Freeze-dried eye mask and preparation method thereof

Abstract

The invention provides a freeze-dried eye mask and a preparation method thereof, and the freeze-dried eye mask is prepared from the following components in parts by weight: 0.05 to 0.25 part of a glycoside nonionic surfactant, 0.03 to 0.25 part of phosphatidylcholine, 0.01 to 0.04 part of cholesterols, 0.03 to 0.2 part of a mould / saccharomycetes fermentation extraction product, 0.5 to 0.8 part of a humectant, 0.35 to 0.85 part of a skin conditioner, 0.01 to 0.015 part of a thickening agent, 0.25 to 0.4 part of an antiseptic bacteriostatic agent and 0.001 to 0.004 part of an acid-base regulator. Compared with the prior art, the freeze-dried eye mask disclosed by the invention has the advantages that components such as a skin conditioner can be entrapped in vesicles, permeation and absorption of functional components in eye skin can be improved, and the effects of removing wrinkles, whitening and the like are enhanced.

Description

Technical Field

[0001] This invention belongs to the field of cosmetic technology, specifically a freeze-dried eye mask and its preparation method. Background Technology

[0002] The skin around the eyes is the most prone to problems and aging, a consequence of its unique physiological characteristics. The epidermis and dermis around the eyes are only 0.25-0.55 millimeters thick, making it the thinnest skin on the entire body and thus more susceptible to external damage. There are virtually no sebaceous or sweat glands in the subcutaneous tissue around the eyes, making the thin skin very prone to dryness and dehydration. The skin around the eyes is sensitive and fragile, with extremely fine capillaries and very little collagen and elastin, lacking muscle support, making it prone to wrinkles, dark circles, and eye bags. The eyes blink 10,000 times a day during normal work, placing a heavy workload on the skin around the eyes and causing fatigue.

[0003] Eye masks are typically applied to the eye area to quickly replenish moisture, relieve fatigue, and rapidly reduce puffiness and dark circles, making them a popular eye care method. Currently, common eye masks are mainly divided into non-woven fabric eye masks, gel eye masks, and sleeping eye masks. Because freeze-drying technology removes moisture through low-temperature freeze-drying, effectively avoiding the destruction of active ingredients by high temperatures, freeze-dried eye masks have become a highly sought-after eye mask product in recent years. However, the absorption of active ingredients in existing freeze-dried eye masks is relatively poor, failing to effectively exert the effects of these ingredients. Summary of the Invention

[0004] Therefore, the purpose of this invention is to provide a freeze-dried eye mask and a method for preparing the same.

[0005] This invention provides a freeze-dried eye mask, which, by weight, comprises the following components:

[0006]

[0007] Compared with existing technologies, this invention uses glycoside nonionic surfactants, phosphatidylcholine derivatives, cholesterol derivatives, and mold / yeast fermentation extracts as the main components to form a microvesicle structure, encapsulating skin conditioning agents in the vesicles. Then, auxiliary ingredients such as moisturizers, thickeners, preservatives, antibacterial agents, and pH regulators are added, which can improve the penetration and absorption of active ingredients in the skin around the eyes and enhance their wrinkle-reducing, whitening, and other effects.

[0008] In one embodiment, the glycoside nonionic surfactant includes one or two of C12-16 alkyl glucoside, C8-C14 alkyl glucoside, lauryl glucoside, cocoyl glucoside, hexadecyl glucoside, decyl glucoside, and isostearyl glucoside.

[0009] In one embodiment, the phosphatidylcholine class includes one or both of phosphatidylcholine and hydrogenated phosphatidylcholine.

[0010] In one embodiment, the cholesterol class includes one or two of cholesterol, dihydrocholesterol, cholesterol chloride, cholesterol polyether-5, cholesterol butyrate, cholesterol succinate, cholesterol nonanoate, cholesterol oleate, cholesterol stearate, and cholesterol lanolinate.

[0011] In one embodiment, the mold / yeast fermentation extract includes one or more of the following: *Brucea buddingis* fermentation product, *Rhizopus oryzae* extract, *Endospora* fermentation product filtrate, *Aspergillus* fermentation product, *Aspergillus* / glucose / soybean / starch fermentation product filtrate, *Pichia pastoris* fermentation lysate filtrate, *Galactomyces*-like fungi fermentation product filtrate, yeast fermentation product extract, yeast fermentation product, yeast fermentation product filtrate, yeast fermentation lysate filtrate, yeast lysate, yeast lysate extract, yeast extract, and hydrolyzed yeast extract.

[0012] In one embodiment, the freeze-dried eye mask comprises 0.05-0.25 parts lauryl glucoside, 0.03-0.25 parts phosphatidylcholine, 0.01-0.04 parts cholesterol, 0.02-0.1 parts Mucor extract, and 0.01-0.1 parts Aspergillus fermentation product.

[0013] In one embodiment, the moisturizer includes one or more of glycerin, 1,3-propanediol, sodium hyaluronate, trehalose, and caprylyl glycol.

[0014] In one embodiment, the skin conditioning agent comprises one or more of the following: soluble collagen, niacinamide, ceramide, hydroxypropyl tetrahydropyrantriol, *Sparganium stoloniferum* extract, *Artemisia umbellatus* extract, *Adenophora stricta* extract, *Nymphaea granatum* extract, benzoin extract, *Ganoderma lucidum* extract, *Witch hazel* bark / twig extract, cardamom fruit extract, tea extract, daisy flower extract, *Lophatherum gracile* leaf extract, hyacinth extract, *Phellodendron amurense* bark extract, turmeric rhizome extract, coltsfoot flower extract, *Trifolium repens* seed extract, litchi seed extract, *Salvia miltiorrhiza* extract, and *Citrus medica* peel extract.

[0015] In one embodiment, the thickener includes one or more of hydroxyethyl cellulose, xanthan gum, carbomer, and maltodextrin.

[0016] On the other hand, the present invention provides a method for preparing the freeze-dried eye mask as described above, characterized in that it includes:

[0017] (1) Take glycoside nonionic surfactants, phosphatidylcholine, cholesterol and mold / yeast fermentation extracts, dissolve them in water and mix them evenly, filter them to obtain solution A;

[0018] (2) Take moisturizer, skin conditioner, thickener, preservative and antibacterial agent and pH regulator, dissolve in water and filter to obtain solution B;

[0019] (3) Mix solution A and solution B and stir evenly. Dispense into freeze-drying molds and freeze quickly to -55°C. Then gradually heat to -25°C, 0°C and 35°C for sublimation drying.

[0020] (4) Remove the freeze-dried eye membrane from the freeze-drying mold, put it into a packaging box and a sealed bag, and store it in a sealed container. Attached Figure Description

[0021] Figure 1 These are electron micrographs of vesicles from Examples 1-4 of the present invention. Detailed Implementation

[0022] To further understand the present invention, preferred embodiments of the present invention are described below in conjunction with examples. However, it should be understood that these descriptions are only for further illustrating the features and advantages of the present invention, and not for limiting the scope of the claims of the present invention.

[0023] To enhance the penetration and absorption of active ingredients, this invention uses glycoside nonionic surfactants, phosphatidylcholine derivatives, cholesterol, and mold / yeast fermentation extracts as the main components to form a microvesicle structure, encapsulating skin conditioning agents within the vesicles. Then, auxiliary ingredients such as moisturizers, thickeners, preservatives, antibacterial agents, and pH regulators are added, and the mixture is freeze-dried to form a freeze-dried eye mask.

[0024] Specifically, the present invention provides a freeze-dried eye mask, which, by weight, comprises the following components:

[0025]

[0026] In this invention, glycosides, nonionic surfactants, and phosphatidylcholine derivatives form the membrane structure of vesicles. Cholesterols are inserted into the membrane structure to provide stability. The fermentation extracts from molds / yeasts contain various biological enzymes that can embed themselves into the vesicle membrane structure. When the vesicles come into contact with the skin, the enzymes can create openings in the skin cell membrane, making it easier for the vesicles to enter the skin cells. Therefore, the freeze-dried eye mask of this invention can encapsulate skin conditioning agents and other ingredients within vesicles, improving the penetration and absorption of active ingredients in the skin around the eyes and enhancing their anti-wrinkle and whitening effects.

[0027] Specifically, glycoside nonionic surfactants include one or two of the following: C12-16 alkyl glucoside, C8-C14 alkyl glucoside, lauryl glucoside, cocoyl glucoside, hexadecyl glucoside, decyl glucoside, and isostearyl glucoside.

[0028] Phosphatidylcholine class includes one or both of phosphatidylcholine and hydrogenated phosphatidylcholine.

[0029] Cholesterols include one or two of the following: cholesterol, dihydrocholesterol, cholesterol chloride, cholesterol polyether-5, cholesterol butyrate, cholesterol succinate, cholesterol nonanoate, cholesterol oleate, cholesterol stearate, and cholesterol lanolinate.

[0030] The mold / yeast fermentation extracts include one or more of the following: *Brucea buddingis* fermentation product, *Mucor* extract, *Endospora* fermentation product filtrate, *Aspergillus* fermentation product, *Aspergillus* / glucose / soybean / starch fermentation product filtrate, *Pichia pastoris* fermentation lysate filtrate, *Galactomyces* fermentation product filtrate, yeast fermentation product extract, yeast fermentation product, yeast fermentation product filtrate, yeast fermentation lysate filtrate, yeast lysate, yeast lysate extract, yeast extract, and hydrolyzed yeast extract.

[0031] Moisturizers include one or more of glycerin, 1,3-propanediol, sodium hyaluronate, trehalose, and caprylyl glycol.

[0032] Skin conditioning agents include one or more of the following: soluble collagen, niacinamide, ceramide, hydroxypropyl tetrahydropyrantriol, *Sparganium stoloniferum* extract, *Artemisia umbellatus* extract, *Adenophora stricta* extract, *Nymphaea granatum* extract, benzoin extract, *Ganoderma lucidum* extract, *Witch hazel* bark / twig extract, cardamom fruit extract, tea leaf extract, daisy flower extract, *Lophatherum gracile* leaf extract, hyacinth extract, *Phellodendron amurense* bark extract, turmeric rhizome extract, coltsfoot flower extract, *Citrus quinquefolia* seed extract, litchi seed extract, *Salvia miltiorrhiza* extract, and *Mandarin orange* peel extract.

[0033] Thickeners include one or more of hydroxyethyl cellulose, xanthan gum, carbomer, and maltodextrin.

[0034] Preservatives and antibacterial agents include one or more of 1,2-hexanediol, butylene glycol, 1,2-pentanediol, and ethylhexylglycerin.

[0035] Acid-base regulators include one or more of citric acid, sodium citrate, ascorbic acid, disodium hydrogen phosphate, sodium dihydrogen phosphate, and triethanolamine.

[0036] In this invention, unless otherwise explicitly stated, percentages and contents are all by mass. Unless otherwise specified, the experimental methods used are conventional methods, and the materials and reagents used are commercially available.

[0037] The present invention will be illustrated by the following specific embodiments.

[0038] Lauryl glucoside is sourced from Guangzhou Maimingshi Biotechnology Co., Ltd., with a purity of >95%.

[0039] C12-16 alkyl glucoside is from Guangzhou Maimingshi Biotechnology Co., Ltd., with a purity of >95%.

[0040] The cocoyl glucoside is from Guangzhou Maimingshi Biotechnology Co., Ltd., with a purity of >95%.

[0041] Phosphatidylcholine glycoside is from Guangzhou Maimingshi Biotechnology Co., Ltd., with a purity of >95%.

[0042] Hydrogenated phosphatidylcholine is from Guangzhou Maimingshi Biotechnology Co., Ltd., with a purity of >95%.

[0043] Cholesterol is sourced from Guangzhou Guangyu Biotechnology Co., Ltd., with a purity of >99%.

[0044] Dihydrocholesterol is from Sigma-Aldrich, with a strength of >95%;

[0045] Cholesterol oleate is from Sigma-Aldrich, with a strength of >95%;

[0046] The extract of *Mucor mellea* is from Guangzhou Maimingshi Biotechnology Co., Ltd., with a concentration >50%.

[0047] The Aspergillus fermentation product is from Guangzhou Maimingshi Biotechnology Co., Ltd., with a specification of >50%.

[0048] The fermentation product of *Bacillus buddingus* was obtained from Guangzhou Maimingshi Biotechnology Co., Ltd., with a specification of >50%.

[0049] The fermentation product filtrate of *Endospora* was obtained from Guangzhou Maimingshi Biotechnology Co., Ltd., with a purity of >50%.

[0050] The yeast fermentation product filtrate was obtained from Guangzhou Maimingshi Biotechnology Co., Ltd., with a purity of >50%.

[0051] The glycerin is from Hunan Ercon Pharmaceutical Co., Ltd., and its purity is >99%.

[0052] Trehalose is sourced from Nanjing Songguan Biotechnology Co., Ltd., with a purity of 99%.

[0053] Sodium hyaluronate is from Bloomage Technology Co., Ltd., with a specification of 100-200kDa; 1,3-propanediol is from Guangzhou Baiyu Biotechnology Co., Ltd., with a specification of 99%.

[0054] Hydroxyethyl cellulose is from Dow Chemical Company, specification QP4400H;

[0055] The maltodextrin is from Shandong Xiwang Sugar Industry Co., Ltd., and is of pharmaceutical grade.

[0056] Xanthan gum is from Ordos Zhongxuan Biochemical Co., Ltd., and is of pharmaceutical excipient grade; 1,2-pentanediol is from Guangzhou Baiyu Biotechnology Co., Ltd., and is of 99% purity.

[0057] Ethylhexylglycerol is from Guangzhou Baiyu Biotechnology Co., Ltd., with a purity of 99%; 1,2-hexanediol is from Guangzhou Baiyu Biotechnology Co., Ltd., with a purity of 99%.

[0058] The soluble collagen is from Zhejiang Zhuji Juyuan Biotechnology Co., Ltd., with a purity of 99%.

[0059] The nicotinamide is from Hubei Jusheng Technology Co., Ltd., and the purity is 99%.

[0060] The ceramide is from Guangzhou Baiyu Biotechnology Co., Ltd., and its purity is 99%.

[0061] Hydroxypropyltetrahydropyrantriol is from Sichuan Jisheng Biomedical Co., Ltd., with a purity of 99%.

[0062] The white crane Ganoderma extract is from Guangzhou Baoyi Biotechnology Co., Ltd., with a specification of 30:1.

[0063] Turmeric rhizome extract is from Guangzhou Baoyi Biotechnology Co., Ltd., with a specification of 30:1;

[0064] The litchi seed extract is from Guangzhou Baoyi Biotechnology Co., Ltd., with a ratio of 30:1.

[0065] The extract of *Trisporium chinense* is from Guangzhou Baoyi Biotechnology Co., Ltd., with a specification of 30:1.

[0066] The extracts from North American witch hazel bark / twigs are from Guangzhou Baoyi Biotechnology Co., Ltd., with a ratio of 30:1; the extracts from Quinoa seeds are from Guangzhou Baoyi Biotechnology Co., Ltd., with a ratio of 30:1.

[0067] Egyptian blue water lily extract is from Guangzhou Baoyi Biotechnology Co., Ltd., with a specification of 30:1;

[0068] Daisy flower extract is from Guangzhou Baoyi Biotechnology Co., Ltd., with a ratio of 30:1.

[0069] The extract of Adenophora stricta comes from Guangzhou Baoyi Biotechnology Co., Ltd., with a specification of 30:1.

[0070] The extract from Phellodendron bark is from Guangzhou Baoyi Biotechnology Co., Ltd., with a ratio of 30:1.

[0071] Cardamom fruit extract is from Guangzhou Baoyi Biotechnology Co., Ltd., with a specification of 30:1;

[0072] The tea extract is from Guangzhou Baoyi Biotechnology Co., Ltd., with a ratio of 30:1.

[0073] The extract of Salvia miltiorrhiza from Europe is from Guangzhou Baoyi Biotechnology Co., Ltd., with a specification of 30:1.

[0074] Sodium dihydrogen phosphate is from Guangzhou Chemical Reagent Factory, 500g specification;

[0075] Sodium citrate is from Guangzhou Chemical Reagent Factory, 500g specification.

[0076] Examples 1-4

[0077] The components and their contents of the freeze-dried eye films of Examples 1-4 are shown in Table 1.

[0078] Table 1. Composition and content of freeze-dried eye masks in each embodiment.

[0079]

[0080]

[0081] The preparation process of the freeze-dried eye masks in Examples 1-4 is as follows:

[0082] (1) Take glycoside nonionic surfactants, phosphatidylcholine, cholesterol, and mold / yeast fermentation extracts, dissolve them in water and mix them evenly, then filter to obtain solution A. The total weight of glycoside nonionic surfactants, phosphatidylcholine, cholesterol, mold / yeast fermentation extracts, and water is 20 parts.

[0083] (2) Take the moisturizer, skin conditioner, thickener, preservative and antibacterial agent and pH adjuster, dissolve them in water and filter to obtain solution B. The total weight of the moisturizer, skin conditioner, thickener, preservative and antibacterial agent, pH adjuster and water is 80 parts.

[0084] (3) Mix solution A and solution B and stir evenly. Dispense into freeze-drying molds and freeze quickly to -55°C. Then gradually heat to -25°C, 0°C and 35°C for sublimation drying.

[0085] (4) Remove the freeze-dried eye membrane from the freeze-drying mold, put it into a packaging box and a sealed bag, and store it in a sealed container.

[0086] Comparative Example 1

[0087] This comparative example provides a freeze-dried eye mask, which differs from Example 1 in that only solution B is dispensed into a freeze-drying mold, rapidly frozen, and then sublimated and dried to obtain the freeze-dried eye mask.

[0088] Comparative Example 2

[0089] This comparative example provides a freeze-dried eye mask, which differs from Example 1 in that: Solution A only includes glycoside nonionic surfactants, phosphatidylcholine, and water, and the amounts of glycoside nonionic surfactants and phosphatidylcholine remain unchanged; the raw materials, amounts, and preparation methods of Solution B are the same as in Example 1.

[0090] Comparative Example 3

[0091] This comparative example provides a freeze-dried eye mask, which differs from Example 1 only in that: solution A includes glycoside nonionic surfactants, phosphatidylcholine, cholesterol and water, and the amounts of glycoside nonionic surfactants, phosphatidylcholine and cholesterol remain unchanged; the raw materials, amounts and preparation methods of solution B are the same as those in Example 1.

[0092] Comparative Example 4

[0093] This comparative example provides a freeze-dried eye mask, which differs from Example 1 only in that: Solution A includes glycoside nonionic surfactants, phosphatidylcholine, mold / yeast fermentation extract and water, and the amounts of glycoside nonionic surfactants, phosphatidylcholine and mold / yeast fermentation extract remain unchanged; the raw materials, amounts and preparation methods of Solution B are the same as those in Example 1.

[0094] Test Example 1

[0095] vesicle electron microscopy observation

[0096] Solution A from Examples 1-4 was dispensed into 3 ml glass vials, rapidly frozen to -55°C, and then subjected to vacuum freeze-drying to obtain vesicle lyophilized powder. 10 mg of the vesicle lyophilized powder was dispersed in 1 ml of pure water, and 10 μl of the liquid was added to the top of conductive double-sided tape mounted on an aluminum tube. The sample was air-dried for 2 hours and then plated with platinum. The sample was observed using a scanning electron microscope (XL30S FEG, Philips, Netherlands) under high vacuum conditions of 5–25 kV. Figure 1 As can be seen, solution A in Examples 1-4 formed spherical vesicles.

[0097] Test Example 2

[0098] Permeability test

[0099] Transdermal absorption was performed using the diffusion cell method according to GB / T 27818-2011 "In vitro test methods for skin absorption of chemicals", and the oligopeptide content in the transdermal liquid was determined by HPLC.

[0100] Test instruments:

[0101] Franz diffusion cell (diffusion area 4.52 cm²) 2 (Acceptance chamber area 13ml);

[0102] HH-2 constant temperature water bath, Changzhou Aohua Instrument Co., Ltd.

[0103] Vortex oscillator, VXMNFS, Shanghai Jianrong Industrial Co., Ltd.;

[0104] High performance liquid chromatography, LC-16, Shimadzu Instruments (Suzhou) Co., Ltd.; UV-Vis detector, SPD-16, Shimadzu Instruments; Column, WondaSil C18 Superb 5μm, Shimadzu Instruments.

[0105] Test method:

[0106] Immediately after euthanizing piglets weighing approximately 7 kg, the abdominal skin and hair were shaved off using an electric razor. The skin at the shaved area was peeled off, and subcutaneous tissue was removed. The skin thickness was 0.98–1.02 mm. The skin was rinsed thoroughly with 0.01 M (pH = 7.4) PBS buffer, soaked in PBS buffer for 30 min, removed, and blotted dry with filter paper. The pigskin was sandwiched between the supply and receiving cells of the diffusion cell, with the outer layer of the pigskin facing the supply cell. The water bath temperature was set to 32 ± 1 °C, based on human skin temperature, and the magnetic stirring speed was 100 rpm. Pre-warmed PBS solution at 32 ± 1 °C was added to the receiving cell, and air bubbles were removed to ensure contact between the dermal surface of the pigskin and the receiving solution in the receiving cell. To minimize potential interference from the solvent, the tested lyophilized eye membrane samples were dissolved in 3 ml / piece of purified water, and 1355 μl of solution (300 μl / cm) was taken. 2 The solution is injected into the supply pool and placed close to the surface of the pigskin. After 1 hour, 4 hours, 8 hours, and 12 hours, approximately 300 μl of the test solution is taken from the receiving pool using a syringe.

[0107] Add the test solution to an ampoule, add 6.0 ml of 3 mol / L hydrochloric acid, purge with nitrogen, seal the ampoule with an alcohol burner, and place it in an oven at 105±1℃ for hydrolysis for 20 h. Transfer the hydrolysis product to a 10 ml volumetric flask, add 2.4 ml of 15 mol / L sodium hydroxide solution to neutralize excess hydrochloric acid, adjust the pH to 6–8, and add water to bring the volume to 10 ml. Filter 2 ml of the solution through a 0.45 pore size filter membrane and set aside for analysis. Accurately weigh 40 mg / L hydroxyproline (L-Hyp), dissolve it in 0.1 mol / L hydrochloric acid, and bring the volume to 25 ml to prepare the standard stock solution. Prepare the α-aminobutyric acid internal standard stock solution using the same method. Take 70 μl of boric acid solution and 10 μl of sample filtrate (or L-Hyp standard solution) from sample vial 1 of AccQ Tag Ultra (Waters Corporation, USA) and add them to the injection vial. Vortex thoroughly. Add 20 μl of derivatizing reagent from sample vial 2A of AccQ Tag Ultra (redissolve the powder from vial 2A with solution from sample vial 2B). Incubate at 55℃ for 10 min. After vortexing, perform the analysis. Flow rate: 2 ml / min; detection wavelength: 260 nm; column temperature: 55℃; injection volume: 10 μl; run time: 15 min.

[0108] Soluble collagen raw materials were used as samples for column chromatography to determine the peak elution time. The peak chromatograms of Examples 1-4 and Comparative Examples 1-4 were compared with the raw material peak chromatograms to identify the collagen peaks in the samples and calculate the peak areas. The relative percentage of collagen content in the samples of the other examples and comparative examples was calculated by using the peak area of ​​the 12-hour sample of Example 1 as 100%.

[0109] The test results are shown in Table 2.

[0110] Table 2 Results of the Permeability Test

[0111]

[0112]

[0113] Compared to Comparative Example 1, which did not contain Solution A, Examples 1-4 all contained Solution A, and the relative percentage of collagen content after 12 hours was significantly increased. Combined with Test Example 1, it can be seen that Examples 1-4 formed vesicle structures, with skin conditioning agents and other ingredients encapsulated within the vesicles, which can improve the penetration and absorption of active ingredients in the skin around the eyes.

[0114] Compared to Comparative Example 1, which did not contain solution A, Comparative Example 2, whose solution A included glycoside nonionic surfactants, phosphatidylcholine derivatives, and water, showed an increased relative percentage of collagen content after 12 hours. This indicates that glycoside nonionic surfactants and phosphatidylcholine derivatives can form vesicle structures, thereby improving the penetration and absorption of active ingredients in the skin around the eyes. Compared to Comparative Example 2, Comparative Example 3, whose solution A contained cholesterol, also showed an increased relative percentage of collagen content after 12 hours, indicating that cholesterol can improve the performance of vesicle structures. The applicant's analysis revealed that glycoside nonionic surfactants and phosphatidylcholine derivatives form the membrane structure of vesicles, while cholesterol derivatives insert into this membrane structure, playing a stabilizing role. Compared to Comparative Example 2, Comparative Example 4, which included mold / yeast fermentation extract, showed a decrease in the relative percentage of collagen content at 12 hours. However, when Example 1 included cholesterol and mold / yeast fermentation extract, the percentage of collagen content at 12 hours increased significantly, indicating that cholesterol and mold / yeast fermentation extract have a synergistic effect, enabling vesicles to better perform their permeation function.

[0115] Test Example 3

[0116] wrinkle removal test

[0117] The anti-wrinkle efficacy of freeze-dried eye masks was evaluated and compared in accordance with T / CAB 0152-2022, "Test Methods for Seven Efficacy Items of Cosmetics: Anti-wrinkle, Firming, Moisturizing, Oil Control, Repairing, Nourishing, and Soothing." Photos of the test areas were acquired using a skin image acquisition instrument, and skin wrinkle parameters (wrinkle volume, wrinkle area, number of wrinkles, etc.) were analyzed. Combined with wrinkle level evaluation (visual evaluation / photographic evaluation), changes in skin wrinkles before and after product use were compared.

[0118] In addition to meeting routine screening requirements, participants were required to have fine lines or wrinkles at the corners of both eyes, conforming to the "Skin Aging Atlas" grading chart for wrinkles at the corners of the eyes at levels 1-6 (Level 0: No wrinkles, rosy complexion, elastic skin. Level 1: Fine pseudo-wrinkles. Level 2: Fine true wrinkles. Level 3: Mild true wrinkles. Level 4: Moderate true wrinkles. Level 5: Severe true wrinkles. Level 6: Severe true wrinkles, poor skin elasticity), or conforming to the "Guidelines for the Evaluation of Anti-wrinkle Products Without New Efficacy" grading chart for wrinkles at the corners of the eyes at levels 1-7, with the wrinkles at the left and right outer corners of the eyes being of the same level.

[0119] Sixty-four volunteer subjects were selected, with a mean age of 53.7 years and a median age of 56.5 years. There were 34 females and 30 males. They were randomly divided into 8 groups of 6 subjects each, using the eye masks from Examples 1-4 and Comparative Examples 1-4, respectively. Before testing, the test area at the corners of the eyes was cleansed with a standardized facial cleanser. Before product use, images of the left and right corners of the eyes were captured using a skin texture analyzer (Courage+Khazaka electronic GmbH, VC20 Plus, Germany). Trained and qualified researchers assessed the wrinkle severity of the subjects according to the wrinkle grading chart of the "Skin Aging Atlas," assigning a rating (visual evaluation) to the corners of the eyes, which was recorded as the initial value. Test samples were distributed, and subjects were instructed on product use. Subjects could randomly choose either side as the experimental group and the other side as the control group, using the lyophilized powder product. Once the selection was made, it could not be changed during the trial period. Image acquisition and rating were conducted again after 2 weeks, 4 weeks ± 1 day, and 8 weeks ± 2 days of product use, and the measured values ​​were recorded. The test results are shown in Table 3.

[0120] Table 3 Results of the wrinkle-removing experiment

[0121]

[0122] Comparative Example 1, which did not contain Solution A, showed a decrease in wrinkle depth of approximately 0.023 mm and a decrease in wrinkle grade score of 0.6 after 8 weeks. Examples 1-4, which all contained Solution A, showed a decrease in wrinkle depth of more than 0.061 mm and a decrease in wrinkle grade score of more than 1.5 after 8 weeks. Clearly, compared to Comparative Example 1, Examples 1-4 showed a significantly greater reduction in wrinkle depth and wrinkle grade score after 8 weeks. Combined with Test Example 1, it can be seen that Examples 1-4 formed vesicle structures, with skin conditioning agents and other ingredients encapsulated within the vesicles, which can enhance the wrinkle-reducing effect of the freeze-dried eye mask.

[0123] In Comparative Example 2, solution A included glycoside nonionic surfactants, phosphatidylcholine derivatives, and water. After 8 weeks, the wrinkle depth decreased by approximately 0.039 mm, and the wrinkle grade score decreased by 1. The decrease in wrinkle depth and wrinkle grade score after 8 weeks was better than that in Comparative Example 1, indicating that glycoside nonionic surfactants and phosphatidylcholine derivatives can form vesicle structures, thereby improving the wrinkle-reducing effect of freeze-dried eye masks.

[0124] Compared to Comparative Example 2, Comparative Example 3, with the addition of cholesterol in solution A, showed a decrease in wrinkle depth of approximately 0.042 mm after 8 weeks, a greater reduction than that in Comparative Example 2, indicating that cholesterol can improve the performance of vesicle structures. The applicant's analysis revealed that glycoside nonionic surfactants and phosphatidylcholine derivatives form the membrane structure of vesicles, while cholesterol inserts into this membrane structure to play a stabilizing role.

[0125] Compared to Comparative Example 2, Comparative Example 4, which included a mold / yeast fermentation extract, showed a decrease in wrinkle depth of approximately 0.049 mm and a decrease in wrinkle grade score of 1.2 after 8 weeks. Both decreases were more significant than in Comparative Example 2, indicating that the mold / yeast fermentation extract can improve the performance of vesicle structures. The applicant's analysis revealed that the mold / yeast fermentation extract contains various biological enzymes that can embed into the vesicle membrane structure. When vesicles come into contact with the skin, these enzymes can create openings in the skin cell membrane, making it easier for vesicles to enter the skin cells.

[0126] In Example 1, when cholesterol and mold / yeast fermentation extracts were included, the wrinkle depth decreased by about 0.066 mm after 8 weeks, and the wrinkle grade score decreased by 1.7. The decrease was significantly higher than that of Comparative Example 3 and Comparative Example 4, indicating that cholesterol and mold / yeast fermentation extracts have a synergistic effect, which can enable vesicles to better enhance the wrinkle-reducing effect.

[0127] Test Example 4

[0128] Eye area whitening test

[0129] Forty-eight volunteers were recruited, aged 36.4–53.1 years, with a median age of 42.8 years. There were 33 females and 15 males. Participants were required to have epidermal pigmentation in the intended test area of ​​the eye, or to have an average ITA° (Individual Type Angle) value between 10° and 41° measured five times at different locations within the intended test area using a tristimulus colorimeter. Exclusion criteria included: birthmarks or congenital pigmentary abnormalities; previous chemical peels, reconstructive laser treatments for pigmentation; use of preparations affecting skin color within the past week or epidermal pigmentation levels within the past month; use of antihistamines within the past week or immunosuppressants within the past month; use of any anti-inflammatory drugs on the test site within the past two months; and other factors that might affect the experimental results. Participants were randomly divided into eight groups of six, using samples from Examples 1, 2, 3, and 4, and Comparative Examples 1–4, respectively. During the trial, no agents that could affect the whitening and spot-removing test should be used on the test site. Subjects should not ingest agents that could affect the whitening and spot-removing test via intravenous drip, injection, oral administration, or other means. Subjects should primarily engage in indoor activities and avoid prolonged exposure to sunlight.

[0130] Before using the product, subjects cleansed their face with water and patted it dry with a towel. They lay supine, applied the lyophilized eye mask sample to the test area of ​​the eye, and covered it with a dressing moistened with a small amount of pure water. This was done once daily. Before the start of the experiment and at 1, 2, and 4 weeks after the test, the ITA° value of the test area was measured using a tristimulus colorimeter (Hyperion, Admesy). Measurements were taken five times at different locations on the test area, and the average value was calculated. The results are shown in Table 4.

[0131] Table 4 Results of the periorbital whitening experiment

[0132]

[0133]

[0134] In the tristimulus value colorimetric method, a low measured value indicates a darker skin tone, while a rising measured value indicates a lighter skin tone. Comparative Example 1, which did not contain solution A, showed an ITA° value increase of approximately 4.3 after 4 weeks. Examples 1-4, which all contained solution A, showed ITA° values ​​increase of over 14.4 after 4 weeks. Clearly, compared to Comparative Example 1, the increase in ITA° values ​​after 4 weeks in Examples 1-4 was significantly greater. Combined with Test Example 1, it can be seen that Examples 1-4 formed vesicle structures, with skin conditioning agents and other ingredients encapsulated within the vesicles, which can enhance the whitening effect of the freeze-dried eye masks.

[0135] In Comparative Example 2, solution A included glycoside nonionic surfactants, phosphatidylcholine derivatives, and water. After 4 weeks, the ITA° value increased by about 6.9, which was better than that in Comparative Example 1. This indicates that glycoside nonionic surfactants and phosphatidylcholine derivatives can form vesicle structures, thereby improving the whitening effect of freeze-dried eye masks.

[0136] Compared to Comparative Example 2, Comparative Example 3, solution A, contained cholesterol, and its ITA° value increased by approximately 7.6 after 4 weeks, a greater increase than that of Comparative Example 2. This indicates that cholesterol can improve the performance of vesicle structures. The applicant's analysis revealed that glycoside nonionic surfactants and phosphatidylcholine derivatives form the membrane structure of vesicles, while cholesterol inserts into this membrane structure to play a stabilizing role.

[0137] Compared to Comparative Example 2, Comparative Example 4 included a mold / yeast fermentation extract. After 4 weeks, the ITA° value increased by approximately 10.3, a greater increase than in Comparative Example 2, indicating that the mold / yeast fermentation extract can improve the performance of vesicle structures. Analysis by the applicant revealed that the mold / yeast fermentation extract contains various biological enzymes that can embed into the vesicle membrane structure. When vesicles come into contact with the skin, these enzymes can create openings in the skin cell membrane, making it easier for vesicles to enter the skin cells.

[0138] In Example 1, when cholesterol and mold / yeast fermentation extracts were included, the ITA° value increased by about 15.7 after 4 weeks. The increase was significantly higher than that of Comparative Example 3 and Comparative Example 4, indicating that cholesterol and mold / yeast fermentation extracts have a synergistic effect, which can enable the vesicles to better enhance the whitening effect.

[0139] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0140] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are specific and detailed, they should not be construed as limiting the scope of the patent application. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the scope of protection of the present invention. Therefore, the scope of protection of this patent should be determined by the appended claims.

Claims

1. A freeze-dried eye mask, characterized in that, By weight, the freeze-dried eye membrane consists of the following components:

2. The freeze-dried eye membrane according to claim 1, characterized in that, The glycoside nonionic surfactants include one or two of the following: C12-16 alkyl glucoside, C8-C14 alkyl glucoside, lauryl glucoside, cocoyl glucoside, hexadecyl glucoside, decyl glucoside, and isostearyl glucoside.

3. The freeze-dried eye mask according to claim 1, characterized in that, The phosphatidylcholine class includes one or both of phosphatidylcholine and hydrogenated phosphatidylcholine.

4. The freeze-dried eye membrane according to claim 1, characterized in that, The cholesterols include one or two of the following: cholesterol, dihydrocholesterol, cholesterol chloride, cholesterol polyether-5, cholesterol butyrate, cholesterol succinate, cholesterol nonanoate, cholesterol oleate, cholesterol stearate, and cholesterol lanolinate.

5. The freeze-dried eye membrane according to claim 1, characterized in that, The mold / yeast fermentation extract includes one or more of the following: *Brucea buddingis* fermentation product, *Mucor* extract, *Endospora* fermentation product filtrate, *Aspergillus* fermentation product, *Aspergillus* / glucose / soybean / starch fermentation product filtrate, *Pichia pastoris* fermentation lysate filtrate, *Galactomyces* fermentation product filtrate, yeast fermentation product extract, yeast fermentation product, yeast fermentation product filtrate, yeast fermentation lysate filtrate, yeast lysate, yeast lysate extract, yeast extract, and hydrolyzed yeast extract.

6. The freeze-dried eye membrane according to any one of claims 1-5, characterized in that, The freeze-dried eye mask comprises 0.05–0.25 parts lauryl glucoside, 0.03–0.25 parts phosphatidylcholine, 0.01–0.04 parts cholesterol, 0.02–0.1 parts Mucor extract, and 0.01–0.1 parts Aspergillus fermentation product.

7. The freeze-dried eye membrane according to any one of claims 1-5, characterized in that, The moisturizer includes one or more of glycerin, 1,3-propanediol, sodium hyaluronate, trehalose, and caprylyl glycol.

8. The freeze-dried eye membrane according to any one of claims 1-5, characterized in that, The skin conditioning agent includes one or more of the following: soluble collagen, niacinamide, ceramide, hydroxypropyl tetrahydropyrantriol, *Sparganium stoloniferum* extract, *Artemisia umbellatus* extract, *Adenophora stricta* extract, *Nymphaea granatum* extract, benzoin extract, *Ganoderma lucidum* extract, *Witch hazel* bark / twig extract, cardamom fruit extract, tea extract, daisy flower extract, *Lophatherum gracile* leaf extract, hyacinth extract, *Phellodendron amurense* bark extract, turmeric rhizome extract, coltsfoot flower extract, *Trifolium repens* seed extract, litchi seed extract, *Salvia miltiorrhiza* extract, and *Citrus medica* peel extract.

9. The freeze-dried eye membrane according to any one of claims 1-5, characterized in that, The thickener includes one or more of hydroxyethyl cellulose, xanthan gum, carbomer, and maltodextrin.

10. A method for preparing a freeze-dried eye mask as described in any one of claims 1-9, characterized in that, include: (1) Take glycoside nonionic surfactants, phosphatidylcholine, cholesterol and mold / yeast fermentation extracts, dissolve them in water and mix them evenly, filter them to obtain solution A; (2) Take moisturizer, skin conditioner, thickener, preservative and antibacterial agent and pH regulator, dissolve in water and filter to obtain solution B; (3) Mix solution A and solution B and stir evenly. Dispense into freeze-drying molds and freeze quickly to -55°C. Then gradually heat to -25°C, 0°C and 35°C for sublimation drying. (4) Remove the freeze-dried eye membrane from the freeze-drying mold, put it into a packaging box and a sealed bag, and store it in a sealed container.

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