KR102653555B1 - Composition with stabilized active ingredient - Google Patents

Abstract

According to an embodiment of the present invention, a composition with stabilized active ingredients is provided. The composition in which the active ingredient is stabilized includes an active ingredient, a water-soluble polymer, and a hydrotrope component, and the active ingredient may be supported on the water-soluble polymer and stabilized by the hydrotrope component.

Description

Composition with stabilized active ingredients {COMPOSITION WITH STABILIZED ACTIVE INGREDIENT}

The present invention relates to a composition in which an active ingredient is stabilized, and specifically, a composition in which an active ingredient that is easily oxidized in the external environment is stabilized using a water-soluble polymer and a hydrotrope component. In particular, the present invention relates to a freeze-dried cosmetic composition in which active ingredients that are easily oxidized in the external environment are stabilized.

Vitamin C, vitamin E, arbutin, adenosine, polyphenols, and various natural oils and extracts are known to prevent wrinkles on the skin and provide various effects such as whitening, antioxidant, and moisturizing. Research is being actively conducted to include these active ingredients in skin improvement compositions. However, active ingredients such as vitamin C and vitamin E react sensitively to external environments such as air, light, heat, and moisture and are easily oxidized, making it difficult to include them stably in the composition.

To solve this problem, a technology was developed to prevent oxidation of the active ingredient by supporting it on a water-soluble polymer and then freeze-drying it. However, even if this method is used, problems such as discoloration of the composition, change in appearance, and decrease in potency over time still occur due to the hygroscopic nature of the freeze-dried formulation.

The present invention is intended to solve the above problem, by additionally including a hydrotrope component in a water-soluble polymer to stabilize the active ingredient that is unstable to air, light, heat, moisture, etc., so that the active ingredient is not lost and maintained at a high content even after a long period of time. The purpose is to provide a composition that can be used.

The technical problems of the present invention are not limited to the technical problems mentioned above, and other technical problems not mentioned will be clearly understood by those skilled in the art from the description below.

According to an embodiment of the present invention, a composition with stabilized active ingredients is provided. The composition in which the active ingredient is stabilized includes the active ingredient, a water-soluble polymer, and a hydrotrope component, and the active ingredient may be stabilized by the water-soluble polymer and the hydrotrope component.

Additionally, the active ingredient may be a component that is oxidized by at least one of air, light, heat, and moisture.

Additionally, the active ingredient may be supported in a porous structure formed by the water-soluble polymer and stabilized through bonding with the hydrotrope component.

Additionally, the active ingredient may be included in an amount of 6 to 80% by weight based on the total weight of the composition.

In addition, the active ingredients include water-soluble vitamins including ascorbic acid or its derivatives, oil-soluble vitamins including retinoic acid or its derivatives; arbutin; Water-soluble bioactive ingredients including adenosine; astaxanthin; polyphenol; And it may include one or more selected from the group consisting of natural extracts.

Additionally, the water-soluble polymer may be included in an amount of 5 to 55% by weight based on the total weight of the composition.

In addition, the water-soluble polymers include sodium hyaluronate, calcium hyaluronate, potassium hyaluronate, hyaluronic acid, hydrolyzed hyaluronic acid, hydrolyzed sodium hyaluronate, and hydrolyzed sodium hyaluronate. Hyaluronic acid, including rolled calcium hyaluronate, hydroxypropyltrimonium hyaluronate, sodium acetylated hyaluronate and sodium hyaluronate crosspolymer; Collagen and denatured collagen; algin; alginate; gelatin; carrageenan; starch; galactomannan; glucomannan; guar gum; Locust bean gum; xanthan gum; gellan; cellulose; polyvinylpyrrolidone (PVP); and polyvinyl alcohol (PVA).

Additionally, the hydrotrope component may include one or more selected from the group consisting of niacinamide, urea, caffeine, citrate, and salicylate.

Additionally, the hydrotrope component may be included in an amount of 8 to 80% by weight based on the total weight of the composition.

Additionally, the hydrotrope component may be included in an amount of 8 to 30% by weight based on the total weight of the composition.

Additionally, the weight ratio of the hydrotrope component to the active ingredient may be 1:0.1 to 10.

Additionally, the composition in which the active ingredient is stabilized may be formulated as a solid or semi-solid form.

Additionally, the composition in which the active ingredient is stabilized may be a freeze-dried formulation.

Additionally, the composition in which the active ingredient is stabilized may have a hardness of 150 dyne/cm ² or more.

According to an embodiment of the present invention, a cosmetic composition for improving skin comprising a composition in which the active ingredient is stabilized is provided.

According to the present invention, as the active ingredient, which has the property of being oxidized by air, light, heat, moisture, etc., is stabilized by the water-soluble polymer and hydrotrope component, the efficacy and potency of the active ingredient are maintained and formulation can be easily performed. .

In addition, according to the present invention, even if the composition is freeze-dried, the formulation and efficacy of the composition can be stably maintained without problems such as browning, external shrinkage, or decrease in potency over time.

In addition, according to the present invention, the weight is lighter than a typical cosmetic composition containing moisture through a freeze-drying process, and through this, carbon emissions can be reduced during the product distribution process. In particular, since it does not require the use of preservatives, it can be more environmentally friendly.

Additionally, according to the present invention, a solid or semi-solid composition with stabilized active ingredients can be rehydrated and used in the form of application, ingestion, etc. In particular, solid or semi-solid compositions with stabilized active ingredients can be quickly dissolved, making them easy to use.

In order to more fully understand the drawings cited in the detailed description of the present invention, a brief description of each drawing is provided.
1 is an SEM photograph of a composition according to an embodiment of the present invention.
Figures 2a and 2b are photographs for explaining the dissolution rate of compositions according to examples and comparative examples of the present invention.
Figure 3 is a graph showing the results of potency stability experiments according to examples and comparative examples of the present invention.

Unless otherwise defined, all technical and scientific terms used in this specification have the same meaning as commonly understood by a person skilled in the art to which the present invention pertains. In general, the nomenclature used herein is well known and commonly used in the art. Additionally, when describing embodiments of the present invention, if detailed descriptions of related known configurations or functions are judged to impede understanding of the embodiments of the present invention, the detailed descriptions will be omitted. In addition, embodiments of the present invention will be described below, but the technical idea of the present invention is not limited or limited thereto and may be modified and implemented in various ways by those skilled in the art.

According to an embodiment of the present invention, a composition with stabilized active ingredients is provided. The composition in which the active ingredient of the present invention is stabilized may include an active ingredient, a water-soluble polymer, and a hydrotrope component. At this time, the active ingredient may be stabilized by water-soluble polymer and/or hydrotrope component. Accordingly, in the present invention, oxidation of the active ingredient is prevented, and the potency may not decrease over time. Here, “potency” refers to the total amount of composition required to produce a given effect. In addition, containing a “high content” of the active ingredient may mean that the active ingredient is contained at 10% by weight or more relative to the total weight of the composition, but is not limited thereto.

In the present invention, “active ingredient” refers to an ingredient that exhibits skin-improving efficacy. Here, the skin improvement effect may include all known effects related to improving skin condition, such as antioxidant, anti-inflammatory, whitening, moisturizing, skin soothing, wrinkle improvement, and exfoliation.

The active ingredient of the present invention may be a component that has the property of being oxidized by at least one of air, light, heat, and moisture. In the present invention, oxidation of such active ingredients can be prevented by water-soluble polymers and/or hydrotrope components.

Depending on the embodiment, the active ingredient may be included in an amount of 6 to 80% by weight, specifically 20 to 80% by weight, and more specifically 50 to 80% by weight, based on the total weight of the composition. If the active ingredient is included in less than 6% by weight, the skin improvement effect may not be sufficiently apparent, and if the active ingredient is included in more than 80% by weight, the active ingredient may precipitate or its potency may decrease over time. Additionally, in the present invention, the active ingredient may be stably contained at 6% by weight, 20% by weight, or 50% by weight or more by water-soluble polymer and/or hydrotrope component.

Depending on the embodiment, the active ingredient may be water-soluble vitamins including ascorbic acid or its derivatives; Oil-soluble vitamins including retinoic acid or its derivatives; arbutin; Water-soluble bioactive ingredients including adenosine; astaxanthin; polyphenol; And it may include one or more selected from the group consisting of natural extracts. However, this is an example, and the active ingredient may be selected from a variety of active ingredients that have skin-improving effects.

Water-soluble polymers can stabilize active ingredients. For example, water-soluble polymers can form a framework for supporting an active ingredient by forming a porous structure, and the active ingredient can be supported on this porous structure.

In embodiments, the water-soluble polymer may be freeze-dried along with the active ingredient and/or hydrotropic component. In other words, a freeze-dried structure containing the active ingredient can be formed. Through freeze-drying, problems such as browning, external shrinkage, and reduced potency can be prevented, and the formulation and efficacy of the composition can be maintained more stably. In particular, it is very environmentally friendly as it reduces the weight of the composition, reduces carbon emissions during the distribution process, and does not contain preservatives.

For example, water-soluble polymers can be freeze-dried to remove moisture to form porous structures, and active ingredients can be supported in these porous structures. However, this is an example, and various methods can be applied, such as the water-soluble polymer existing as a porous structure at room temperature and the active ingredient being supported thereon.

Depending on the embodiment, the porous structure may have an apparent density of 0.02 to 0.3 g/cm ³ , specifically 0.02 to 0.28 g/cm ³ , and more specifically 0.02 to 0.25 g/cm ³ . Here, “apparent density” may mean the overall density including the pore portion in a porous structure having a solid portion and a pore portion within an object, such as powder, particle, fiber, foam, etc. In the present invention, apparent density can be calculated as the mass of the porous structure divided by the total volume including both the solid portion and the pore portion. When the apparent density of the porous structure satisfies the above range, the shape of the composition is maintained stably, and the composition can be dissolved at a rapid rate when rehydrated.

Depending on the embodiment, the water-soluble polymer may be included in an amount of 5 to 55% by weight based on the total weight of the composition. If the water-soluble polymer is included in less than 5% by weight, the stability of the active ingredient may be reduced, for example, by precipitating the active ingredient, and if the water-soluble polymer is included in more than 55% by weight, it may interfere with the effectiveness of the active ingredient.

Depending on the embodiment, the water-soluble polymer is sodium hyaluronate, calcium hyaluronate, potassium hyaluronate, hyaluronic acid, hydrolyzed hyaluronic acid, and hydrolyzed sodium hyaluronate. , hyaluronic acid including hydrolyzed calcium hyaluronate, hydroxypropyltrimonium hyaluronate, sodium acetylated hyaluronate and sodium hyaluronate crosspolymer; Collagen and denatured collagen; algin; alginate; gelatin; carrageenan; starch; galactomannan; glucomannan; guar gum; Locust bean gum; xanthan gum; gellan; cellulose; polyvinylpyrrolidone (PVP); and polyvinyl alcohol (PVA). However, this is an example, and the water-soluble polymer may be selected from various water-soluble polymers that can form a porous structure.

Hydrotropic components are components that exhibit the “hydrotropy” phenomenon. Here, the hydrotropy phenomenon refers to a phenomenon in which the solubility in water increases when a third substance is added to a substance that is insoluble or poorly soluble in water, and the hydrotrope component is the third substance used to increase the solubility of the insoluble or poorly soluble substance. means substance.

For example, the hydrotrope component can stabilize the active ingredient through binding to the active ingredient. In the examples of the present application, as the hydrotrope component is added to the composition, the active ingredient can be stabilized even if it is contained in a high content, and the potency may not decrease over time. Specifically, when an active ingredient is supported on a framework formed by freeze-drying a water-soluble polymer, problems such as browning of the composition, shrinkage in appearance, or decrease in potency occur over time due to moisture absorption over time. In the examples of the application, these problems can be effectively solved as the active ingredient is stabilized within the framework by binding with the hydrotrope component.

Depending on the embodiment, the hydrotrope component may be included in an amount of 8 to 80% by weight relative to the total weight of the composition, specifically may be included in an amount of 8 to 50% by weight relative to the total weight of the composition, and more specifically may be included in an amount of 8 to 40% by weight, and the most Specifically, it may contain 8 to 30% by weight. Within the above range, the stability and efficacy of the active ingredient are maximized, and if the hydrotrope ingredient content is outside the above weight range, the active ingredient may precipitate, browning or external shrinkage may occur over time, and the potency may decrease. .

Depending on the embodiment, the hydrotrope component may include one or more selected from the group consisting of niacinamide, urea, caffeine, citrate, and salicylate. However, this is an example, and the hydrotropic component may be freely selected from components having hydrotropic properties.

Depending on the embodiment, the weight ratio of the hydrotrope component to the active ingredient may be 1:0.1 to 10, specifically 1:0.1 to 8, more specifically 1:0.1 to 5, and more specifically 1:0.1 to 8. : Can be 1 to 5. Within the above range, the stability and efficacy of the active ingredient are maximized, and if the weight ratio of the hydrotrope component to the active ingredient is outside the above range, the active ingredient may precipitate, browning or external shrinkage may occur over time, and the potency may decrease. It can be.

Depending on the embodiment, the weight ratio of the hydrotrope component to the water-soluble polymer may be 1:0.1 to 10, specifically 1:0.1 to 8, and more specifically 1:0.1 to 5. Within the above weight ratio range, the solubility of the active ingredient or the rehydration rate of the composition may be optimized, and if it is outside the above weight ratio range, the active ingredient may precipitate or the rehydration rate may decrease.

Depending on the embodiment, the composition in which the active ingredient is stabilized may further include at least one of a moisturizer, powder, oil, and additives. Here, the moisturizer is an ingredient that gives the composition a skin moisturizing function, the powder is an ingredient that gives the composition a function such as giving color to the composition or improving the feel of application, and the oil is an ingredient that dissolves fat-soluble ingredients or improves the feel of application of the composition. Ingredients, and additives are components that provide other functions to the composition and may include various substances such as antioxidants, binders, and metal ion sequestrants. In addition, this is an example, and the composition in which the active ingredient is stabilized may further include all kinds of additives known in the art, such as preservatives and flavorings.

Depending on the embodiment, the composition with stabilized active ingredients may be formulated as a solid or semi-solid form. For example, the composition can be formulated into a solid or semi-solid form by being freeze-dried. At this time, freeze drying may be carried out to stabilize the active ingredient through water-soluble polymer and/or hydrotrope component. The freeze-dried material is converted into a solid or semi-solid formulation in the form of a solid or powder as moisture is removed. In the case of the present invention, the active ingredient, water-soluble polymer, and hydrotrope component are mixed and then freeze-dried to form a solid or semi-solid formulation. It can be formulated into a solid form.

Depending on the embodiment, when the composition in which the active ingredient is stabilized is formulated in a solid or semi-solid form, the composition may be used after being rehydrated. Specifically, a solid or semi-solid composition can be prepared in liquid form by dissolving it in a solvent such as water, and then applied to the skin. However, this method of use is an example, and various methods can be used, such as applying the solid or semi-solid composition directly to the skin or ingesting it.

Depending on the embodiment, when a composition in which solid or semi-solid active ingredients are stabilized is rehydrated and used, the dissolution rate of the composition in water may be 50 mm ³ /sec, particularly 150 mm ³ /sec or more. At this time, the dissolution rate can be measured based on the time required for a composition measuring 1.2 cm wide x 1.2 cm long x 0.9 cm high to completely dissolve in 1 mL of solvent (particularly, water). In the examples of the present application, a composition in which the active ingredient is stabilized at a high content by water-soluble polymer and/or hydrotrope component can be easily used after rehydration at a fast dissolution rate of 50 mm ³ /sec, especially 150 mm ³ /sec or more. there is.

Depending on the embodiment, the composition in which the active ingredient is stabilized may have a hardness of 150 dyne/cm ² or more. At this time, hardness can be measured using a Fudoh rheo meter. For example, the maximum load value can be measured when applied and pressed at a speed of 30 cm/min to a depth of 5 mm using a 20 mm Φ spindle. In the present invention, as the active ingredient is stabilized by water-soluble polymer and/or hydrotrope component, hardness of 150 dyne/cm ² or more can be stably achieved.

Depending on the example, a composition with stabilized active ingredients may be stably maintained at a potency value of 90% or more 3 months after production compared to the potency value immediately after production. In the present invention, it is possible to prevent the titer from falling below 90% over time while containing a high content of the active ingredient through water-soluble polymer and/or hydrotrope components, thereby maximizing the skin improvement effect of the active ingredient. You can.

According to an embodiment of the present invention, a method for stabilizing an active ingredient is provided. According to the above method, a composition in which the above-mentioned active ingredients are stabilized can be prepared.

First, the active ingredient, water-soluble polymer, and hydrotrope component can be mixed to form a mixture. Mixing may be performed, for example, through a blender at room temperature, but is not limited to this and may be performed under various conditions and using various devices.

The mixture can then be freeze-dried. When the mixture is freeze-dried, moisture in the water-soluble polymer is removed to form a porous structure. The active ingredient is supported and stabilized in this porous structure, and the active ingredient can be additionally stabilized by attraction with the hydrotrope component.

According to an embodiment of the present invention, a cosmetic composition containing a composition with stabilized active ingredients may be provided.

Depending on the embodiment, the cosmetic composition of the present invention can be manufactured into various products effective in improving skin. In the present invention, “skin improvement” may mean effects that improve skin conditions such as antioxidant, anti-inflammatory, whitening, moisturizing, skin soothing, wrinkle improvement, and exfoliation, but is not limited to this and includes various known skin-related effects. can do.

Additionally, depending on the embodiment, the cosmetic composition of the present invention can be manufactured into functional cosmetics such as nutritional cream, essence, and ampoule, or basic cosmetics such as lotion and lotion. In addition, it can be manufactured into soap, detergent, cleansing cream, cleansing water, etc., or into color cosmetics such as lipstick, lip balm, mascara, blusher, shading, highlighter, makeup base, foundation, pact, concealer, skin cover, etc. . It can also be manufactured into hair cleaning products such as shampoo, rinse, hair conditioner, hair gel, etc. Additionally, for example, it may be manufactured as a product that is attached to the skin, such as a pack, hydrogel slimming patch, etc., or may be manufactured as a product that is sprayed on the skin, such as a mist or aerosol.

Depending on the embodiment, the cosmetic composition of the present invention may be provided in a formulation commonly prepared in the art. For example, it may be provided in the form of a solution, an emulsion obtained by dispersing an oil phase in an aqueous phase, an emulsion obtained by dispersing an aqueous phase in an oil phase, suspension, emulsion, gel, etc. Additionally, the cosmetic composition of the present invention can be formulated into solid or semi-solid form and processed into powder, bead, stick, etc.

Depending on the embodiment, the cosmetic composition of the present invention may contain other ingredients commonly used in the industry, such as thickeners, pH adjusters, isotonic agents, surfactants, and stabilizers, within the range that does not impair the effect of the present invention. It may further include topicals, preservatives, preservatives, ultraviolet absorbers, disinfectants, moisturizers, blockers, antioxidants, organic pigments, inorganic pigments, fragrances, vitamins, etc. The mixing amount of the above components can be easily selected by a person skilled in the art within a range that does not impair the purpose and effect of the present invention.

According to an embodiment of the present invention, a food composition containing a composition with stabilized active ingredients may be provided.

Depending on the embodiment, the food composition of the present invention can be manufactured into various products that are effective in improving skin. For example, the food composition of the present invention can be manufactured into products such as functional foods, nutritional supplements, health foods, food additives, special nutritional foods, processed meat products, seasoned foods, pickled foods, and dairy products. However, this is an example, and the food composition of the present invention can be manufactured into a product having various effects, such as having an anti-inflammatory effect such as improving inflammation caused by atopy, acne, insect bites, etc., depending on the embodiment.

Depending on the embodiment, the food composition of the present invention may be provided in various forms commonly prepared in the art. For example, it may be provided in dosage form such as powder, granule, pill, tablet, capsule, candy, syrup, beverage, etc.

Depending on the embodiment, the food composition of the present invention may contain other ingredients commonly used in the industry, such as flavor, extract, food additives such as nutritional ingredients, and food materials, within the range that does not impair the effect of the present invention. It may further include the like. For example, food ingredients include flavoring agents, natural carbohydrates, nutrients, vitamins, electrolytes, flavors, colorants, organic acids, protective colloidal thickeners, pH adjusters, stabilizers, preservatives, glycerin, alcohol, and carbonated beverages used in carbonated beverages. It may include topicals, pulp used in drinks, etc. For example, as a flavoring agent, natural flavoring agents including thaumatin, stevia extract, etc., or synthetic flavoring agents including saccharin, aspartame, etc. can be used, and natural carbohydrates include monosaccharides such as glucose and fructose, and horseradish. Disaccharides including sucrose and sucrose, polysaccharides including textrin and cyclotenstrin, and sugar alcohols including xylitol, sorbitol, and erythritol can be used. The mixing amount of the above components can be easily selected by a person skilled in the art within a range that does not impair the purpose and effect of the present invention.

Below, examples are shown to further explain the present invention in more detail, but the present invention is not limited thereto.

Preparation of examples and comparative examples

(1) Preparation of Examples 1 to 5

Examples of compositions were prepared using the ingredients listed in Table 1 below. The unit of ingredient content in Table 1 is weight%.

Specifically, Examples 1 and 2 are compositions in which the type of active ingredient was changed within the scope of the example, Example 3 is a composition in which the type of hydrotrope component was changed within the scope of the example, and Examples 4 and 5 were This is a composition in which the weight ratio of hydrotrope to active ingredient was changed within the scope of the example.

In addition, Table 2 below lists the weight ratio of the hydrotrope component to the water-soluble polymer or active ingredient.

division ingredient Example 1 Example 2 Example 3 Example 4 Example 5 water-soluble polymer Hyaluronic Acid 10 10 10 10 10 Collagen 1.9 1.9 1.9 1.9 1.9 Hydrotrope Ingredients Niacinamide 19.5 19.5 - 13.0 8.65 Caffeine - - 19.5 - - active ingredient Ascorbic Acid 65.5 - 65.5 72.0 76.35 Astaxanthin - 65.5 - - - additive Phenoxyethanol 0.1 0.1 0.1 0.1 0.1 moisturizer Propanediol 1.0 1.0 1.0 1.0 1.0 1,3-butylene glycol 1.0 1.0 1.0 1.0 1.0 panthenol 1.0 1.0 1.0 1.0 1.0 total 100 100 100 100 100

Example 1 Example 2 Example 3 Example 4 Example 5 Hydrotrope ingredient: water-soluble polymer 1 : 0.61 1 : 0.61 1 : 0.61 1:0.92 1:1.38 Hydrotrope Ingredients: Active Ingredients 1:3.36 1:3.36 1:3.36 1:5.54 1:8.83

(2) Preparation of Comparative Examples 1 to 4

A comparative example of a composition was prepared using the ingredients listed in Table 2 below. The unit of ingredient content in Table 2 is weight%.

Specifically, Comparative Example 1 is a composition that does not contain a hydrotrope component, Comparative Example 2 is a composition in which cyclodextrin, which performs a similar function, is added instead of the hydrotrope component, and Comparative Examples 3 and 4 are compositions containing hydrotrope versus active ingredient. This is a composition in which the weight ratio of was changed outside the scope of the example.

In addition, in Table 4 below, the content ratio with water-soluble polymer or active ingredient is listed based on the hydrotrope component.

division ingredient Comparative Example 1 Comparative example 2 Comparative Example 3 Comparative Example 4 water-soluble polymer Hyaluronic Acid 20 10 10 10 Collagen 11.4 1.9 1.9 1.9 Hydrotrope Ingredients Niacinamide - - 80 7 Cyclodextrin - 19.5 - - active ingredient Ascorbic Acid 65.5 65.5 5 78 Adenosine - - - - additive Phenoxyethanol 0.1 0.1 0.1 0.1 moisturizer Propanediol 1.0 1.0 1.0 1.0 1,3-butylene glycol 1.0 1.0 1.0 1.0 panthenol 1.0 1.0 1.0 1.0 total 100 100 100 100

Comparative Example 1 Comparative example 2 Comparative example 3 Comparative example 4 Hydrotrope ingredient: water-soluble polymer - 1 : 0.61 1 : 0.15 1:1.70 Hydrotrope Ingredients: Active Ingredients - 1:3.36 1:0.06 1:11.14

Experiment example

(1) Stability measurement experiment immediately after freeze-drying

After the compositions of Examples 1 to 5 and Comparative Examples 1 to 4 were freeze-dried, hardness and precipitation of active ingredients were measured, respectively, and are shown in Table 5. At this time, hardness was measured using a Fudoh rheo meter. Specifically, hardness was measured by measuring the maximum load value when applied and pressed at a speed of 30 cm/min to a depth of 5 mm using a 20 mm Φ spindle. In addition, a photograph of freeze-dried Example 1 taken with a scanning electron microscope (SEM) is shown in Figure 1.

As a result of the experiment, referring to FIG. 1, it can be confirmed that in Example 1, the active ingredient is stably contained in the porous structure. The same can be expected to be observed in Examples 2 to 5.

Additionally, in Examples 1 to 5, the hardness was measured to be 180 dyne/cm ² or more immediately after freeze-drying, confirming that the solid dosage form was stably formed. On the other hand, in Comparative Examples 1 to 4, the hardness was measured to be less than 130 dyne/cm ² immediately after freeze-drying, confirming that the solid dosage form was not stably formed.

In addition, in Examples 1 to 4, no precipitation of the active ingredient was observed immediately after freeze-drying, but in Comparative Examples 1 to 4, precipitation of the active ingredient was observed in all cases.

division Hardness immediately after freeze-drying (dyne/cm ² ) Precipitation immediately after freeze-drying Example 1 180 X Example 2 190 X Example 3 180 X Example 4 210 X Example 5 212 X Comparative Example 1 34 ● Comparative Example 2 42 ● Comparative Example 3 105 ● Comparative Example 4 121 ● ●: Active ingredient precipitates
X: Active ingredient does not precipitate

(2) Experiment to measure the ease of dissolution upon rehydration

The freeze-dried compositions of Examples 1 to 5 and Comparative Examples 1 to 4 were taken in a size of 1.2 cm wide x 1.2 cm long x 0.9 cm high, respectively, and dissolved in 1 mL of solvent (water). Time and speed were measured, and whether lumps remained after dissolution were observed, which are shown in Table 6. Among these, Example 1 and Comparative Example 1 are shown in Figures 2A and 2B. Specifically, Figure 2a is a photograph of Example 1 and Comparative Example 1 immediately after dissolution, and Figure 2b is a photograph of Example 1 and Comparative Example 1 60 seconds after dissolution.

As a result of the experiment, in the case of Examples 1 to 5, the dissolution rate was observed to be 50 mm ³ /sec, especially 150 mm ³ /sec or more, confirming the ease of use of the composition. However, in the case of Comparative Examples 1 to 4, the dissolution rate was observed to be 50 mm 3 /sec or more. As all were observed to be less than 50 mm ³ /sec, it was confirmed that the composition was inconvenient to use.

In addition, in Examples 1 to 5, it was confirmed that no lumps remained after dissolution and that the composition was completely dissolved. However, in Comparative Examples 1 and 2, the composition was not completely dissolved in water and the active ingredient was not evenly dispersed. Since there were lumps remaining, it is judged that it will not be easy to use.

division Dissolution time (sec) Dissolution rate (mm ³ / sec) Whether lumps remain after dissolution Example 1 One 1296 X Example 2 3 432 X Example 3 3 432 X Example 4 4 324 X Example 5 8 162 X Comparative Example 1 63 20.57 ● Comparative Example 2 71 18.25 ● Comparative Example 3 28 46.28 X Comparative Example 4 31 41.80 X ●: Clumps remain.
X: All dissolved with no remaining lumps

(3) Temporal stability measurement experiment

After freeze-drying the compositions of Examples 1 to 5 and Comparative Examples 1 to 4, respectively, they were stored for 3 months at 25°C and 60% relative humidity or 40°C and 75% relative humidity, and then the color for each , size and hardness were measured and shown in Table 7. At this time, in the case of Comparative Examples 1 and 2, the hardness could not be measured because the formulation was not maintained after 3 months.

As a result of the experiment, in the case of Examples 1 to 5, no change in color or size was observed, and there was no significant difference in hardness compared to immediately after freeze-drying, confirming that the composition remained stable over time. .

On the other hand, in the case of Comparative Examples 1 to 4, browning in color and shrinkage in appearance occurred after 3 months, and a decrease in hardness was observed compared to immediately after freeze-drying, confirming the lack of stability of the composition. there was.

division Stability - Color Stability - Size Stability - physical properties (hardness) 25℃,
60%RH 40℃,
75%RH 25℃,
60%RH 40℃,
75%RH 25℃,
60%RH 40℃,
75%RH Example 1 Good Good Good Good 179 181 Example 2 Good Good Good Good 181 190 Example 3 Good Good Good Good 177 183 Example 4 Good Good Good Good 205 211 Example 5 Good Good Good Good 217 210 Comparative Example 1 ● ● ● ● not measurable not measurable Comparative Example 2 ● ● ● ● not measurable not measurable Comparative Example 3 ○ ◐ ○ ◐ 104 79 Comparative Example 4 ○ ◐ ◐ ◐ 46 42 * Stability - color judgment criteria
●: Browning to brown
◐: Browning to yellow
○: Browning to light yellow
* Stability - size judgment criteria
●: Shrinkage of more than 90% compared to the original size
◐: Shrinkage of 10-60% compared to existing size
○: Shrinkage to less than 10% of original size

(4) Potency change measurement experiment

Immediately after freeze-drying the compositions of Examples 1 to 5 and Comparative Examples 1 to 4, the content (i.e., titer) of the active ingredient remaining in each composition was measured through HPLC (High Performance Liquid Chromatography). . In addition, after storing the compositions for 3 months at 25°C and 60% relative humidity conditions or 40°C and 75% relative humidity conditions, respectively, the content (titer) of the active ingredients remaining in each composition was measured through HPLC. Next, the ratio (%) of the titer after 3 months compared to the titer immediately after freeze-drying is shown in Table 8 and Figure 3.

As a result of the experiment, in the case of Examples 1 to 5, it was measured that the titer was maintained at more than 90% even after 3 months, confirming that the titer was maintained stably even if a high content of the active ingredient was contained.

On the other hand, in the case of Comparative Examples 1 to 4, the titer was measured to be less than 85% after 3 months, and it was confirmed that due to lack of stability, the active ingredient was not maintained stably over time and the titer decreased.

division Potency change (%) 25℃, 60%RH 40℃, 75% RH Example 1 99.5 99.8 Example 2 102.1 100.6 Example 3 101.2 100.7 Example 4 100.8 99.4 Example 5 100.0 97.8 Comparative Example 1 66.7 45.6 Comparative Example 2 69.9 44.5 Comparative Example 3 82.3 82.9 Comparative Example 4 83.7 77.1

As the specific parts of the present invention have been described in detail above, it is clear to those skilled in the art that these specific techniques are merely preferred embodiments and do not limit the scope of the present invention. It will be obvious. Accordingly, the actual scope of the present invention will be defined by the appended claims and their equivalents.

Claims (14)

A composition with stabilized active ingredients,
Contains the above active ingredients, water-soluble polymers, and hydrotrope components,
The active ingredient is stabilized by the water-soluble polymer and the hydrotrope component,
The weight ratio of the hydrotrope component to the water-soluble polymer is 1:0.1 to 10,
The composition is a freeze-dried formulation with stabilized active ingredients. According to claim 1,
A composition with a stabilized active ingredient, wherein the active ingredient is a component that is oxidized by at least one of air, light, heat, and moisture. According to claim 1,
A composition with a stabilized active ingredient, wherein the active ingredient is supported on a porous structure formed by the water-soluble polymer and stabilized through bonding with the hydrotrope component. According to claim 1,
A composition in which the active ingredient is stabilized, wherein the active ingredient is contained in an amount of 6 to 80% by weight based on the total weight of the composition. According to claim 1,
The active ingredients include water-soluble vitamins including ascorbic acid or its derivatives; Oil-soluble vitamins including retinoic acid or its derivatives; arbutin; Water-soluble bioactive ingredients including adenosine; astaxanthin; polyphenol; And a composition with stabilized active ingredients, comprising at least one selected from the group consisting of natural extracts. According to claim 1,
A composition with stabilized active ingredients, wherein the water-soluble polymer is contained in an amount of 5 to 55% by weight based on the total weight of the composition. According to claim 1,
The water-soluble polymers include sodium hyaluronate, calcium hyaluronate, potassium hyaluronate, hyaluronic acid, hydrolyzed hyaluronic acid, hydrolyzed sodium hyaluronate, and hydrolyzed Hyaluronic acid, including calcium hyaluronate, hydroxypropyltrimonium hyaluronate, sodium acetylated hyaluronate and sodium hyaluronate crosspolymer; Collagen and denatured collagen; algin; alginate; gelatin; carrageenan; starch; galactomannan; glucomannan; guar gum; Locust bean gum; xanthan gum; gellan; cellulose; polyvinylpyrrolidone (PVP); and polyvinyl alcohol (PVA). A composition containing stabilized active ingredients, comprising at least one selected from the group consisting of polyvinyl alcohol (PVA). According to claim 1,
The hydrotrope component includes at least one selected from the group consisting of niacinamide, urea, caffeine, citrate, and salicylate. A composition with a stabilized active ingredient. According to claim 1,
A composition with stabilized active ingredients, wherein the hydrotrope component is contained in an amount of 8 to 80% by weight based on the total weight of the composition. According to claim 1,
A composition in which the active ingredient is stabilized, wherein the weight ratio of the hydrotrope component to the active ingredient is 1:0.1 to 10. According to claim 1,
A composition with stabilized active ingredients, wherein the composition with stabilized active ingredients is formulated in a solid or semi-solid form. delete According to claim 1,
The active ingredient-stabilized composition has a hardness of 150 dyne/cm ² or more. A cosmetic composition for improving skin, comprising the composition in which the active ingredient according to claim 1 is stabilized.