product prepared in Example 1 as the mask matrix.

[0059] Experimental Example 1 Take the mask matrix from Examples 1-3, weigh out W0, add 3 times its weight of deionized water, and take out samples at 5 min, 15 min, and 30 min after rehydration. After absorbing the surface moisture with filter paper, weigh out W. t Continue soaking until the sample mass no longer increases, then record the equilibrium rehydration rate. Rehydration rate (%) = (W t -W0) / W0×100%. Each sample was measured in triplicate, and the average value was taken.

[0060] In addition, the water content of the gel product of Comparative Example 3 was determined: water content (%) = (mass of water in the gel product / total mass of the gel product) × 100%.

[0061] The rehydration rate of the mask matrix in Examples 1-3 is shown in Table 1. The water content of the gel product in Comparative Example 3 was 64.8%.

[0062] Table 1. Results of the rehydration rate test of the mask matrix in Examples 1-3

[0063] As shown in Table 1, the porous network structure formed by the freeze-drying process can effectively improve the water absorption and retention capacity of the hydrogel matrix.

[0064] Experimental Example 2 The in vitro release behavior of *Bombyx mori* active peptides in the mask matrices obtained in Examples 1-3 and Comparative Examples 1-3 was determined using the Franz diffusion cell method. The release medium was phosphate-buffered saline (PBS, pH 5.5), the receiving cell volume was 6.5 mL, and the effective diffusion area was 1.77 cm². 2 The temperature was 32±0.5℃, and the stirring speed was 300r / min.

[0065] Each sample (containing an equal amount of *Bombyx mori* active peptide extract, with each sample equivalent to 10 mg of protein / peptide added to each chamber based on total protein / peptide content) was placed in the supply chamber of the diffusion cell. 1 mL of the receiving solution was collected at 0.5 h, 1 h, 2 h, 4 h, 6 h, 8 h, and 12 h, and an equal amount of fresh medium was added. The protein / peptide content in the receiving solution was determined using the BCA method (detection wavelength 562 nm), and the cumulative release rate was calculated. Each sample was measured in triplicate, and the average value was taken.

[0066] The cumulative release rate test results are shown in Table 2. Meanwhile, to more clearly and intuitively demonstrate the differences in release behavior among the groups, a comparison chart of the cumulative release rates of *Bombyx mori* active peptides in the mask matrices obtained in Examples 1-3 and Comparative Examples 1-3 was plotted, as shown below. Figure 1 As shown.

[0067] Table 2. Cumulative Release Rate Test Results (%)

[0068] The above results indicate that, compared with the comparative examples, the mask matrices of Examples 1-3 exhibit a good sustained-release effect on the active peptides of *Bombyx mori*.

[0069] Experimental Example 3 Thirty healthy female volunteers (aged 25-45 years) were randomly divided into 6 groups of 5 each, using the mask bases of Examples 1-3 and Comparative Examples 1-3 respectively. Usage: Take one sheet (approximately 2g) of the mask base from Examples 1-3 or Comparative Examples 1-2, add 6mL of deionized water, let stand for 3 minutes to fully rehydrate, then apply to the face and remove after 20 minutes. Comparative Example 3 was a wet gel product; 2g was directly applied to the face and removed after 20 minutes.

[0070] The evaluation indicators included: (1) Adhesion (1-5 points, with 5 points being the best; the evaluation criteria were the ratio of the area of ​​the matrix to the skin surface and whether slippage or detachment occurred during use); (2) Skin comfort (1-5 points; the evaluation criteria were whether there was stinging, itching, and overall comfort); and (3) Skin hydration after use (1-5 points; the evaluation criteria were the softness and smoothness of the skin after use). Each volunteer scored independently on each indicator, and the final score for each group was the arithmetic mean of the scores from the five volunteers.

[0071] The user experience evaluation results are shown in Table 3.

[0072] Table 3 User Experience Evaluation Results

[0073] As shown in Table 3, the mask bases of Examples 1-3 are superior to the comparative examples in terms of adhesion, skin comfort, and moisturizing properties.

[0074] Experiment Example 4 Thirty-six healthy female volunteers (aged 25-45 years) were randomly divided into 6 groups of 6, using the mask bases of Examples 1-3 and Comparative Examples 1-3, respectively. In a constant temperature and humidity environment (temperature 22±1℃, relative humidity 50±5%), the subjects sat quietly for 30 minutes after cleansing their faces with water. The stratum corneum moisture content of the skin on the cheekbone area was measured using a skin moisture meter and recorded as the initial value. The rehydrated mask base was applied to the face and removed after 20 minutes. The stratum corneum moisture content of the same area was measured immediately after removal, at 1 hour, 2 hours, and 4 hours. Measurements were taken three times at each time point, and the average value was used. The rate of change of skin moisture content relative to the initial value was calculated using the following formula: Rate of change (%) = (Measured value - Initial value) / Initial value × 100%.

[0075] The results of the moisturizing effect test are shown in Table 4.

[0076] Table 4. Results of Moisturizing Effect Test (%)

[0077] As shown in Table 4, the mask bases of Examples 1-3 have good moisturizing effects, which are significantly better than those of Comparative Examples 1-3.

[0078] Experimental Example 5 Thirty healthy volunteers (15 males and 15 females, aged 18-60 years) were selected for a closed patch test. A 1cm × 1cm piece of the rehydrated mask matrix obtained in Example 1 was cut and placed in a patch applicator, then applied to the flexor surface of the volunteer's forearm. A 1cm × 1cm piece of non-woven fabric soaked in deionized water served as a blank control. The patch was secured with non-irritating adhesive tape. After 48 hours, the patch applicator was removed, and skin reactions were observed at 0.5h, 24h, and 48h after removal. Skin reactions were graded according to the skin reaction grading standards in the *Cosmetic Safety Technical Specifications* (2015 edition): Grade 0: no reaction; Grade 1: slight erythema; Grade 2: erythema, infiltration, papules; Grade 3: erythema, edema, papules, vesicles; Grade 4: severe edema, bullae.

[0079] Test results showed that, after 0.5h, 24h, and 48h following patch removal, no irritation or allergic reactions such as erythema, edema, itching, or burning occurred at the sites where the mask matrix of Example 1 was applied in any of the 30 volunteers. The skin reaction grade was 0 (negative). No reaction was observed at the blank control sites either.

[0080] In summary, this invention uses silkworm pupae active peptide extract as the active ingredient and polyvinyl alcohol, sodium alginate, and carboxymethyl chitosan as gel backbone materials. The sodium alginate crosslinks through a glucono-delta-lactone and calcium citrate crosslinking system, synergistically with the physical crosslinking of polyvinyl alcohol and the hydrogen bonding / electrostatic interactions of carboxymethyl chitosan, forming an interpenetrating polymer network structure. This is then combined with a freeze-drying process to prepare the mask matrix. This mask matrix achieves the integrated construction of silkworm pupae active peptides and a gel network, exhibits excellent rehydration properties, and can delay the release rate of the active peptides. The raw materials of this invention are stable, the preparation process is mature, and the safety is good, making it suitable for widespread application in the cosmetics field.

[0081] Finally, it should be noted that the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of this invention.

Claims

1. A composite mask matrix containing active ingredients from silkworm pupae, characterized in that, The components include the following parts by mass: 1-8 parts of active peptide extract of silkworm pupae, 5-20 parts of polyvinyl alcohol, 2-10 parts of sodium alginate, 1-6 parts of carboxymethyl chitosan, 5-15 parts of glycerin, 0.1-1 part of sodium hyaluronate, 0.5-3 parts of gluconolactone, 0.5-3 parts of calcium citrate, and 40-80 parts of water.

2. The composite mask matrix of silkworm active ingredients according to claim 1, characterized in that, The preparation method of the *Bombyx mori* active peptide extract includes: The silkworm, water, and complex protease were mixed and enzymatically hydrolyzed. After enzyme inactivation, the hydrolysate was obtained. The enzymatic hydrolysate was sequentially passed through an ultrafiltration membrane and a nanofiltration membrane for membrane separation. The nanofiltration retentate was collected and dried to obtain the active peptide extract of *Bombyx mori*.

3. The composite mask matrix of silkworm active ingredients according to claim 2, characterized in that, The mass ratio of the silkworm pupae to water is 1:(10-20); the amount of the compound protease added accounts for 0.5-2.5% of the mass of the silkworm pupae; the compound protease includes neutral protease and papain, and the mass ratio of the two is (1-2):1; the pH of the enzymatic hydrolysis is 6.5-8.0, the temperature is 35-55℃, and the time is 2-6h; the enzyme inactivation temperature is 80-100℃, and the time is 10-20min.

4. The composite mask matrix of silkworm active ingredients according to claim 2, characterized in that, The ultrafiltration membrane has a molecular weight cutoff of 80-120 kDa; the nanofiltration membrane has a molecular weight cutoff of 1-3 kDa.

5. The composite mask matrix of silkworm active ingredients according to claim 1, characterized in that, The degree of alcoholysis of the polyvinyl alcohol is 87-89%, and the degree of polymerization is 1700-2400.

6. The composite mask matrix of silkworm active ingredients according to claim 1, characterized in that, The degree of substitution of the carboxymethyl chitosan is 0.8-1.2, and the molecular weight is 50-200 kDa.

7. The composite mask matrix of silkworm active ingredients according to claim 1, characterized in that, The molecular weight of the sodium hyaluronate is 50-150 kDa.

8. A method for preparing a composite mask matrix containing active ingredients of silkworm pupae as described in any one of claims 1-7, characterized in that, Includes the following steps: S1. Mix polyvinyl alcohol, sodium alginate, carboxymethyl chitosan, glycerin, sodium hyaluronate, silkworm active peptide extract and water to obtain a drug-loaded mixture; S2. Mix the drug-loaded mixture with gluconolactone and calcium citrate, and then gel the mixture to obtain a gel product; S3. The gel product is freeze-dried and freeze-dried sequentially to obtain the composite mask matrix of the active ingredients of silkworm.

9. The preparation method according to claim 8, characterized in that, In S2, the gelation temperature is 20-30℃ and the time is 24-48h.

10. The preparation method according to claim 8, characterized in that, In S3, the freezing temperature is -20 to -40°C, and the time is 12-24 hours; the freeze-drying vacuum degree is 5-20 Pa, and the time is 24-48 hours.

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