KR102562217B1 - Film composition - Google Patents

Abstract

The present invention relates to a film useful in personal care compositions, wherein the film is stable in the formulation of the composition, but releases active ingredients (including colorants) as it decomposes during use. More specifically, a film made of one or more water-insoluble polymers and one or more water-insoluble inorganic salts or inorganic oxides does not decompose in the formulation state, but is decomposed when a certain pressure is applied during use, and active ingredients (including colorants) it will be released

Description

Film composition {Film composition}

The present invention relates to a film composition contained in a personal care composition. More specifically, it relates to a film composition that is stable within the composition formulation, but is decomposed by pressure applied when the personal care composition is used, and has a characteristic of releasing active ingredients contained in the film composition.

Efforts have been made to effectively deliver active ingredients during use as well as differentiated appearances by including capsules or films containing various functions in personal care compositions.

Among them, as an example of a prior patent containing a film in a toothpaste composition, Korean Patent Application No. 10-2015-7017700 discloses a water-soluble film, wherein the water-soluble film contains 50% or more polyvinyl alcohol and 50% or less water-soluble film. It contains a polymer matrix containing cellulose esters. In addition, as another example, the film in Korean Patent Application No. 10-2008-7017832 contains a first polymer having a first solubility and a second polymer having a second solubility, and the film in water The first solubility is higher than the second solubility.

Since both films according to the above two prior patents require water-soluble polymers, and Korean Patent Application No. 10-2015-7017700 is a water-soluble film, it is difficult to maintain stability in the formulation as well as during manufacture. There was a concern that the active ingredient in the film would be released before use.

Therefore, it is an object of the present invention to solve the above problems and provide a film composition having excellent stability. More specifically, the problem to be solved by the present invention is to provide a film composition in which the film composition is decomposed and the active ingredient is released only when used, and a film prepared therefrom. In addition, it is to provide a personal care composition including a film that is stably maintained without release of active ingredients before use, for example, in a manufacturing step, a distribution step, or a storage step.

In order to solve the above problems, the present invention is a film composition contained in a personal care composition, a film composition containing at least one water-insoluble polymer and at least one water-insoluble inorganic salt or inorganic oxide, a film prepared therefrom, and a personal care composition comprising such a film.

The present inventors have found that a film prepared using one or more water-insoluble polymers and one or more water-insoluble inorganic salts or inorganic oxides maintains stability in the manufacturing step of a toothpaste composition containing the same, and is not affected by brushing pressure applied during use of the toothpaste composition. It was confirmed that there was an effect of rapidly releasing the active ingredient present in the film by decomposition, and completed the present invention.

More specifically, the film composition according to the present invention will be described.

The film composition according to the present invention is intended to be included in a personal care composition, and includes one or more water-insoluble polymers and one or more water-insoluble inorganic salts or inorganic oxides.

In the present invention, one or more water-insoluble polymers are included as components forming the film matrix, and are substantially insoluble, non-hydrophilic, and substantially insoluble in water in the formulation prior to use and under conditions of use. The term 'substantially insoluble' or 'substantially insoluble' means that it is soluble in water at less than 1% by weight, less than 0.5% by weight, less than 0.1% by weight, more preferably less than 0.01% by weight.

The water-insoluble polymer according to the present invention can be used without limitation as long as it is suitable for use in the human body, particularly for oral cavity, and is safe. For example, hydrophobically modified acrylic copolymers and derivatives thereof; ethylene-vinyl acetate copolymer, cross-linked poly(vinyl pyrrolidone), poly(vinyl acetate) (PVAc); cellulose derivatives including cellulose acetate, cellulose nitrate, alkyl cellulose (eg, ethyl cellulose, butyl cellulose, isopropyl cellulose, methylcellulose, etc.), cellulose acetate phthalate, unneutralized carboxymethyl cellulose, shellac; Silicone polymers (eg, dimethylsilicone, etc.), polyester, polyurethane, nylon, gums (eg, xanthan gum, carrageenan gum, etc.), polyethylene, polypropylene, or mixtures of two or more thereof may be included, Not limited to this. A preferred acrylic copolymer is a film forming polymer, and more specifically, the weight average molecular weight of the acrylic copolymer may be about 20,000 or more, more preferably about 50,000 or more and about 1,000,000 or less, more preferably about 900,000 or less. Preferably, a water-insoluble cellulose derivative may be used, and more preferably, an alkyl cellulose may be used.

The water-insoluble polymer according to the present invention may be included in 10 to 65% by weight, more preferably 30 to 50% by weight, based on the total weight of the film composition. When included in less than 10% by weight, it is difficult to maintain the stability of the film, and when included in more than 65% by weight, there is a problem in that film production is difficult due to high viscosity of the film during film production.

In the present invention, one or more water-insoluble inorganic salts or inorganic oxides are supported in the film matrix, and the water-insoluble inorganic salts or inorganic oxides help the film matrix to collapse (decompose) by a certain external pressure applied to the film. It is substantially insoluble, non-hydrophilic, and substantially insoluble in water in the formulation prior to use and under conditions of use. The term 'substantially insoluble' or 'substantially insoluble' means that it is soluble in water at less than 1% by weight, less than 0.5% by weight, less than 0.1% by weight, more preferably less than 0.01% by weight.

The water-insoluble inorganic salt or inorganic oxide according to the present invention can be used without limitation as long as it is suitable for use in the human body, especially for oral use, and is safe. For example, silicas (eg, colloidal silica, dental type silica, silicon dioxide, precipitated silica, etc.), magnesium oxide, calcium carbonate, titanium oxide, dicalcium phosphate dehydrate, inorganic calcium, or these Mixtures of two or more of are included, but are not limited thereto. Preferably, silicas can be used, and silicon dioxide can be used more preferably.

The water-insoluble inorganic salt or inorganic oxide according to the present invention may be included in 10 to 40% by weight, more preferably 20 to 40% by weight, based on the total weight of the film composition. When included in less than 10% by weight, the film does not decompose even at a certain pressure or more, so there is a problem with the rapid release of the active ingredient, and when included in more than 40% by weight, it is difficult to maintain film stability before use.

In the film composition according to the present invention, the weight ratio of the water-insoluble polymer to the water-insoluble inorganic salt or inorganic oxide is 1: 1 to 100: 1 (water-insoluble polymer: water-insoluble inorganic salt or inorganic oxide), more preferably 1: 1 to 100: 1. 1 to 70:1, most preferably 3:1 to 40:1. If the weight ratio is out of the above, there is a problem that it is difficult to maintain a stable form in the composition because it does not decompose quickly or decomposes too quickly.

In the film composition according to the present invention, the water-soluble polymer is not substantially included. More specifically, less than 30% by weight, less than 15% by weight, more preferably less than 10% by weight, even more preferably less than 5% by weight, still more preferably less than 1% by weight, and most preferably less than 0.1% by weight relative to the weight of the total film composition. can be included as In addition, the water-soluble polymer is less than 75% by weight, less than 50% by weight, less than 30% by weight, less than 10% by weight, more preferably less than 5% by weight, and most preferably less than 1% by weight based on the weight of the polymer included in the total film composition. can According to a specific embodiment of the present invention, when a film composition including hydroxymethylcellulose, which is a water-soluble polymer, is prepared, the stability is not maintained over time and the film is decomposed (collapsed), which is regardless of the storage temperature. Could know.

In the film composition according to the present invention, various components commonly included in film compositions included in personal care compositions may be further included. For example, it may contain plasticizers or active ingredients, but is not limited thereto.

The plasticizer is used to impart sufficient flexibility to the film, and varies depending on the type of polymer included in the film composition and its prescription, but for example, polypropylene glycol, castor oil, Sorbitol, glycerin, or polyethylene glycol and mixtures thereof may be used, but are not limited thereto.

The active ingredient refers to a material that provides an aesthetic or decorative effect to a personal care composition or exhibits desired efficacy in the composition when used for its intended use, and includes, for example, medicinal agents, flavoring agents, and coloring agents.

Examples of the medicinal agent include, but are not limited to, sodium fluoride, sodium monofluorophosphate, tin fluoride, chlorhexidine, allantoin chlorohydroxyaluminate, aminocaproic acid, tranexamic acid, zinc chloride, pyridoxine hydrochloride , Tocopherol Acetate, Cetylpyridinium Chloride, Isopropylmethylphenol, Sulfur Extract, Centella Quantitative Extract, Green Tea Extract, Phosphoric Acid Compounds (Sodium Phosphate, Disodium Phosphate, Trisodium Phosphate, Sodium Tripolyphosphate, Tetrasodium Pyrophosphate, etc.) Alternatively, enzymes and the like may be used alone or in combination of two or more.

Examples of flavoring agents include, but are not limited to, sodium saccharin, xylitol, erythritol, aspartame, stevioside, peppermint oil, spearmint oil, menthol, menthol derivatives, etc. alone or in combination.

The colorant includes, for example, but is not limited thereto, a lake pigment, iron oxide, and a water-insoluble pigment other than a water-soluble colorant, and the like may be used alone or in combination.

In the film composition according to the present invention, the solvent may be various types of solvents commonly used in the art depending on the type and prescription of the components included in the film composition, but is not limited thereto, for example, lower carbon alcohol can be used, and in a specific embodiment of the present invention, ethanol was used as a solvent. The solvent used in the film composition according to the present invention is dried and volatilized in the film production step.

A film composition according to the present invention is made into a film.

In the present invention, the film includes mixing and drying the film composition, and may be prepared according to various methods commonly employed in the art.

In the present invention, the film may be of various shapes or shapes. Also, the film may be of any desired shape and thickness, and may be present as multiple plates, fragments, or pieces. When the film is produced in one layer or several layers, the final thickness is 300um or less, preferably 10um - 300um. If it is less than 10um, it may be broken during the manufacturing process, and if it is more than 300um, it may be difficult to elute the active ingredient because it is not decomposed even during use.

The film according to the present invention does not disintegrate (decompose) before use, but only disintegrates (decomposes) when used, so that the active ingredient in the film is rapidly released.

In the present invention, 'use' means to use the personal care composition according to the purpose or function, and for example, when the personal care composition is formulated as a toothpaste, the use will mean brushing teeth. In addition, 'before use' refers to all predictable steps (eg, storage step, distribution step, etc.) from film manufacturing to before use, including the manufacturing step of the film and the manufacturing step of the personal care composition. .

The factor causing collapse (decomposition) of the film during use is pressure, which means the pressure applied when using the personal care composition, more specifically, the pressure applied when using the personal care composition for oral cavity, and more specifically, the toothpaste formulation It may mean the pressure applied when using the personal care composition for oral cavity.

The film according to the present invention maintains safety under the pressure applied during mixing for toothpaste production, which means that water-insoluble inorganic salts or inorganic oxides among the components of the film do not absorb moisture or oil in the toothpaste during toothpaste production, After manufacturing, it absorbs moisture or oil present in toothpaste little by little, and the strength of the film becomes weaker than at the time of manufacture. The pressure of the decomposed film during brushing is 500 cm ² or less, more preferably 400 g/cm ² below If it is 500 g / cm ² or more, it is not easy for the film to be broken, and excessive force is applied to break the film, which can damage the gums in the case of oral care and damage the skin in personal care products.

In the present invention, disintegration (decomposition) means a state in which the film does not maintain its structure and shape, for example, means that the film is divided into several parts, whereby components contained in the film, in particular active ingredients, are released. It can be.

In addition, the film according to the present invention has temperature stability and is stably maintained without collapse (decomposition) in the temperature range of room temperature to 60 °C.

In addition, a personal care composition comprising the film according to the present invention is provided.

In the present invention, the film may be appropriately adjusted according to the function, purpose, target of use, etc. of the personal care composition, but may be included in 0.01-5.00% by weight, more preferably 0.1-0.5% by weight, based on the total weight of the personal care composition. there is. Outside the above weight% range, if the weight% is less than invisible, if the weight% is exceeded, there is a problem that agglomerates during use or increases the manufacturing cost.

In addition to the film, the personal care composition according to the present invention may further include various components that may be commonly included in personal care compositions. More specifically, in the case of a personal care composition for oral cavity, for example, an active ingredient, a wetting agent, an abrasive, a medicinal agent, a sweetener, a pH adjuster, a preservative, a binder, a flavoring agent, a foaming agent, or a mixture of two or more thereof may be contained, Not limited to this.

The abrasive is, for example, one or more of precipitated silica, silica gel, zirconium silicate, calcium monohydrogen phosphate, anhydrous calcium monohydrogen phosphate, hydrous alumina, precipitated calcium carbonate, heavy calcium carbonate, calcium pyrophosphate, insoluble metaphosphate, and aluminum silicate. The degree of abrasion of the final product may be measured using a radiographic sample tooth wear amount measurement method or a wear surface tooth specimen area measurement method adopted as a standard method in the United States or England to have a value of 200 or less, but is not limited thereto.

Humectants not only prevent dryness and solidification when exposed to air and provide gloss, but also serve to give a sweetening effect depending on the type. For example, one or more of concentrated glycerin, glycerin, sorbitol aqueous solution, amorphous sorbitol aqueous solution, polyethylene glycols, and propylene glycol may be used, but is not limited thereto. The amount used may be 1 to 70% by weight relative to the total toothpaste composition.

The binder serves to prevent separation between the solid powder component and the liquid component, and any type of water-soluble polymer may be used. For example, carboxymethyl cellulose sodium, carbomer, carrageenan, xanthan gum, alginates, etc. can be used, and as a foaming agent, anionic and nonionic surfactants such as sodium alkyl sulfate, sodium lauryl sulfate, sucrose fatty acid ester, sorbitan fatty acid ester, etc. and the like, but is not limited thereto.

The foaming agent enhances the feeling of use of the product, helps the cleaning action, accelerates the dispersion and penetration of other active ingredients, and reduces the interfacial tension to easily remove foreign substances in the oral cavity. As the foaming agent, for example, sodium Lauring sulfate as an anionic surfactant, a copolymer of polyoxyethylene polyoxypropylene as a nonionic surfactant (poloxamer), polyoxyethylene hydrogenated castor oil, polyoxyethylene sorbitan fatty acid ester, etc. This may be used, but is not limited thereto.

The medicinal agent is, for example, one or more fluorine compounds selected from sodium fluorophosphate, sodium fluoride, amine fluoride and tin fluoride, sodium pyrophosphate, potassium pyrophosphate or sodium acid pyrophosphate, enzymes, aminocaproic acid, allantoin or One or more allantoin derivatives or vitamins may be selectively used, but are not limited thereto.

As the sweetening agent, for example, sodium saccharin (hydrate), xylitol, erythritol, aspartame, etc. may be used, and as the pH adjusting agent, for example, sodium phosphate, disodium phosphate, citric acid, triethanolamine, etc. may be used, and the preservative As examples, methyl paraoxybenzoate, sodium benzoate and the like can be used. However, it is not limited to these.

As the flavoring agent, for example, peppermint oil and spearmint oil may be mixed and used, and as other additives, enzymes such as textranase may be used, but are not limited thereto.

In addition, the remaining amount of water may be included in 20% or less, but is not limited thereto.

Examples of personal care compositions in which the film can be used include cosmetics, toiletries, and topical health care personal care products, and more specifically, oral hygiene products (eg, toothpaste, oral suspension, and mouth care products); shampoo; chemical and non-chemical hair curling and hair straightening products; hair styling and hair conditioning products; lotions and creams for coloring nails, hands, feet, face, scalp and/or body hair; face and body makeup; nail care products; astringent; deodorant; antiperspirants; depilatory agent; creams and lotions for skin protection (such as sunscreens); skin and body cleansers; skin conditioner; skin toner; skin firming compositions; liquid soap; bar soap; bath products; and shaving products, any of which may additionally contain pharmaceutical, herbal, and/or neutraceutical ingredients.

The forms of these personal care products are not limited, but include, but are not limited to, liquids, gels, sprays, emulsions (eg, lotions and creams, etc.), shampoos, pomades, foams, ointments, tablets, sticks ( For example, lip care products), makeup, suppositories, any of which can be applied to the mouth, skin or hair, and are typically removed by rinsing with, for example, water or shampoo or soap. It is designed to remain in contact until Gels can be soft, hard or compressible. Emulsions can be oil-in-water, water-in-oil, water-and-silicone, or multi-phase. The spray may be a non-pressurized aerosol or a pressurized aerosol delivered from a manually pumped, finger-actuated sprayer.

The present invention relates to a film useful in a personal care composition, particularly a personal care composition for oral cavity. The film is stable in the composition formulation, but is decomposed when a certain pressure or more is applied, and components contained in the film composition, such as It has the effect of releasing functional ingredients or colorants.

According to the present invention, the film composition can be used for separate inclusion from other components to be included in the personal care composition, and depending on the characteristics of the material contained in the film composition, aesthetic or long-term effects caused by pressure applied when the personal care composition is used Changes (eg, color change, flavor change, etc.) may be used, and various applications are possible, such as manufacturing a personal care composition containing a component with weak stability among functional materials as a film composition.

Hereinafter, examples and experimental examples will be described in detail to explain the present invention in detail. However, the examples and experimental examples according to the present invention may be modified in many different forms, and the scope of the present invention should not be construed as being limited to the examples and experimental examples detailed below. Examples and experimental examples of the present invention are provided to more completely explain the present invention to those skilled in the art.

manufacturing example

The film compositions of Examples 1 to 4 and Comparative Examples 1 to 10 were prepared with the ingredients and composition ratios shown in Tables 1 and 2 below. That is, all the ingredients listed in Table 1 or Table 2 (eg, water-insoluble polymers, water-insoluble inorganic salts or inorganic oxides, powders or useful ingredients such as active ingredients) were first dispersed in ethanol, and finally mixed with ethanol. Evaporation produced a film composition. The thickness of the obtained film was approximately 0.2 mm. It was cut into square sizes and added to toothpaste at 0.3% by weight.

In addition, the toothpaste composition of the present invention may be formulated with components used in conventional toothpaste compositions. In the dentifrice composition of the present invention, first, a small amount of additives are mixed in a liquid part composed of purified water and a wetting agent, and then an abrasive is mixed. In addition to this, a foaming agent, flavoring agent and other additives were blended and mixed according to a conventional method for preparing toothpaste to prepare toothpaste.

last name name Ingredient ratio silica 20.0 Agriglycerin (98%) 30.0 Sorbitol aqueous solution (70%) 30.0 sodium lauryl sulfate 1.0 Sodium Carboxymethyl Cellulose 0.5 xanthan gum 0.5 sodium fluoride 0.22 Spices 1.0 sodium saccharin 1.0 Citric Acid, TEA Appropriate amount Purified water To 100

The film composition except for the toothpaste will be described in more detail with Examples and Comparative Examples of the present description below.

Ingredients Example 1 Example 2 Example 3 Example 4 Ethyl Cellulose 30 30 50 50 Hydroxymethyl Cellulose silica 20 35 20 35 pigment One One One One Centella Quantitative Extract 0.01 0.01 0.01 0.01 glycerin 10 10 10 10 ethanol TO 100 TO 100 TO 100 TO 100

Ingredients Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Comparative Example 6 Comparative Example 7 Comparative Example 8 Comparative Example 9 Comparative Example 10 ethyl cellulose 30 50 30 30 30 30 Hydroxymethyl Cellulose 10 10 20 20 10 10 20 20 silica 20 35 20 35 20 35 20 35 pigment One One One One One One One One One One Centella quantification
extract 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 0.01 glycerin 10 10 10 10 10 10 10 10 10 10 ethanol TO 100 TO 100 TO 100 TO 100 TO 100 TO 100 TO 100 TO 100 TO 100 TO 100

Experimental example 1. Evaluation of the long-term stability of the film in the formulation

The prepared film is cut into square sizes (0.2 mm in width and length, respectively), added to toothpaste at 0.3% by weight and mixed (mixing during manufacture to uniformly distribute the film in toothpaste), in the final toothpaste containing the film For each temperature (60 ℃, 50 ℃, 40 ℃, room temperature), one month stability was evaluated.

Stability good: O Stability poor: x Broken by mixer: -

sample number Film stability after mixing 1 month stability
(60℃) 1 month stability (50℃) 1 month stability (40℃) 1 month stability
(normal temperature) Example 1 0 0 0 0 0 Example 2 0 0 0 0 0 Example 3 0 0 0 0 0 Example 4 0 0 0 0 0 Comparative Example 1 - - - - - Comparative Example 2 - - - - - Comparative Example 3 - - - - - Comparative Example 4 - - - - - Comparative Example 5 0 0 0 0 0 Comparative Example 6 0 0 0 0 0 Comparative Example 7 0 X X X X Comparative Example 8 0 X X X X Comparative Example 9 0 X X X X Comparative Example 10 0 X X X X

In the case of Comparative Examples 1 to 4, the film was formed, but was broken by the friction of the mixer during manufacture, so that the film in the toothpaste was not visible after mixing. In Comparative Examples 5 and 6, the films were stably maintained in the toothpaste. Comparative Examples 7 to 10 were good at the time of manufacture, but did not remain stable for each temperature after 1 month.

Experimental example 2. Evaluation of film stability during brushing

When brushing teeth with a constant pressure for at least 30 seconds with a product that has been neglected for one month and then spitting it out, the stability of the film in the formulation was evaluated and confirmed.

When brushing your teeth, the film is disassembled and invisible: O

Film does not disintegrate when brushing: X

Products that cannot be evaluated (the film decomposes after manufacturing or after 1 month): -

sample number Presence of film after brushing teeth Example 1 0 Example 2 0 Example 3 0 Example 4 0 Comparative Example 1 - Comparative Example 2 - Comparative Example 3 - Comparative Example 4 - Comparative Example 5 X Comparative Example 6 X Comparative Example 7 - Comparative Example 8 - Comparative Example 9 - Comparative Example 10 -

In the case of Examples 1 to 4, the film was decomposed during brushing in the products aged 1 month and the film was not found in the spit-out part, but in the case of Comparative Examples 5 and 6, the film was decomposed in the product aged 1 month It was released as it is without being turned on. Also, in Comparative Examples 7 to 10, the film was not found from the discharge for brushing teeth.

Claims (12)

As a film composition contained in a personal care composition,
containing at least one water-insoluble inorganic salt or inorganic oxide, and at least one water-insoluble polymer;
The water-insoluble inorganic salt or inorganic oxide includes silica in an amount of 10 to 40% by weight based on the total weight of the film composition,
The water-insoluble polymer is a hydrophobically modified acrylic copolymer, a derivative thereof, Cross-linked poly(vinyl pyrrolidone), poly(vinyl acetate) (PVAc), cellulose acetate, cellulose nitrate, alkyl cellulose, cellulose acetate phthalate, unneutralized carboxymethyl cellulose, cellulose derivatives including shellac, ethylene- At least one selected from the group consisting of vinyl acetate copolymers, silicone polymers including dimethylsilicone, polyesters, polyurethanes, nylons, gums, polyethylenes, and polypropylenes, and contained in an amount of 10 to 65% by weight based on the total weight of the film composition. become,
The film composition, characterized in that the film composition does not contain hydroxymethylcellulose. delete The film composition according to claim 1, wherein the silica is at least one selected from the group consisting of colloidal silica, dental type silica and silicon dioxide. The film composition according to claim 1, wherein the water-insoluble polymer is contained in an amount of 30 to 50% by weight based on the total weight of the film composition. The film composition according to claim 1, wherein the water-insoluble inorganic salt or inorganic oxide is contained in an amount of 20 to 40% by weight based on the total weight of the film composition. The film composition according to claim 1, wherein the film composition contains an active ingredient including a pigment. The film composition according to claim 1, wherein the film composition contains a plasticizer including propylene glycol, glycerin, polyethylene glycol, castor oil, or a mixture of two or more thereof. The film composition according to claim 1, wherein the personal care composition is a personal care composition for oral cavity. A film made of the film composition of any one of claims 1 and 3 to 8 and degraded at a pressure of 500 g/cm ² or less. 10. The film of claim 9, wherein the film is insoluble in water. A personal care composition comprising the film of claim 9. 12. The method of claim 11, wherein the personal care composition is an oral care product comprising toothpaste; shampoo; chemical and non-chemical hair curling and hair straightening products; hair styling and hair conditioning products; lotions and creams for coloring nails, hands, feet, face, scalp or body hair; face and body makeup; nail care products; astringent; deodorant; antiperspirants; depilatory agent; creams and lotions for skin protection; skin and body cleansers; skin conditioner; skin toner; skin firming compositions; liquid soap; bar soap; bath products; And a personal care composition characterized in that formulated with at least one selected from the group consisting of shaving products.