TW202302062A - Non-erosive composition for tooth whitening comprising high-content peroxide - Google Patents

Abstract

The present invention relates to a gel composition for teeth whitening which is applied to the surface of teeth. The composition may comprise: a film-forming agent including at least one type selected from polyvinyl acetate (PVAc) and ethyl acetate (EC); a peroxide; and a volatile solvent. The composition can continuously maintain the whitening effect since the formulation thereof can be maintained even in moist conditions such as saliva.

Description

Non-erosive tooth whitening compositions containing high levels of peroxides

This application claims priority based on Korean Patent Application No. 10-2021-0024925 filed on February 24, 2021 and Korean Patent Application No. 10-2021-0089984 filed on July 8, 2021, the specification and All the contents disclosed in the drawings are used in this application. The present invention relates to a tooth whitening composition, and more particularly, to a tooth whitening composition comprising a high content of hydrogen peroxide.

Recently, in response to consumers' requests for teeth whitening, products that impart a tooth whitening effect have been actively developed.

Various forms of teeth whitening products have been developed, among which, for products in the form of patches attached to teeth to impart a whitening effect, there is the inconvenience of being attached to teeth with hands and needing to be peeled off after use. In order to solve these inconveniences, a product in the form of a gel type that dries quickly after being applied to teeth to form a film-like coating is being developed. Products in the form of gels that are applied to teeth can be applied to the surface of the teeth without putting the hands directly into the mouth, so it is convenient to use, but there is a problem that the dosage form cannot be maintained and is eroded due to saliva, and the staying power is reduced question. Not only that, but there was also a problem that the eroded and dissolved gel was continuously ingested into the esophagus.

In order to improve these problems, gel-type products that use non-water-soluble materials so as not to be eroded by saliva have been studied, but for dosage forms that add hydrogen peroxide or water, there has been a decrease in the solubility of non-water-soluble materials. And may induce the problem of dosage form instability.

industrial availability

The present invention provides a product for whitening teeth.

technical issues

Therefore, the problem to be solved by the present invention is to provide a novel composition for tooth whitening that can maintain the stability of the dosage form without being eroded in the oral environment.

Technical solutions

In order to solve the above-mentioned problems, it is intended to provide a non-erosive gel composition for tooth whitening.

A specific example of the present invention can provide a tooth whitening gel composition as a tooth whitening gel composition coated on the tooth surface.

The above composition comprises more than one film forming agent selected from polyvinyl acetate (PVAc) and ethyl acetate (EC), a peroxide and a volatile solvent.

Relative to the total weight of the composition, the content of the above-mentioned peroxide may exceed 2.5% by weight and be 15% by weight or less.

Relative to the total weight of the above-mentioned composition, the content of the above-mentioned film-forming agent may be 5 to 30% by weight.

The above composition may also comprise hydroxypropylmethylcellulose (HPMC) or an ester thereof. Here, the above-mentioned ester of HPMC may include hydroxypropylmethylcellulose phthalate (HPMCP).

The aforementioned HPMC or its ester may be present in a composition mixed with a peroxide and/or a film former, and the aforementioned composition may be provided as a single composition.

The above-mentioned HPMC or its ester compound can be in the composition, and the weight ratio of film forming agent:HPMC or its ester compound is 1:0.1 to 1.5.

The above composition contains 3 to 25% by weight of water, and the peroxide may exist as an aqueous peroxide solution or in a state of being dissolved in a volatile solvent.

The above composition may substantially not contain one or more aggressive polymers selected from the group consisting of polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA) and carbomer.

The above-mentioned composition may not include the polymer precipitated from the following solution: the solution is based on a room temperature of 22 to 25° C. and 5 ml, relative to the total weight of the composition, comprising 9% by weight to 11% by weight of peroxide and 15% by weight. % by weight to 20% by weight of water.

A specific example of the present invention can provide a tooth whitening product, the tooth whitening product can be a tooth whitening product that forms a coating film on the tooth surface, and it includes: a tooth whitening product containing a film forming agent, a peroxide and a volatile solvent A gel composition, the film-forming agent comprising one or more selected from polyvinyl acetate (PVAc) and ethyl acetate (EC); and a container for storing the composition.

The tooth whitening product described above may further include an applicator for applying the gel composition and/or instructions for use.

For the tooth whitening product above, the viscosity of the gel in the container is 1000 cps or more as measured at Brookfield DV2T, Spindle No. 62, 25°C, 5rpm and 100cps or less as measured at 100rpm, and after being applied to the teeth The film formed within 1 minute.

A specific example of the present invention can provide a tooth whitening method. The tooth whitening method described above may include the following steps.

(S1) The step of treating the teeth with a tooth whitening gel composition comprising a film-forming agent, a peroxide, and a volatile solvent, the film-forming agent comprising polyvinyl acetate (PVAc) and ethyl acetate (EC ) of more than one.

(S2) A step of coating the tooth surface by forming a non-erosive film on the tooth surface within 10 seconds to 10 minutes after treating the above composition.

(S3) The step of maintaining the non-erosive film on the tooth surface for a time sufficient to whiten the tooth surface.

The composition of the above (S1) step may contain a peroxide in an amount of more than 2.5% by weight and not more than 15% by weight relative to the total weight of the composition.

The sufficient and sufficient time for whitening the tooth surface in the step of (S3) above may mean that more than 90% of the total peroxide content contained in the composition is released, and the coating film is kept for about 5 minutes after the coating film is formed to about 10 hours.

It will be described in detail below.

The above-mentioned composition may contain at least one or more film-forming agents, and the above-mentioned film-forming agents may be provided in admixture with peroxides and volatile solvents.

In one embodiment, the composition described above is intended to be provided in a dosage form capable of being applied to the teeth in the form of a gel. The term "gel" as used herein refers to a form that includes a liquid medium and has fluidity, and in this specification, it is understood that it can be irreversibly formed by volatilization of the solvent in the gel-forming composition those of the film. Preferably, the above-mentioned gel can be partially or completely attached to the tooth surface at least immediately after being applied to the tooth without running off. In one embodiment, the composition, preferably the gel composition, comprising the above-mentioned film forming agent can form a non-erosive film in the oral environment, preferably within 10 seconds to 10 minutes, such as at least 10 minutes after application. A non-erosive film is formed within minutes, within 5 minutes, within 2 minutes, within 1 minute, preferably within 40 seconds, more preferably within 35 seconds. The above-mentioned "non-erosion" means that the formed film will not be decomposed, and will not be dissolved or swelled by moisture such as water or saliva. The above-mentioned non-erosion can be understood as also including the meaning of "water insolubility". The composition herein prepared according to one embodiment does not substantially contain aggressive polymers, such as more than one selected from the group consisting of polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA) and carbomer (Carbomer). The erosive polymer allows to maintain a non-erosive membrane. Here, substantially not containing means containing 1% by weight or less relative to the total weight of the composition, for example, 0.9, 0.8, 0.7, 0.6, 0.5, 0.4, 0.3, 0.2, 0.1% by weight or less, or 0.09, 0.08 , 0.07, 0.06, 0.05, 0.04, 0.03, 0.02, or 0.01% by weight or less, or 0.005% or less, and it is included to the extent that it does not affect the solubility of the film, and it may also include cases where it is not included at all. The above-mentioned non-erosion film may have a transparent or translucent property, and in particular may form or maintain a transparent or translucent film when the product is used. Preferably, the above-mentioned non-erosion film has the advantage that the transparency before and after coating hardly changes, so that it can block the foreign feeling that may occur when using the product (especially the foreign feeling felt by the eyes in appearance). ).

The ingredients contained in the above composition, the preparation method, etc. will be specifically checked.

[film former]

An embodiment of the present invention may include at least one or more film-forming agents in the composition applied to the tooth surface. The above-mentioned film-forming agent may include alcohol-soluble and/or water-insoluble polymers within the range not impairing the object or effect of the present invention. The aforementioned alcohol-soluble polymers refer to polymers suitable for use with solvents such as ethanol. Preferably, the above-mentioned film-forming agent may include one or more selected from polyvinyl acetate (PVAc) and ethyl acetate (EC).

The inventors of the present invention recognized the problem that the lasting power of the tooth whitening effect decreases when a water-soluble film-forming agent is used, and attempted to complete the present invention by selecting a water-insoluble film-forming agent. In the non-water-soluble film-forming agent, especially when any one or more selected from polyvinyl acetate (PVAc) and ethyl acetate (EC) is included, it has been confirmed that even if excess hydrogen peroxide (for example, relative to (more than 2.5% by weight of the total weight of the composition), compatibility with peroxides is also excellent, and a dosage form that meets the purpose of the present invention can be provided without the problem of polymer precipitation or precipitation. Not only that, even the polymers classified as non-water-soluble polymers in the industry can significantly reduce their stability when excessive peroxides are used, so for the purpose of the present invention, considering peroxides, solvents (Water or volatile solvent), other ingredients for improving adhesion, and compatibility with them, when the above-mentioned film-forming agents disclosed herein are included, excellent results can be obtained.

The above-mentioned film forming agent can form a transparent coating film when dried after coating, and thus is excellent in workability, and can also be excellent in dosage form stability even if the hydrogen peroxide content is increased. Relative to the total weight of the composition, the content of the above-mentioned film-forming agent may be 5 to 30% by weight, preferably 10 to 25% by weight, more preferably 15 to 20% by weight. When the above-mentioned film-forming agent has the above-mentioned content range, it is possible to provide a composition having an appropriate viscosity when formulated with other ingredients such as peroxides without affecting the stability of the dosage form.

The composition according to the present invention may contain a volatile solvent, and the above-mentioned film-forming agent may be included in the composition of the present invention by utilizing a volatile solvent. Here, the use can be understood as including the concept of having solubility in the above-mentioned volatile solvent. . The above-mentioned volatile solvent may include, for example, one or more selected from alcohols such as ethanol or diols such as ethanol, benzyl alcohol, isopropanol, propylene glycol and acetone. Preferably, ethanol may be included in terms of the characteristics of application in the oral cavity.

[Teeth Whitening Ingredients]

As the above-mentioned tooth whitening component, peroxide may be included, and the above-mentioned peroxide is a liquid phase peroxide aqueous solution, which can be prepared in the form of aqueous solution when preparing the gel. The above-mentioned peroxides can be used without limitation within the scope of not impairing the object of the present invention, but preferably can include hydrogen peroxide, urea peroxide, potassium peroxide, Tetrasodium pyrophosphate peroxidate or mixtures thereof, but preferably both are provided and formulated as aqueous solutions. The above peroxide may exist as an aqueous peroxide solution or in a state dissolved in a volatile solvent.

With respect to the total weight of the composition, the above-mentioned peroxide may be included in a content of 2 to 15% by weight, preferably, the content may be 2% by weight or more, 2.5% by weight or more, 2.9% by weight or more, 3% by weight or more, 3% by weight or more % or more, 4% by weight or more, 5% by weight or more, 6% by weight or more, 7% by weight or more, 8% by weight or more, 9% by weight or more, 10% by weight or more, preferably, the content can be 15% by weight or less, 14% by weight % by weight or less, 13% by weight or less, 12% by weight or less, 11% by weight or less. In particular, the composition according to the present embodiment can contain peroxide exceeding 2.5% by weight and 15% by weight or less, and can maintain the dosage form stably even if excess peroxide exceeding 3% by weight is contained. The peroxide input during the preparation of the composition may be preferably 25 to 50% by weight aqueous hydrogen peroxide solution, more preferably 30 to 40% by weight aqueous hydrogen peroxide solution, and when the above-mentioned hydrogen peroxide solution is added When prepared, it is possible to prepare a composition that is excellent in stability with the formulated ingredients while containing a high content of peroxide.

The composition of one embodiment herein may further optionally contain a stabilizer having excellent compatibility with peroxides within a range that does not impair the object or effect of the present invention. As examples of the aforementioned stabilizer, tetrasodium pyrophosphate, sodium acid pyrophosphate, sodium hexametaphosphate, sodium tripolyphosphate, etc. may be included as polyphosphates. (sodium tripolyphosphate), sodium potassium tripolyphosphate, tetrapotassium pyrophosphate, acidic sodium meta-polyphosphate, acidic sodium polyphosphate or their mixtures, but not limited to this. The above composition may also contain a tooth whitening aid capable of enhancing the whitening effect of the peroxide. The above-mentioned tooth whitening auxiliary agent may include a dissolving agent for coloring material and/or a chelating agent, and may include without limitation those known in the industry to remove coloring materials attached to the tooth surface, for example may include citric acid, etc., and the above-mentioned chelating agent Ethylenediaminetetraacetate may be included, for example.

[Hydroxypropylmethylcellulose (HPMC) or its esters]

The gel composition for tooth whitening according to one embodiment may further contain hydroxypropylmethylcellulose in consideration of the purpose of stability of the dosage form, improvement of adhesion to teeth, or stable formulation when containing a high content of hydrogen peroxide, etc. Hydrogen (HPMC) or its ester compounds. The above-mentioned HPMC or its ester compound may include, for example, hydroxypropylmethylcellulose (HPMC), hydroxypropylmethylcellulose phthalate (HPMCP), hydroxypropylmethylcellulose acetate succinate (HPMCAS ) or mixtures thereof, preferably, considering compatibility with other polymers that can be stably formulated with high levels of hydrogen peroxide, and used with other polymers, may include hydroxypropyl methylcellulose phthalate ( HPMCP). The aforementioned HPMCP or an ester compound thereof may have, for example, a weight average molecular weight of 1,000 to 10,000,000, 1,500 to 90,000,000, 2,000 to 85,000,000 Mw, and for example, may include HPMCPs having a weight average molecular weight of 1,000 to 10,000,000 Mw.

The aforementioned HPMCP or its ester compound can also compensate for the possible loosening of the film-forming agent when it is applied to the tooth surface.

The above-mentioned HPMC or its ester compound may be included in the composition with a film-forming agent: HPMC or its ester compound in a weight ratio of 1:0.1 to 1.5, preferably 1:0.3 to 1, and when having the above-mentioned When the content ratio is high, the film-forming agent will not be separated out and the stability of the dosage form can be maintained. In addition, when it has the above-mentioned content ratio, it has an appropriate viscosity, can be well and evenly spread on the tooth surface, and provides excellent tooth adhesion. HPMC or an ester compound thereof may be formulated with hydrogen peroxide in the present composition to be provided as a single composition. Alternatively, HPMC or an ester compound thereof may be present in the above composition in admixture with a film-forming agent. Here, the single composition means that, when applied to teeth, a coating of a single layer can be formed at the coated site. According to an embodiment of the present invention, preferably HPMC or its ester compound and the film forming agent form a single composition.

[combination]

The compositions disclosed herein may have adhesion or viscosity to the extent that they are applied to the tooth surface and do not run off during the drying time (e.g., the viscosity measured on a Brookfield DV2T, Spindle No. 62, 25°C, 5 rpm is 1000 cps or more, while the viscosity measured at 100 rpm is 100 cps or less), any component that provides it can also be included within the scope of not impairing the purpose of the present invention. However, it is preferred to exclude components that may form or precipitate precipitates due to poor compatibility with volatile solvents, film-forming agents and/or peroxides contained in the composition or to prepare them with a content below the precipitated content. . For example, it is not necessary to contain polymers that precipitate out after sufficient stirring in the following solution. For example, compounds such as acrylate/octyl acrylamide copolymer (trade name DERMACRYL 79) can be excluded or prepared below the level of precipitation. The solution Based on room temperature of 22-25°C and 5ml, relative to the total weight of the composition, hydrogen peroxide of 9 to 11% by weight and water of 15 to 20% by weight are included. Here, the precipitation refers to a state in which the presence of a precipitate can be recognized or the precipitate is floating in a solution when confirmed with the naked eye.

In a specific example, the fragrance contained in the above composition can be used without limitation in an appropriate amount within the scope of not impairing the object of the present invention, commonly used fragrances in the industry, such as fruity fragrances, mint fragrances and the like. In addition, additives such as surfactants may optionally be included in the composition.

In addition, in another specific example, the above-mentioned composition can use components commonly used in oral compositions such as surfactants, antibacterial compositions, vitamins, and pigments without limitation within the scope of not impairing the purpose of the present invention.

The water contained in the composition can be used in consideration of the compatibility of the components used and the stability of the dosage form, etc., for example, 3% by weight to 25% by weight, more preferably 5% by weight to 20% by weight, can be included in the composition. weight%. The water contained in the composition according to the invention may be formulated from an aqueous solution of hydrogen peroxide. According to one embodiment of the present invention, even if there is more than 5%, more than 11%, or more than 18% of water relative to the total weight of the composition in the composition, the film-forming agent used will not be precipitated and can keep the coagulation. Gel type, and even after attaching to the teeth, it will not be eroded in the presence of external moisture such as saliva. Therefore, the composition according to the present invention can provide a composition capable of forming an excellent non-wetting film in which hydrogen peroxide is not diluted by moisture such as saliva and effectively obtains a tooth whitening effect.

[Teeth Whitening Products]

One embodiment of the present invention may provide a gel-type tooth whitening product that forms a non-erosive film or a non-erosive coating film on the tooth surface. The compositions disclosed in this specification can be stored in containers and circulated. Together with the above-mentioned container, the tooth whitening product can be provided including an application part that can be exemplified by a brush (brush), a tip (tip), etc. that can apply the composition, and if necessary, the above-mentioned application part can also be separated from the container provided separately. Instructions, instructions, etc. that can explain the method of use can also be provided together with the above-mentioned container or the above-mentioned composition.

The tooth whitening product mentioned above can be provided without special limitation on distribution conditions such as room temperature, low temperature, refrigeration, high temperature, etc. The composition in the above tooth whitening product can maintain the stability of the dosage form even when the external temperature changes. Here, maintaining the stability of the dosage form can be understood as the degree to which no sediment occurs or no suspended matter is found and the properties remain similar to the initial state.

Another embodiment of the present invention may be provided to the tooth surface in the form of a tooth wash or the like without a separate coating process within the scope of not impairing the object of the present invention.

[Teeth whitening method]

A specific example of the present invention can provide a tooth whitening method. Here, the tooth whitening method can be used instead of a method of bleaching teeth, a method of removing stains stained on the surface of teeth, and the like.

In a specific example, the tooth whitening method includes the step of treating the above-mentioned composition on the teeth (S1), forming a non-erosion film on the tooth surface within 10 seconds to 10 minutes after treating the above-mentioned composition to coat the tooth surface Step (S2), and the step (S3) of maintaining the above-mentioned non-erosion film on the tooth surface for a time sufficient to whiten the tooth surface.

Preferably, the tooth whitening composition of the above (S1) step comprises more than one film-forming agent, peroxide and volatile solvent selected from polyvinyl acetate (PVAc) and ethyl acetate (EC), preferably Alternatively, here, the above-mentioned composition may further comprise hydroxypropylmethylcellulose (HPMC) or an ester thereof.

The above-mentioned composition may contain more than 2.5% by weight and less than 15% by weight of peroxide relative to the total weight of the composition to maintain a stable dosage form, and may have an excellent ability to maintain a non-erosive film on the tooth surface.

Regarding the above (S2) step, the above tooth whitening method can form a non-erosive film on the tooth surface within 10 seconds to 10 minutes after the composition is applied or treated on the tooth surface, preferably within at least 10 minutes, 5 minutes A non-erosive film is formed within 2 minutes, 1 minute, preferably 40 seconds, more preferably 35 seconds.

The time for sufficient whitening of the tooth surface in the above (S3) step can be understood as referring to more than 99%, more than 95%, more than 93%, or more than 90% of the total peroxide content contained in the composition under oral environment conditions. More than % can be released from non-erosive membranes. In addition, preferably, it can be understood as referring to maintaining a non-erosive film on the tooth surface for about 5 minutes to about 10 hours, 10 minutes to 9 hours, 15 minutes to 8 hours, 20 minutes to 7 hours, 25 minutes to 6 hours.

Regarding the preparation methods of the compositions disclosed herein, if each ingredient can be stably formulated, it should not be construed as being limited to the preparation methods of the examples herein. The preparation method of the examples is just one example for illustrating the preparation process of the composition.

[Invention effect]

The gel composition of the present invention has excellent staying power. Also, since it can contain high levels of peroxide, it can be offered as an effective tooth whitening product. The gel composition of the present invention can be dried quickly and has excellent compatibility among formulated ingredients. The non-erodible film made of the gel composition of the present invention will not be dissolved by saliva, so it has excellent whitening effect lasting power, and can improve the disadvantage of dosage form dissolution leading to product ingestion into the esophagus.

The composition of the present invention is hygienic as it is used without having to put hands directly in the mouth and apply the product.

Hereinafter, in order to facilitate the understanding of the present invention, examples and the like will be given and described in detail. However, the embodiments according to the present invention can be modified into various forms, and the scope of the present invention should not be construed as being limited to the following embodiments. The embodiments of the present invention are provided to more completely explain the present invention to those skilled in the art to which the present invention pertains. % in this specification can be understood as referring to % by weight, unless otherwise stated.

[Experimental Example 1] Confirmation of Properties of Composition Containing 3% Hydrogen Peroxide

Mixtures were prepared with the composition of Table 1 below, and the initial properties varying according to the polymer used as the film former were confirmed. Put the polymer in the solvent (ethanol), stir for more than 1hr (hour) and dissolve (stirring conditions: 1000rpm/1hr, room temperature (22~25℃)), then slowly add hydrogen peroxide aqueous solution and incense to it to prepare the dosage form . The content of water contained in each composition was 5.525% by weight (the ratio of water in the aqueous hydrogen peroxide solution=0.65×8.5% of the prepared amount of hydrogen peroxide). [Table 1] Composition/prescription (unit: weight %) PVAc EC DERMACRYL ^® 79 (DER) polyvinyl acetate 15.0 Ethyl cellulose 15.0 Acrylates/octylacrylamide copolymer (DERMACRYL ^® 79) 15.0 Hydrogen peroxide (35% aqueous solution) 8.5 8.5 8.5 fragrant 0.5 0.5 0.5 ethanol 76.0 76.0 76.0 total 100 100 100

Each composition of Table 1 above was put into a 5 ml vial, and the properties immediately after preparation were confirmed. The temperature is kept at 22~25°C, and the humidity is kept at 45~50%. As a result, as shown in the photograph of Figure 1, when 3% by weight of peroxide was included in the composition as shown above, it was observed that the composition containing PVAc was a clear solution, and the composition containing EC was a slightly cloudy transparent solution. Solution, the composition comprising DER is a clear solution.

[Experimental Example 2] Confirmation of solution phases with different hydrogen peroxide contents

1. Confirmation of properties when using vinyl acetate resin and increasing the content of hydrogen peroxide

The change in appearance and the stability of the dosage form due to the increase in the content of hydrogen peroxide were confirmed when the vinyl acetate resin was used in the composition of Table 2 below. Put the polymer into the solvent (ethanol), stir for more than 1hr and dissolve (stirring conditions: 1000rpm/1hr, room temperature (22~25°C)), then slowly add hydrogen peroxide to it according to the content, additionally add fragrance to Preparation of dosage forms. [Table 2] Composition 1 Composition 2 Composition 3 Composition/Prescription PVAc (peroxide 3%) PVAc (peroxide 6%) PVAc (peroxide 10%) polyvinyl acetate 15.0 15.0 15.0 Hydrogen peroxide (35% aqueous solution) 8.5 17.2 28.6 fragrant 0.5 0.5 0.5 ethanol 76.0 67.3 55.9 total 100 100 100 water content 5.525 11.18 18.59

Each composition of Table 2 above was placed into a 5ml vial and the properties immediately after preparation were confirmed. The temperature is kept at 22~25°C, and the humidity is kept at 45~50%. As a result, as shown in the photograph of FIG. 2 , it was confirmed that a transparent solution state was maintained even when the water content was high. That is, it can be seen that even if a large amount of hydrogen peroxide is contained, there is no problem with the stability.

2. Confirm the properties when ethyl cellulose is used and the content of hydrogen peroxide is increased

When ethylcellulose was used in the composition of Table 3 below, the change in appearance and the stability of the dosage form due to the increase in the content of hydrogen peroxide were confirmed. Put the polymer into the solvent (ethanol), stir for more than 1hr and dissolve (stirring conditions: 1000rpm/1hr, room temperature (22~25°C)), then slowly add hydrogen peroxide to it according to the content, additionally add fragrance to Preparation of dosage forms. [table 3] Composition 4 Composition 5 Composition 6 Composition/Prescription EC (peroxide 3%) EC (peroxide 6%) EC (peroxide 10%) Ethyl cellulose 15.0 15.0 15.0 Hydrogen peroxide (35% aqueous solution) 8.5 17.2 28.6 fragrant 0.5 0.5 0.5 ethanol 76.0 67.3 55.9 total 100 100 100 water content 5.525 11.18 18.59

Each composition of Table 3 above was placed into a 5ml vial and the properties immediately after preparation were confirmed. The temperature is kept at 22~25°C, and the humidity is kept at 45~50%. As a result, as shown in the photograph of FIG. 3 , it was confirmed that no deposits occurred even when the water content was increased. That is, it can be seen that even if a large amount of hydrogen peroxide is contained, there is no problem with the stability.

3. Confirmation of properties when using acrylate/octylacrylamide copolymer (DERMACRYL 79, DER) and increasing the content of hydrogen peroxide

When the acrylate/octyl acrylamide copolymer was used in the composition of Table 4 below, the change in appearance and the stability of the dosage form due to the increase in the content of hydrogen peroxide were confirmed. Put the polymer into the solvent (ethanol), stir for more than 1hr and dissolve (stirring conditions: 1000rpm/1hr, room temperature (22~25°C)), then slowly add hydrogen peroxide to it according to the content, additionally add fragrance to Preparation of dosage forms. [Table 4] Composition 7 Composition 8 Composition 9 Composition/Prescription DER (peroxide 3%) DER (peroxide 6%) DER (peroxide 10%) Acrylates/octyl acrylamide copolymer 15.0 15.0 15.0 Hydrogen peroxide (35% aqueous solution) 8.5 17.2 28.6 fragrant 0.5 0.5 0.5 ethanol 76.0 67.3 55.9 total 100 100 100 water content 5.525 11.18 18.59

Each composition of Table 4 above was placed into a 5ml vial and the properties were confirmed immediately after preparation. The temperature is kept at 22~25°C, and the humidity is kept at 45~50%. The results can be confirmed from Figure 4, where it can be seen that as the water content increases, it becomes suspended and precipitates at a low temperature environment (0°C (refrigerated) or below -15°C (frozen)) at DER 6% As a result, the polymer entangled without dissolving and was precipitated out at DER 10%.

4. Confirmation of the results of the temperature-dependent properties of the compositions prepared according to the categories 1 to 3 above

It was confirmed whether the storage temperature of the above-mentioned tooth-whitening gel composition changes properties. [table 5] 50℃ high temperature 0°C (refrigerated) Below -15°C (frozen) PVAc ○ ○ ○ PVAc 6% ○ ○ ○ PVAc 10% ○ ○ ○ EC ○ ○ ○ EC 6% ○ ○ ○ EC 10% ○ ○ ○ DER ○ ○ ○ DER 6% ○ △ x DER 10% x x x ○: Good (no change in properties from initial state) △: Fair (property becomes suspension, but no sediment) X: Insufficient (sediment occurs, no longer dissolves)

Therefore, when PVAc and EC are included, it can be seen that a stable dosage form can be formed even if the content of hydrogen peroxide in the dosage form is increased. That is, when PVAc and EC are contained, it can be confirmed that the dosage form stability can be maintained not only immediately after preparation but also under temperature changes that may occur during distribution.

[Experimental example 3] compare the solution phase when different polymers comprise HPMC or HPMCP

Changes in appearance and stability of dosage forms were confirmed when HPMC or HPMCP was further included in each polymer used as a film former. Put the ethanol-soluble polymer (PVAc, EC, DER) into the solvent (ethanol), stir for more than 1hr and dissolve (stirring condition: 1000rpm/1hr, room temperature (22~25℃)), and then slowly add it according to the content Hydrogen peroxide, additionally fragranced to prepare dosage forms. Slowly add HPMC or HPMCP according to the content, stir and dissolve at 1000rpm/1hr. [Table 6] Composition 1 Composition 1-1 Composition 1-2 Composition 4 Composition 4-1 Composition 4-2 Composition 7 Composition 7-1 Composition 7-2 Composition/Prescription PVAc PVAc+HPMC PVAc +HPMCP EC EC+HPMC EC+HPMCP DER DER+HPMC DER+HPMCP polyvinyl acetate 15.0 10.0 10.0 Ethyl cellulose 15.0 10.0 10.0 Acrylates/Octyl Acrylamide Copolymer (DERMACRYL® 79) 15.0 10.0 10.0 HPMC 5.0 5.0 5.0 HPMCP 5.0 5.0 5.0 Hydrogen peroxide (35%) 8.5 8.5 8.5 8.5 8.5 8.5 8.5 8.5 8.5 fragrant 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 ethanol 76.0 76.0 76.0 76.0 76.0 76.0 76.0 76.0 76.0 total 100 100 100 100 100 100 100 100 100 *HPMC: AnyAddy AN6 (Manufacturer: lottefinechemical), 10,000 ~ 1,000,000 (Mw) *HPMCP: AnyCoat-P HP-55 (Manufacturer: lottefinechemical), 10,000 ~ 1,000,000 (Mw) *Polyvinyl acetate: VINNAPAS B 100 Special (Manufacturer: Wacker Chemie AG), 1,000,000 Mw *Ethylcellulose: Aqualon EC N7 PHARM (Manufacturer: ashland), 65,000 Mw

Each composition of Table 4 above was placed into a 5ml vial and the properties were confirmed immediately after preparation. The temperature is kept at 22~25°C, and the humidity is kept at 45~50%.

As a result, it can be confirmed from FIG. 5 that when HPMC was added, it was not dissolved and precipitated, and sank or adhered to the vial. When HPMCP was added, it was dissolved in ethanol and no precipitation or precipitation was observed.

Therefore, it can be seen that HPMCP is preferred to obtain a tooth whitening gel that does not generate deposits on the tooth surface and spreads well and evenly.

[Experimental Example 4] Confirmation of other physical properties such as film strength/adhesion

The strength and adhesion of the oral membrane (membrane) prepared by applying the gel prepared by the formulation in Table 6 above to the tooth surface were confirmed. The durability of the film was evaluated by coating each formulation on a nail tip and drying it, then soaking in distilled water for 12 hr, and then confirming the change of the film. Adhesion of the film was evaluated by whether or not the film remained when the nail sheet for evaluating the durability of the above-mentioned film was dried and then scratched with other nail sheets. The substrate used was H2NAIL/PEDI TIP size 1.

1. Experimental method

Specifically, experiments were performed in the following order. (1) Use a brush to paint three times on the substrate (nail sheet) to be used in the experiment. (2) Fully dry for 1 minute under the condition of maintaining temperature/humidity (temperature: 22~25℃, humidity: 45~50%). (3) Confirm the dry state with the naked eye. (4) Soak the nail piece coated with the dosage form in distilled water at 35°C for 12 hours. (5) Fully dry the sample soaked for 12hr for more than 24hr under the condition of maintaining temperature/humidity (temperature: 22~25℃, humidity: 45~50%). (6) Film durability was evaluated by confirming whether or not there was a change in the film. (7) Using the unused nail piece in the experiment, scrape the coated surface with 50 gf using a texture analyzer. (8) Confirm the damage degree of the coated surface to evaluate the film adhesion. The same experiment was repeated 3 times to investigate the phenomenon.

2. Experimental results

For PVAc, EC formulations, it is clear when applied, while for DER formulations, it appears white when applied. Since the produced film was white and very conspicuous, it was judged that the usability decreased when DER was included, and the durability and adhesion of the film were confirmed using a combination made of a transparent film. In the evaluation of film durability against distilled water immersion, it was confirmed that all had film durability, but it was found that the adhesion was improved in the formulation containing HPMCP. The results are shown in Table 7 and Figure 6 below. [Table 7] prescription PVAc (P) PVAc +HPMCP (PH) EC (E) EC +HPMCP (EH) film form transparent transparent transparent transparent membrane durability no change no change no change no change Adhesion slightly scratched no change slightly scratched no change

[Experimental example 5] Confirmation of drying time of different polymers

As a result of the drying time test on the previously selected formulations, it was confirmed that all can dry within 30 seconds and form an immediate film in the oral cavity.

1. Experimental method (1) Preparation of dosage forms prepared with each formulation. The brackets of the formulations in Table 8 below indicate the content of peroxide, and make the total weight of ① film former or ② film former and HPMC or their combination in the composition be 15% by weight. (2) Transfer the dosage form into a 3 ml brush container, and then use the brush to apply 4 cm to the right on the slide glass at one time (use 1~2 drops: 0.03~0.05g ). (3) Taking the 3 cm portion except the 0.5 cm portion on both sides as the measurement range, use a texture analyzer to generate an indentation every 5 seconds with a force of 113 g, and measure the time until the indentation does not appear. A photograph of the measurement method is shown in Figure 7. (4) Measured in a space that maintains temperature/humidity (temperature: 22~25°C, humidity: 45~50%). [Table 8] prescription PVAc (3%) PVAc +HPMCP (3%) EC (3%) EC+HPMCP (3%) drying time about 20 seconds about 20 seconds about 25 seconds about 25 seconds prescription PVAc (6%) PVAc +HPMCP (6%) EC (6%) EC+HPMCP (6%) drying time about 20 seconds about 20 seconds about 30 seconds about 30 seconds prescription PVAc (10%) PVAc +HPMCP (10%) EC (10%) EC+HPMCP (10%) drying time about 25 seconds about 25 seconds about 30 seconds about 30 seconds

As shown in Table 8 above, all were quickly dried in about 30 seconds even with increased water content. While HPMCP increases the adhesion, it does not affect the drying time, so it can be formulated with the above-mentioned film-forming agents to obtain excellent results.

Here, "about" can be understood as including an error range up to +/-1 second.

[Experimental example 6] Confirmation of whitening effect

The results of comparing the whitening effects of different prescriptions and different hydrogen peroxide contents are shown in Table 9 below.

A certain amount (0.15±0.05g) was applied to the stained HAP (stained-HAP) test piece, and then left for 1hr. Use a color difference meter to measure the initial color and the color change after whitening evaluation, and record the color change value (ΔE) after coating.

ΔE is the value obtained according to the formula ΔE = [(ΔL*)2 + (Δa*)2 + (Δb*)2]1/2 commonly used in the industry, L* represents the brightness value in the range of 0 to 100, the closer to 0 means darker, closer to 100 means brighter. a* and b* indicate saturation, a* indicates a value of red-green chromaticity, and b* indicates a value of yellow-blue chromaticity. [Table 9] prescription Composition 1 Composition 1-2 Composition 4 Composition 4-2 Composition 7 Composition 7-2 PVAc (3%) PVAc +HPMCP (3%) EC (3%) EC+HPMCP (3%) DER (3%) DER +HPMCP (3%) Color change (ΔE) 3.59±0.24 3.65±0.09 3.45±0.58 3.55±1.88 3.76±1.18 3.34±0.07 prescription Composition 2 Composition 2-2 Composition 5 Composition 5-2 - - PVAc (6%) PVAc +HPMCP (6%) EC (6%) EC+HPMCP (6%) Color change (ΔE) 7.20±1.13 6.98±0.84 6.99±1.42 6.85±0.13 prescription Composition 3 Composition 3-2 Composition 6 Composition 6-2 - - PVAc (10%) PVAc +HPMCP (10%) EC (10%) EC+HPMCP (10%) Color change (ΔE) 9.36±1.68 9.57±1.47 9.25±1.98 8.91±1.46

The compositions of the above compositions 2-2, 3-2, 5-2 and 6-2 were as follows. [Table 10] Composition 2-2 Composition 3-2 Composition 5-2 Composition 6-2 Composition/Prescription PVAc +HPMCP (6%) PVAc +HPMCP (10%) EC+HPMCP (6%) EC+HPMCP (10%) polyvinyl acetate 10.0 10.0 Ethyl cellulose 10.0 10.0 HPMCP 5.0 5.0 5.0 5.0 Hydrogen peroxide (35%) 17.2 28.6 17.2 28.6 fragrant 0.5 0.5 0.5 0.5 ethanol 67.3 55.9 67.3 55.9 total 100 100 100 100

As can be confirmed from the above table, it can be seen that the polymers formulated together have no negative influence on the efficacy of the tooth whitening component, and even if the concentration of the polymer is increased, there is no problem in the exertion of the whitening effect.

[Experimental Example 7] Confirmation of the whitening effect by time

HAP test pieces with 47 ~ 49 L* value were screened out, and then immersed in distilled water at 37°C for 30min. After taking out the HAP test piece, wipe off the moisture and lightly moisten the surface with a wet paper towel. Prepare the PVAc (peroxide 3%) formulations in Table 2, the formulations containing DER instead of PVAc, and the formulations containing polyvinylpyrrolidone (PVP) instead of PVAc, and treat them on the HAP test strips in the same amount (1 time, 12 mg ~ 17 mg). The HAP coupons were dried for 1 minute, then immersed in a 37°C water bath for 1 hour and 12 hours. The test pieces treated at different times were stirred in ethanol for 30 min, and then washed once in tap water (wash-off). The test piece was dried in an oven at 50° C., and then the color change from the original test piece was confirmed using a color difference meter. The results are shown in FIG. 9 .

The oblique line on the left represents the whitening evaluation result after 1 hour, and the spot on the right represents the whitening evaluation result after 12 hours. The larger the value, the stronger the whitening effect, and PVAc exhibiting non-erosive physical properties has a more excellent whitening effect than PVP that cannot maintain a film due to water such as saliva in the oral environment. In particular, PVAc maintained the dosage form even if it contained an excess of hydrogen peroxide, but other polymers were unstable due to gelation, etc., and when 6% by weight of peroxide was included in the total composition, PVP was not formed Stable dosage form.

none

The following drawings attached to this specification illustrate the preferred embodiments of the present invention, and play a role in further understanding the technical idea of the present invention with the content of the foregoing invention, so the present invention should not be construed as being limited to these drawings recorded matters.

[ FIG. 1 ] is a photograph confirming properties of each solution immediately after preparation according to Experimental Example 1. [ FIG. [ Fig. 2 ] is a photograph for confirming properties of each solution immediately after preparation when a vinyl acetate resin was used and the content of hydrogen peroxide was increased in Experimental Example 2. [ Fig. 3 ] is a photograph for confirming properties of each solution immediately after preparation when ethyl cellulose was used in Experimental Example 2 and the content of hydrogen peroxide was increased. [ Fig. 4 ] is a photograph for confirming properties of each solution immediately after preparation when an acrylates/octylacrylamide copolymer was used in Experimental Example 2 and the content of hydrogen peroxide was increased. [ Fig. 5 ] is the result of confirming the state of the solution when HPMC or HPMCP is added to the polymer used as a film-forming agent. [ Fig. 6 ] shows the state of change immediately after coating and after scratch evaluation after the composition of each formulation is coated on the test substrate. [ Fig. 7 ] is a photograph showing how to check the drying time of different formulations, showing a state where no indentation is formed while drying. [ Fig. 8 ] is a graph showing the results of evaluating the whitening effect of different formulations and different hydrogen peroxide contents. [ Fig. 9 ] shows the results showing that the whitening effect differs depending on the polymer used, and the other polymer is an acrylate/octylacrylamide copolymer.

Claims (16)

A composition, a tooth whitening gel composition coated on the surface of teeth, the composition comprising: It includes more than one film forming agent, a peroxide and a volatile solvent selected from polyvinyl acetate (PVAc) and ethyl acetate (EC). The composition according to claim 1, wherein, relative to the total weight of the composition, the content of the peroxide exceeds 2.5% by weight and is 15% by weight or less. The composition according to claim 1, wherein, relative to the total weight of the composition, the content of the film-forming agent is 5% by weight to 30% by weight. The composition according to claim 1, wherein the composition further comprises hydroxypropylmethylcellulose (HPMC) or a monoester compound comprising the hydroxypropylmethylcellulose. The composition as claimed in item 4, wherein the ester compound comprises monohydroxypropylmethylcellulose phthalate (HPMCP). The composition according to claim 4, wherein the hydroxypropylmethylcellulose or the ester compound exists in admixture with the peroxide and/or the film former, and the composition is provided as a single composition. The composition according to claim 4, wherein the weight ratio of the film forming agent: the hydroxypropylmethylcellulose or the ester compound is 1:0.1 to 1.5. The composition as claimed in claim 1, wherein the composition contains 3% by weight to 25% by weight of water, and the peroxide exists in the form of an aqueous peroxide solution, or is dissolved in the volatile solvent status exists. The composition as described in any one of claims 1 to 8, wherein the composition does not substantially comprise polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA) and carbomer (Carbomer) More than one aggressive polymer in the group. The composition as described in any one of claim items 1 to 8, wherein the composition does not include polymers precipitated in the following solution: the solution is based on room temperature of 22-25°C and 5ml, relative to Based on the total weight of the composition, 9% to 11% by weight of the peroxide and 15% to 20% by weight of water are included. A tooth whitening product that forms a coating on the surface of teeth, comprising: A gel composition for tooth whitening, comprising a film-forming agent, a peroxide and a volatile solvent, the film-forming agent comprising more than one selected from polyvinyl acetate (PVAc) and ethyl acetate (EC) ;as well as A container for storing the tooth whitening gel composition. The tooth whitening product according to claim 11, further comprising a coating part and/or a usage guide for coating the tooth whitening gel composition. The tooth whitening product as claimed in claim 11, wherein the viscosity of the tooth whitening gel composition in the container is measured at Brookfield DV2T, Spindle No. 62, 25°C, and 5rpm. The viscosity is above 1000cps, and at 100rpm The measured viscosity is below 100 cps and forms a film within 1 minute after being applied to a tooth. A method of teeth whitening comprising: (S1) A step of treating a tooth with a tooth whitening gel composition comprising a film-forming agent, a peroxide and a volatile solvent, the film-forming agent comprising polyvinyl acetate (PVAc) and One or more of ethyl acetate (EC); (S2) After treating the above gel composition for tooth whitening, within 10 seconds to 10 minutes, a step of forming a non-erosive film on the tooth surface to coat the tooth surface; and (S3) The step of maintaining the non-erosive film on the tooth surface for a time sufficient to whiten the tooth surface. The tooth whitening method according to claim 14, wherein the tooth whitening gel composition in the (S1) step contains more than 2.5% by weight and 15% by weight relative to the total weight of the tooth whitening gel composition following the peroxide. The tooth whitening method according to claim 14, wherein, in the (S3) step, the sufficient time for whitening the tooth surface is 90% of the total peroxide content contained in the tooth whitening gel composition More than % is released and maintained for a period of about 5 minutes to about 10 hours after forming a coating film.

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