Cosmetic lyophilized particles and method for their preparation

Abstract

The present application relates to the technical field of freeze-dried cosmetics, in particular to IPC A61K9, more particularly to a cosmetic freeze-dried particle and a preparation method thereof.The freeze-dried particle of the present application is composed of a hydrophobic powder and a content, the content mixed solution is added drop by drop onto the wrapper, freeze-dried, vacuumized, heated and dried after shaping, and the freeze-dried particle is obtained.The preparation method of the present application provides a new form of freeze-dried product, i.e., freeze-dried particle, which can be taken according to the demand and reduce the waste phenomenon.

Description

Technical Field

[0001] This invention relates to the field of freeze-dried cosmetics technology, particularly to IPC A61K9, and more specifically to a type of freeze-dried cosmetic granules and its preparation method. Background Technology

[0002] Freeze-drying technology is widely used in the cosmetics industry. It allows for the removal of moisture and other volatile substances at relatively low temperatures (generally not exceeding 40°C). This not only avoids the damage to active ingredients caused by the high temperatures of traditional drying methods but also preserves the shape of the dried product. Furthermore, the active ingredients are less prone to hydrolysis and microbial growth during subsequent storage. Common freeze-dried products on the market include freeze-dried powder and freeze-dried spheres. These products require the liquid to be filled into vials or molds for freeze-drying before use. They are then mixed with a solvent and applied to the skin.

[0003] Existing patent CN202010374782.0 discloses a vial-dried facial mask and its preparation method. The raw materials for preparing the mask are deionized water, mannitol, niacinamide, NB835, trehalose, copper peptide, disodium hydrogen phosphate, sodium chloride, tetrahydromethylpyrimidine carboxylic acid, and sodium dihydrogen phosphate. After freeze-drying, the mask is stored and packaged in vials. The amount of product in each vial is fixed, and the amount of freeze-dried mask used may be excessive, resulting in waste.

[0004] Existing patent CN202110232069.7 discloses a freeze-dried ball and its preparation method. The raw materials for preparation include polyols, polysaccharides, and hyaluronic acid salts. The raw materials are prepared into a freeze-dried ball. The quality of the freeze-dried ball is fixed and its dosage cannot be controlled.

[0005] For a long time, the form of freeze-dried products on the market has been relatively limited, with only two common forms: freeze-dried powder and freeze-dried spheres. Consumers have not been able to try novel forms of freeze-dried products. Both freeze-dried powder and freeze-dried sphere products are designed for single-use, and must be used up at once. Unused products exposed to air are prone to microbial growth, so these products cannot flexibly adjust the dosage. However, consumers have different face sizes and require different amounts, and there is also a need for localized application, leading to waste of some product. Therefore, there is a need to develop a novel form of freeze-dried granules that allows for adjustable dosage, maintaining the activity of the contents while reducing microbial growth and controlling dosage. Summary of the Invention

[0006] To address the problems in the prior art, the first aspect of the present invention provides a cosmetic freeze-dried particle, the freeze-dried particle comprising an encapsulant and contents.

[0007] Preferably, the encapsulation material comprises a hydrophobic powder.

[0008] Preferably, the hydrophobic powder includes one or both of the following: organic material powder and powder with an inorganic interior and an organic exterior.

[0009] Preferably, the organic material powder accounts for 80% to 100% of the mass percentage of the hydrophobic powder.

[0010] Preferably, the organic material powder is one or more of polymethylsilsesquioxane, vinyl polydimethylsiloxane-polymethylsilsesquioxane crosslinked polymer, nylon-12, and lauroyl lysine.

[0011] Preferably, the powder, which has an inorganic interior and an organic exterior, is one or more of silyl alkyl silicate, dimethyl silyl silicate, and trimethylsiloxy silicate; more preferably, it is one or more of silyl alkyl silicate and dimethyl silyl silicate.

[0012] Preferably, the contents include a plasticizer and an active ingredient, but do not include ingredients that can significantly reduce surface tension.

[0013] Preferably, the component that significantly reduces surface tension includes one or more of fatty alcohol ether sulfates, alkyl acyl glycinates, alkyl acyl glutamates, alkyl glucosides, fatty alcohol sulfates, fatty alcohol polyethers, and fatty acid polyethers.

[0014] Preferably, the shaping agent includes one or more of mannitol, trehalose, sucrose, betaine, raffinose, sodium alginate, xylose, xylitol, and rhamnose; more preferably, the shaping agent includes one or more of mannitol, trehalose, sucrose, betaine, and raffinose.

[0015] Preferably, the active ingredient includes one or more of ascorbic acid, copper peptide, bromelain, papain, glutathione, arbutin, allantoin, dipotassium glycyrrhizate, and glycerol glucoside; more preferably, it includes one or more of ascorbic acid, copper peptide, bromelain, papain, glutathione, and arbutin.

[0016] Preferably, the active ingredient further includes one or more of sodium hyaluronate, Sphingomonas fermentation product extract, Tremella fuciformis fruiting body extract, polyvinylpyrrolidone, 1,2-hexanediol, 1,2-pentanediol, glycerol, 1,3-butanediol, glycine, alanine, and arginine; more preferably, it is one or more of sodium hyaluronate, Sphingomonas fermentation product extract, Tremella fuciformis fruiting body extract, polyvinylpyrrolidone, 1,2-hexanediol, 1,2-pentanediol, and glycerol.

[0017] Preferably, the plasticizer accounts for 1-15% of the mass percentage of the contents; more preferably, it is 3-12%.

[0018] Preferably, all contents are water-soluble substances.

[0019] In this invention, a hydrophobic powder and its contents are compounded, wherein the hydrophobic powder is an organic material powder or a combination of an organic material powder with an inorganic interior and an organic exterior. The organic material powder constitutes 80-100% of the hydrophobic powder by mass. This compound can form a 2-4 mm sphere with the water-soluble contents, improving the success rate of sphere formation while maintaining the usability of the freeze-dried granules. The inventors unexpectedly discovered that if too much of the inorganic interior and organic exterior powder is added, it becomes impossible to form a spherical shape on the tray surface. Furthermore, if the contents contain components that significantly reduce surface tension, such as fatty alcohol ether sulfates, alkyl acyl glycinates, alkyl acyl glutamates, alkyl glucosides, fatty alcohol sulfates, fatty alcohol polyethers, or fatty acid polyethers, it is also difficult to form spherical freeze-dried granules. In a chance experiment, it was discovered that the selected hydrophobic powders were all organic materials or had an organic material content of over 80% by mass. The water-soluble contents formed a large contact angle on the surface of the hydrophobic powder, forming water spheres and creating relatively regular freeze-dried particles that met the requirements.

[0020] In this invention, by selecting water-soluble ingredients and ensuring that the plasticizer accounts for 3-12% of the total ingredients by mass, freeze-dried granules with a size of 2-4 mm can be formed, while simultaneously improving the skin feel of the freeze-dried granules. The inventors discovered that when oil-soluble raw materials are used as ingredients, hydrophobic powders dissolve directly into the raw materials, forming a paste that cannot form freeze-dried granules. Simultaneously, when the plasticizer content is low, the viscosity of the ingredients decreases, and during the freeze-drying process, the ingredients may continue to disperse, failing to form regular 2-4 mm freeze-dried granules. Furthermore, the inventors unexpectedly discovered that the plasticizer content has a significant impact on the skin feel of the freeze-dried granules; when the plasticizer content is too high, the skin feel deteriorates, becoming noticeably rougher. Therefore, it is necessary to select water-soluble ingredients, and for the plasticizer to account for 3-12% of the total ingredients by mass, to form freeze-dried granules with a size of 2-4 mm.

[0021] A second aspect of this invention provides a method for preparing freeze-dried cosmetic granules, comprising the following steps:

[0022] S1: Dissolve the contents in water and mix well to obtain a mixture of contents;

[0023] S2: After mixing the contents, spread them evenly on the surface of a plastic tray, and then add the contents mixture drop by drop onto the contents to obtain powder-coated, non-mixed liquid spheres.

[0024] S3: Freeze the liquid spheres obtained in S2, shape them, vacuum them, heat them, and dry them to obtain freeze-dried granules.

[0025] Preferably, the contents constitute 1-15% of the mass of the contents mixture; more preferably, 3-12%.

[0026] Preferably, the contents mixture is a contents solution or a contents dispersion.

[0027] Preferably, the thickness of the covering material on the surface of the plastic tray in S2 is 1 μm to 1 mm.

[0028] Preferably, the device used for adding liquid in S2 is a multi-head dripping device.

[0029] Preferably, the freezing temperature in S3 is -60 to -30°C, and the freezing time is 1 to 12 hours.

[0030] Preferably, the vacuum level evacuated in step S3 is 2 to 30 Pa.

[0031] Preferably, in step S3, the temperature is raised to 20–40°C, and the drying time is 1–12 hours.

[0032] This invention utilizes a multi-head dripping device to add the contents dropwise onto a package, resulting in a new freeze-dried product state: freeze-dried granules of 2-4 mm. This allows for various packaging options and enables consumers to flexibly adjust the dosage, enhancing convenience. The inventors discovered that directly mixing active substances and plasticizers to form small droplets, then freeze-drying them in vials to form freeze-dried powder or lyophilized spheres, results in a fixed amount for each use, easily leading to waste or insufficient product. However, by using a multi-head dripping device to add the contents dropwise onto the package, the contents drip and, upon impact with the powder, spread out and then contract into a small sphere. During this process, the powder automatically adheres to the liquid surface, forming spheres with a particle size of 2-4 mm. These hydrophobic powder-encapsulated liquid spheres are then frozen in a freeze dryer, and the freeze-dried granules are collected and stored conveniently. This method allows for various packaging options and enables consumers to flexibly adjust the dosage, further enhancing convenience.

[0033] Beneficial effects

[0034] 1. In this invention, a hydrophobic powder and its contents are compounded, wherein the hydrophobic powder is an organic material powder or a combination of an organic material powder and an inorganic material powder on the outside and an organic material powder on the inside. The organic material powder accounts for 80-100% of the mass percentage of the hydrophobic powder. It can form a 2-4 mm sphere with the water-soluble contents, thereby improving the success rate of sphere formation of freeze-dried granules while maintaining the usability of the freeze-dried granules.

[0035] 2. In this invention, by selecting water-soluble contents and making the plasticizer account for 3-12% of the total contents by mass, the skin feel of the freeze-dried granules is improved.

[0036] 3. This invention utilizes a multi-head dripping device to add the contents drop by drop onto the package, resulting in a new freeze-dried product state, which is freeze-dried granules of 2-4 mm. It can be used in a variety of outer packaging forms, and consumers can flexibly adjust the dosage when using it, thus improving convenience.

[0037] 4. The freeze-dried cosmetic particles of the present invention have the advantages of conventional freeze-dried products, such as protecting active ingredients and improving stability, eliminating the need for preservatives, and facilitating storage and transportation. At the same time, the use of hydrophobic powder can improve the smoothness of the powder when used.

[0038] 5. This invention prepares a freeze-dried granule product that has never appeared on the market before, with a novel granular appearance. Attached Figure Description

[0039] Figure 1 This is a diagram of the freeze-dried cosmetic particles prepared in Example 1.

[0040] Figure 2 This is a diagram of the freeze-dried cosmetic particles prepared in Example 3.

[0041] Figure 3 This is a graph showing the stability results of the freeze-dried particles and contents in Example 1 after being stored at 50°C for 2 weeks. Detailed Implementation

[0042] Example 1

[0043] This embodiment provides freeze-dried cosmetic granules and their preparation method. The preparation method of the freeze-dried cosmetic granules includes the following steps:

[0044] S1: Weigh out 6 parts mannitol, 3.8 parts ascorbic acid, 0.2 parts glutathione, and 90 parts water by weight. Add mannitol, ascorbic acid, and glutathione to the water and stir continuously at 25°C until completely dissolved to obtain a mixture of contents.

[0045] S2: Spread polymethylsilsesquioxane powder evenly on the surface of a plastic tray with a thickness of 0.2 mm. Use a multi-head dripping device to add the contents mixture drop by drop onto the surface of the polymethylsilsesquioxane powder to obtain powder-encapsulated, non-fused liquid spheres.

[0046] S3: Place the liquid microspheres in a freeze dryer, first cool to -60℃ and maintain for 3 hours. At this time, the liquid microspheres will solidify and form. Then, apply a vacuum to maintain a pressure of 15Pa, raise the temperature to 25℃ and dry for 1 hour to obtain 2-4mm freeze-dried cosmetic granules. See [link to product details]. Figure 1 .

[0047] The mannitol was purchased from D-MANNITOL of DUKSAN.

[0048] The ascorbic acid was purchased from DSM as VITAGIN A.

[0049] The glutathione was purchased from KYOWA's L-GLUTATHIONE REDUCED.

[0050] The polymethylsilsesquioxane was purchased from MOMENTIVE's TOSPEARL 2000B.

[0051] Example 2

[0052] This embodiment provides freeze-dried cosmetic granules and their preparation method. The preparation method of the freeze-dried cosmetic granules includes the following steps:

[0053] S1: Weigh out 3 parts mannitol, 0.05 parts sphingomonas fermentation product extract, 0.2 parts bromelain, and 96.75 parts water by weight. Add mannitol and sphingomonas fermentation product extract to water, heat to 70°C and stir continuously until completely dissolved. Then lower the temperature to 25°C, add bromelain, and mix well to obtain the contents mixture.

[0054] S2: Spread the vinyl polydimethylsiloxane / polymethylsiloxane silsesquioxane crosslinked polymer powder evenly on the surface of a plastic tray with a thickness of 0.2 mm. Use a multi-head dripping device to add the contents mixture dropwise to the surface of the vinyl polydimethylsiloxane / polymethylsiloxane silsesquioxane crosslinked polymer powder to obtain powder-encapsulated, non-fused liquid spheres.

[0055] S3: Place the liquid microspheres in a freeze dryer, first cool to -30℃ and keep for 12 hours. At this time, the liquid microspheres solidify and take shape. Then, evacuate and keep the air pressure at 15Pa. Raise the temperature to -20℃ and dry for 12 hours. Raise the temperature to 25℃ and dry for 12 hours to obtain 2-4mm freeze-dried cosmetic granules.

[0056] The mannitol was purchased from D-MANNITOL of DUKSAN.

[0057] The sphingomonas fermentation product extract was purchased from KELCO-CARE DIUTAN GUM in LUBRIZOL.

[0058] The bromelain was purchased from AC Bromelain Powder of ACTIVECONCEPTS.

[0059] The vinyl polydimethylsiloxane / polymethylsiloxane sesquioxane crosslinked polymer powder was purchased from SHIN-ETSU KSP 101.

[0060] Example 3

[0061] This embodiment provides freeze-dried cosmetic granules and their preparation method. The preparation method of the freeze-dried cosmetic granules includes the following steps:

[0062] S1: Weigh out 5 parts raffinose, 1 part trehalose, 1 part betaine, 0.5 parts sucrose, 0.5 parts copper peptide, and 92 parts water by weight. Add raffinose, trehalose, betaine, sucrose, and copper peptide to the water and stir continuously at 25°C until completely dissolved to obtain a mixture of contents.

[0063] S2: Mix polymethylsilsesquioxane powder, silylated silica and dimethylsilylated silica in a mass ratio of 8:1:1 and spread them evenly on the surface of a plastic tray with a thickness of 0.6 mm. Use a multi-head dripping device to add the contents mixture drop by drop to the surface of the mixture on the tray to obtain powder-coated, non-fused liquid spheres.

[0064] S3: Place the liquid microspheres in a freeze dryer, first cool to -30℃ and maintain for 12 hours, at which point the liquid microspheres will solidify. Then, apply a vacuum to maintain a pressure of 15 Pa, raise the temperature to 0℃ and dry for 3 hours, then raise the temperature to 45℃ and dry for 2 hours to obtain 2-4 mm freeze-dried cosmetic granules. See [link to product details]. Figure 2 .

[0065] The raffinose was purchased from OLIGO GGF by ASAHI KASEI.

[0066] The trehalose was purchased from Trehalose of HAYASHIBARA.

[0067] The betaine was purchased from DUPONT's GENENCARE OSMS BA.

[0068] The sucrose was purchased from CASTER SUGAR in SAMYANGSA.

[0069] The copper peptide was purchased from Shenzhen Winkey Pharmaceutical R&D Co., Ltd. as WKPEPCOPPER PEPTIDE X.

[0070] The polymethylsilsesquioxane was purchased from MOMENTIVE's TOSPEARL 2000B.

[0071] The silylated silica was purchased from EVONIK. R 812S.

[0072] The dimethylsilylated silica mentioned above was purchased from EVONIK. R 974.

[0073] Example 4

[0074] This embodiment provides freeze-dried cosmetic granules and their preparation method. The preparation method of the freeze-dried cosmetic granules includes the following steps:

[0075] S1: Weigh out 4 parts mannitol, 2 parts trehalose, 2 parts arbutin and 92 parts water by weight. Add mannitol, trehalose and arbutin to water and stir continuously at 25°C until completely dissolved to obtain a mixture of contents.

[0076] S2: Nylon-12 powder and lauroyl lysine powder are mixed at a mass ratio of 9:1 and spread evenly on the surface of a plastic tray with a thickness of 0.2 mm. The contents mixture is then added drop by drop to the surface of the mixture on the tray using a multi-head dripping device to obtain powder-coated, non-fused liquid spheres.

[0077] S3: Place the liquid microspheres in a freeze dryer, first cool to -30℃ and keep for 12 hours. At this time, the liquid microspheres will solidify and take shape. Then, evacuate and keep the air pressure at 15Pa. Raise the temperature to 0℃ and dry for 3 hours. Raise the temperature to 45℃ and dry for 2 hours to obtain 2-4mm freeze-dried cosmetic particles.

[0078] The mannitol was purchased from D-MANNITOL of DUKSAN.

[0079] The trehalose was purchased from Trehalose of HAYASHIBARA.

[0080] The arbutin was purchased from ARBUTIN of HUBEI ARTEC BIOTECHNOLOGY.

[0081] The nylon-12 was purchased from TORAY's NYLON POWDER SP-10.

[0082] The lauroyl lysine was purchased from AJINOMOTO's AMIHOPE-LL.

[0083] Comparative Example 1

[0084] The specific implementation method of Comparative Example 1 is the same as that of Example 1, except that, in S1: by mass, 5 parts of mannitol, 0.5 parts of copper peptide, 2 parts of decyl glucoside (50wt% aqueous solution), and 92.8 parts of water are weighed. Mannitol, copper peptide, and decyl glucoside are added to water, heated to 60°C and stirred continuously until completely dissolved. Then, the temperature is lowered to 25°C and bromelain is added. The mixture is stirred evenly to obtain the contents mixture.

[0085] The decyl glucoside was purchased from BASF's PLATNACARE 2000UP.

[0086] Comparative Example 2

[0087] The specific implementation of Comparative Example 2 is the same as that of Example 3, except that the ratio of polymethylsilsesquioxane powder, silylated silica and dimethylsilylated silica is 5:2:3.

[0088] Comparative Example 3

[0089] The specific implementation of Comparative Example 3 is the same as that of Example 4, except that the lauroyl lysine is replaced with dimethylsilylated silica powder, and the mass ratio of nylon-12 powder to dimethylsilylated silica powder is 4:6.

[0090] Comparative Example 4

[0091] The specific implementation of Comparative Example 4 is the same as that of Example 4, except that the plasticizer accounts for 20% of the mass of the contents.

[0092] Performance testing

[0093] 1. The results of observing the freeze-dried cosmetic particles of Examples 1-4 and Comparative Examples 1-4 are shown in Table 1.

[0094] As shown in Table 1, the cosmetic freeze-dried particles prepared using this invention in Examples 1-4 are obtained by first preparing non-fused liquid spheres encapsulated by hydrophobic powder and aqueous solution or dispersion, followed by freeze-drying of the spheres. If a component that reduces surface tension is added to the aqueous solution or dispersion, non-fused spheres encapsulated by powder cannot be formed, thus preventing the acquisition of cosmetic freeze-dried particles. If the ratio of organic material powder to powder with an inorganic interior and an organic exterior in the hydrophobic powder is less than 80:20, the liquid spheres cannot be completely encapsulated.

[0095] 2. The contents obtained in Examples 1-4 were placed directly into vials without encapsulation and freeze-dried to obtain the control samples of Examples 1-4. Four volunteers with healthy arm skin were selected and divided into four groups. A double-blind experiment was conducted on the left and right arms of the volunteers. The four groups used the control samples of Examples 1-4 and the freeze-dried granule samples, respectively. The control samples and freeze-dried granule samples were mixed evenly with purified water as a solvent and applied to the arms. The volunteers' feelings about the product on both arms were recorded. The volunteers all felt that the freeze-dried granule product had a smooth feeling after use, while the control sample made their skin feel rougher.

[0096] In addition, using the freeze-dried granules obtained in Example 4 and Comparative Example 4, a double-blind experiment was conducted on the left and right arms of two volunteers with healthy arm skin. The products used were the freeze-dried granules of Example 4 and Comparative Example 4. The freeze-dried granules of Example 4 and Comparative Example 4 were mixed evenly with purified water as a solvent and applied to the arms. The volunteers' feelings about the product on both arms were recorded. The volunteers felt that the freeze-dried granule product of Example 4 had a smooth feel after use, while the freeze-dried granule product of Comparative Example 4 had a noticeably rougher feel on the skin. This indicates that the amount of shaping agent should not be too high.

[0097] 3. Stability Test

[0098] The freeze-dried granules obtained in Example 1 were stored at 50°C for 2 weeks and then dissolved in water in a bottle. Conversely, the contents of Example 1 were placed directly in a bottle and stored at 50°C for 2 weeks. Comparing the two, it was found that the freeze-dried granules of Example 1 showed almost no discoloration after being dissolved in water, while the solution of the contents of Example 1 turned noticeably yellow, indicating that the method of the present invention significantly improves stability. (See results below.) Figure 3 The left side of the figure shows the stability sample of Example 1, and the right side shows the stability sample with the contents solution placed directly.

[0099] Table 1

[0100]

Claims

1. A type of freeze-dried cosmetic granules, characterized in that, The freeze-dried granules comprise an encapsulation material and contents; the encapsulation material comprises a hydrophobic powder; the hydrophobic powder is a combination of polymethylsilsesquioxane, silylated silica, and dimethylsilylated silica; the polymethylsilsesquioxane accounts for 80% of the mass percentage of the hydrophobic powder; the contents comprise a plasticizer and an active ingredient, excluding one or more of fatty alcohol ether sulfates, alkyl acyl glycinates, alkyl acyl glutamates, alkyl glucosides, fatty alcohol sulfates, fatty alcohol polyethers, and fatty acid polyethers; the plasticizer comprises one or more of mannitol, trehalose, sucrose, betaine, raffinose, sodium alginate, xylose, xylitol, and rhamnose; the plasticizer accounts for 3-12% of the mass percentage of the contents.

2. The freeze-dried cosmetic granules according to claim 1, characterized in that, The active ingredients include one or more of the following: ascorbic acid, copper peptide, bromelain, papain, glutathione, arbutin, allantoin, dipotassium glycyrrhizate, and glycerol glucoside.

3. The freeze-dried cosmetic granules according to claim 2, characterized in that, The active ingredients also include one or more of the following: sodium hyaluronate, Sphingomonas fermentation product extract, Tremella fuciformis fruiting body extract, polyvinylpyrrolidone, 1,2-hexanediol, 1,2-pentanediol, glycerol, 1,3-butanediol, glycine, alanine, and arginine.

4. A method for preparing cosmetic freeze-dried granules according to any one of claims 1 to 3, characterized in that, Includes the following steps: S1: Dissolve the contents in water and mix well to obtain a mixture of contents; S2: After mixing the contents, spread them evenly on the surface of a plastic tray, and then add the contents mixture drop by drop onto the contents to obtain powder-coated, non-mixed liquid spheres. S3: Freeze the liquid spheres obtained in S2, shape them, vacuum them, heat them, and dry them to obtain freeze-dried granules.

5. The method for preparing freeze-dried cosmetic granules according to claim 4, characterized in that, The contents constitute 1-15% of the mass of the contents mixture.

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