KR102569590B1 - Film type dentifrice - Google Patents

Abstract

The present invention provides a film-type toothpaste comprising i) polyethylene oxide or a polymer thereof, ii) a polymer mixture including a hydrophobic cellulose-based polymer and iii) a hydrophilic cellulose-based polymer, iv) an abrasive, and v) a medicinal agent. The film-type toothpaste of the present invention can be made into a single layer, has excellent compatibility between the abrasive and the medicinal agent, and can provide sufficient contact time between the teeth and the toothpaste.

Description

Film type toothpaste {Film type dentifrice}

The present invention relates to a film-type toothpaste, and more specifically, to a film-type toothpaste capable of effectively delivering medicinal substances into the oral cavity while increasing tooth cleaning power by securing sufficient time to contact the teeth by attaching the toothpaste to the teeth and then using the toothpaste. it's about

There are various formulations of toothpaste, such as powders, liquids, tablets, pastes, etc., but most of the toothpastes actually sold are pastes for reasons such as convenience of use or economy. However, when brushing the teeth with a toothbrush, the paste is not effectively delivered to the desired area by spreading the medicinal substance for dental and oral health or beauty throughout the mouth. For example, in the case of fluoride used in most toothpastes, the effect of preventing tooth decay or remineralization can be expected only when it acts on the teeth. The amount is limited and the effect is not as great as expected. In addition, the toothpaste has a problem that the effect of the active ingredient is insufficient due to the lack of contact time of the active ingredient as the use time is 1 to 3 minutes.

For the above reasons, a technology for making a toothpaste formulation into a film type has been developed, but there is a problem in that the film has to be manufactured in a layered structure of several layers due to poor compatibility between the active pharmaceutical ingredient and the abrasive.

Specifically, when hydrogen peroxide is included to the extent that it can show a whitening effect, the compatibility of peroxide with hydrous silicic acid (silica), DCPD, calcium carbonate, etc., which are the most commonly used abrasives in toothpaste, is not good. There was a problem that the whitening effect was lowered due to decomposition. Therefore, in order not to contact each other, they had to be separately put into a water-soluble layer, and a basic layer (a layer composed of a water-insoluble or partially water-soluble polymer) was in the middle, so it was inevitably composed of three layers.

That is, since the compatibility of highly reactive peroxide with general toothpaste abrasives such as hydrous silicic acid (silica), DCPD, and calcium carbonate was poor, there was a problem that the stability of the peroxide during storage was poor over time, so that it could not be added to the layer.

On the other hand, since the manufacturing cost increases when it is composed of such a multi-layer, there has been a great burden in actual commercialization. In addition, it is not easy to manufacture a thickness of 100 um or more at a time when manufacturing by the solvent casing method, which is a general method for manufacturing patches, so that the thickness becomes thick, resulting in not only manufacturing costs, but also a poor feeling of use and poor adhesion to teeth. there was. In the case of making it thin to solve this thickness problem, the absolute amount is smaller than the amount required for one-time use, which may cause a problem that the abrasive power and cleaning power are somewhat insufficient compared to paste toothpaste.

In order to solve the above problems, the present invention is to provide a toothpaste in the form of a film that can effectively deliver active ingredients into the oral cavity while maintaining cleaning power and freshness like paste-type toothpaste.

The present invention is to provide a film-type toothpaste with excellent form stability even in a humid oral cavity and excellent compatibility of active ingredients.

The toothpaste of the present invention is intended to provide adequate adhesive strength, and at the same time exhibit abrasive power and be removed by brushing after a certain period of time.

The present invention is to provide a toothpaste in the form of a film that is attached to the tooth or the tooth periphery.

The present invention has been completed as a result of repeated research to solve the problem of recognizing the problem that the film-type toothpaste has somewhat insufficient abrasive power and cleaning power compared to paste toothpaste. The present invention is to solve the problem that the film-type toothpaste cannot have sufficient thickness and weight, and to provide a method capable of providing the same level as conventional toothpaste in terms of cleaning power and freshness.

An object of the present invention is to provide a toothpaste that can have a sufficient contact time between an active ingredient and a target site and give a sensible effect in a short period of time. The film-type toothpaste of the present invention exhibits abrasive power and can be removed by brushing after a certain period of time and appropriate adhesive strength.

The formulation of the present invention is suitable for cold teeth, gingivitis, fluoride reinforcement, tooth remineralization, etc., which require oral preventive and alleviating effects, since sufficient contact time is required with the teeth and gums, which are the target areas. In particular, the inventors of the present invention are The present invention was completed in order to solve the problem of affecting the aging stability of the peroxide when a peroxide capable of providing a whitening effect is included together with an abrasive.

The present invention is to provide a film-type toothpaste comprising i) polyethylene oxide or a polymer thereof, ii) a hydrophobic cellulose-based polymer, and iii) a polymer mixture including a hydrophilic cellulose-based polymer, iv) an abrasive, and v) a medicinal agent.

Specifically, the present invention is a film in which components of a toothpaste composition are distributed in a polymer matrix formed by a polymer mixture including i) polyethylene oxide or a polymer thereof, ii) a hydrophobic cellulose polymer, and iii) a hydrophilic cellulose polymer. I would like to provide toothpaste.

As used herein, 'film type' may mean a form such as a thin film. It may have a standardized form, but is not limited thereto.

The film-type toothpaste of the present invention can be understood to mean a toothpaste that can clean the oral cavity by brushing while the film dissolves after a certain time elapses after the toothpaste in the form of a thin film is attached to the tooth or around the tooth. .

The predetermined time can be designed in various ways to suit the purpose , but preferably can be understood as a close contact time of about 10 minutes as short as 30 minutes-3 hours (h) as long as possible.

In the film-type toothpaste of the present invention, all or part of the active drug contained in the matrix forming the toothpaste may be released to the tooth or the tooth periphery during the period of time when the toothpaste is adhered.

The tooth periphery may preferably be understood as gum tissue close to the tooth.

In one embodiment of the present invention, the polymer mixture included in the film-type toothpaste has a content ratio of i) polyethylene oxide or a polymer thereof and ii) a hydrophobic cellulose-based polymer and iii) a hydrophilic cellulose-based polymer of 1:0.05 to 1:1 ( Weight of polyethylene oxide or its polymer: weight of hydrophobic cellulose-based polymer and hydrophilic cellulose-based polymer). Preferably, it may be 1:0.1 to 1:0.9, more preferably 1:0.15 to 1:0.8.

The inventors of the present invention have confirmed that when polyethylene oxide or its polymer is used, it can have sufficient decomposition power to serve as a toothpaste while maintaining adhesive strength in a moist oral cavity. In particular, the object of the present invention could be achieved by using a mixture of cellulose-based polymers.

When having the above content ratio, it is possible to remove by brushing while giving sufficient adhesive strength to the teeth or gums in the oral cavity. And when it has the above content ratio, it is possible to give the abrasive power, which is the basic function of toothpaste, while maintaining the stability of the active substance in the polymer matrix. In particular, considering the stability of the peroxide and the abrasive, the film-type toothpaste should be prepared by dividing into separate layers, but the inventors of the present invention can confirm that the stability of the peroxide and the abrasive can be achieved by the polymer matrix within the above content range. there was.

In one embodiment of the present invention, polyethylene oxide having a molecular weight of 3,000 to 5,000 kDa may be used as the polyethylene oxide, more preferably polyethylene oxide having a molecular weight of 3,500 to 4,500 kDa may be used. When having the above molecular weight, excellent moldability can be provided and adhesion to the tooth surface can be improved.

In another embodiment of the present invention, two or more types of polyethylene oxide or polymers thereof having different degrees of polymerization may be used. Preferably, the polyethylene oxide is a mixture of polyethylene oxide having a molecular weight of 100 kDa to 1,000 kDa, preferably 150 kDa to 900 kDa, more preferably 200 kDa to 600 kDa, together with polyethylene oxide having a molecular weight of 3,000 to 7,000 kDa. can be used

As described above, when two or more types of polyethylene oxides having different molecular weights are included, better wet tack and formability can be provided, and thickening properties can be provided. In particular, in the present invention, the release rate of the active ingredient in the film can be adjusted by using polyethylene oxide having a molecular weight of 100 kDa to 1,000 kDa together with polyethylene oxide having a molecular weight of 3,000 to 7,000 kDa.

The film-type toothpaste of the present invention is prepared by using a cellulose-based polymer together with the polyethylene oxide. The cellulose-based polymer may be used in combination with a hydrophobic cellulose-based polymer and a hydrophilic cellulose-based polymer.

The inventors of the present invention have confirmed that it is preferable to use the polyethylene oxide or a polymer thereof as a polymer that has no adhesive force in a dry state but can generate sufficient adhesive force using a small amount of moisture on the tooth surface. In addition, as a result of studying a combination of suitable polymers to prepare a film-type toothpaste that can be easily attached to the tooth surface but not excessively sticky and can be removed by brushing, a cellulose-based polymer, more preferably a hydrophilic cellulose-based polymer and a hydrophobic It was confirmed that it is easy to achieve the object of the present invention when a cellulose-based polymer is used together.

In one embodiment of the present invention, the hydrophobic cellulose-based polymer may include all hydrophobic cellulose well-known in the industry, for example, hydroxypropylmethyl cellulose phthalate, ethyl cellulose, ethylmethylcellulose, ethyl hydroxy Oxyethylcellulose or mixtures thereof may be used. Preferably, ethyl cellulose may be used as the hydrophobic cellulose-based polymer considering the compatibility with ethylene oxide and the object of the present invention.

In one embodiment of the present invention, the hydrophilic cellulose-based polymer may include all hydrophilic cellulose known in the industry, for example, hydroxypropyl cellulose, hydroxypropylmethyl cellulose, hydroxyethyl cellulose, methyl cellulose or mixtures thereof may be used. Preferably, considering the compatibility with ethylene oxide of the present invention and the object of the present invention, the hydrophilic cellulose-based polymer may be hydroxypropyl cellulose and/or hydroxypropyl methyl cellulose.

The film-type toothpaste of the present invention may include a weight ratio of a hydrophobic cellulose-based polymer and a hydrophilic cellulose-based polymer of 3: 1 to 1: 3 (hydrophobic cellulose-based polymer: hydrophilic cellulose-based polymer), preferably 2: 1 to It can be included in a ratio of 1:2.

The matrix structure formed by the polymer mixture included in the toothpaste composition of the present invention preferably has the above weight ratio in order to have excellent compatibility with the components included in the toothpaste composition and not to impair the stability of the components.

The dentifrice composition of the present invention may further contain a water-insoluble polymer in order to maintain a constant shape and achieve compatibility with medicinal agents. For example, polyethylene (PE), polypyrophylene (PP), ethylene vinyl acetate (EVA), shellac, poly vinyl acetate, poly methyl methacrylate, methacryloyl ethyl betaine/methacrylate air Copolymer (Yukaformer: manufactured by Mitsubishi, methacryloylethyl betaine/ methacrylate copolymer), methacrylic acid copolymer (Eudragit L 100, Eudragit L 12,5, Eudragit L 100-55, Eudragit L 30D-55), aminoalkyl Methacrylate copolymers (aminoalkyl methacrylate copolymer; Eudragit E 100, Eudragit E 12,5, Eudragit RL 100, Eudragit RL 30D) and the like may be used.

In the present invention, an abrasive is used to remove foreign substances in the oral cavity. Examples of preferred abrasives for the purposes of the present invention include calcium pyrophosphate (CPP), hydrous silicic acid (silica), calcium carbonate, sodium carbonate, baking soda, dicalcium phosphate dehydrate (DCPD), abhydrous dicalcium phosphate (DCPA), colloidal silicon dioxide ( At least one selected from fumed silica) and alumina (aluminum oxide) may be used. Preferably, considering the object of the present invention and compatibility with peroxide, in the case of tooth whitening, calcium pyrophosphate and colloidal silicon dioxide alone or a mixture thereof may be used as the abrasive.

Medicinal agents included in the film-type toothpaste of the present invention may include, for example, components capable of improving oral symptoms including teeth, and include, for example, tooth whitening components and caries preventing components including a fluoride ion source. , tartar formation inhibitory component, anti-inflammatory component, antibacterial component, and other vitamins and minerals. In addition, it may include ingredients to improve ache and alleviate symptoms. The medicinal agent may include all components aimed at improving symptoms that may occur in the oral cavity. More specifically, for example, any one selected from the group consisting of sodium fluoride, stannous fluoride, indium fluoride, amine fluoride, and sodium monofluorophosphate. anti-cavity components such as one or more sources of fluoride ions; remineralization agents including hydroxyapatite; As teeth whitening ingredients, hydrogen peroxide, carbamide peroxide, calcium peroxide, perborate, percarbonate, peroxyacids, persulfates, May contain calcium chlorite, barium chlorite, magnesium chlorite, lithium chlorite, sodium chlorite, or mixtures thereof, and produce tartar It is possible to use condensed phosphate with excellent solubility in water for whitening effect by suppressing and removing extrinsic staining. Condensed phosphates that can be used include TSPP (tetrasodium pyrophosphate), TKPP (tetrapotassium pyrophosphate), SAPP (sodium acid pyrophosphate), and sodium polyphosphate (sodium tripolyphosphate, multiphos). One or two or more of these may be used together. Triclosan, chlorhexidine, alexidine, hexetidine, sanguinarine, benzalkonium chloride, salicylanilide, domiphen bromide ), tetradecylpyridinium chloride (tetradecylpyridinium chloride, TPC), or antimicrobial or antibacterial agents including mixtures thereof; anti-inflammatory agents including aspirin, ketorolac, flurbiprofen, piroxicam, meclofenamic acid, or mixtures thereof; or thiamine, riboflavin, nicotinic acid, pantothenic acid, pyridoxine, biotin, folic acid, vitamin B12, lipoic acid ), ascorbic acid, vitamin A, vitamin D, vitamin E, vitamin K, or mixtures thereof; or mixtures thereof, but is not limited thereto. In addition, drugs effective for preventing and improving periodontal disease include sodium succinate, hinokichiol, bamboo salt, corn unsaponifiable extract, silver leaf extract, cetylpyridinium chloride (CPC), myrrh, ratania, chamomile, polycresol Len, centella clove extract, nutmeg extract, dexpanthenol, β-sitosterol, acetyl salicylic acid, etc. may be included alone or as a mixture in a certain ratio. Ingredients for improving and alleviating symptoms of Shirin include zinc chloride, potassium phosphate, potassium diphosphate, tripotassium phosphate, calcium chloride, oxalic acid, potassium oxalate, ferric oxalate, strontium chloride, potassium nitrate, and vitamin E. etc. may be included singly or in combination of two or more.

The medicinal agent may be uniformly dispersed in the polymer matrix for film formation, and even if the dispersion is non-uniform, it may be included in the mixing of the present invention.

The film-type toothpaste of the present invention may further include a foaming agent, a flavoring agent, a sweetener, and the like.

The foaming agent may be sodium lauryl sulfate, betaine, poloxamer, or the like. Components commonly used in the industry may be used as the flavoring and sweetening agents.

The film-type toothpaste of the present invention may be formed as a single-layer film structure without being divided into a separate hydrophilic polymer layer and a hydrophobic polymer layer.

The film-type toothpaste of the present invention may include a release paper, and the release paper may be used after being removed before being attached to the teeth.

The film-type toothpaste can have any thickness, but in the case of paste toothpaste, about 0.5 g to 1 g is used at a time to obtain a tooth brushing effect, so the thickness of the film is also 400 to 1,200 μm, preferably 450 to 1,150 μm, more preferably A thickness of 480 to 1,120 μm can give a higher feeling of use. It is possible to provide excellent adhesion within the above thickness range, and it is possible to secure sufficient contact time with the target area.

The film-type toothpaste of the present invention may be manufactured by a casting process using a solvent, or may be manufactured by an extrusion method. Preferably, the film toothpaste of the present invention can be molded by an extrusion process because of its thermoplastic properties.

In one embodiment of the present invention, the solvent that can be used in the casting process is water, ethanol alone or a mixture thereof, and other organic solvents such as ethyl acetate, methylene chloride, isopropyl alcohol, acetonitrile alone or a mixture thereof It can be used by adjusting the ratio according to the polymer.

The present invention can provide toothpaste in the form of a film that is attached to teeth or teeth periphery. Preferably, the present invention can provide a film-type toothpaste made of one layer.

The film-type toothpaste of the present invention provides a film-type toothpaste excellent in compatibility with active ingredients such as whitening agents, while having excellent cleaning power and freshness.

The present invention allows the active ingredient and the target area to have sufficient contact time, and can give a sensible effect in a short period of time.

The film-type toothpaste of the present invention exhibits abrasive power and can be removed by brushing after a certain period of time and appropriate adhesive strength.

Hereinafter, the following examples and the like will be described in order to explain the present invention in more detail. However, embodiments according to the present invention can be modified in many different forms, and the scope of the present invention should not be construed as being limited to the embodiments described below. Embodiments of the present invention are provided by way of example to help a detailed understanding of the present invention. Unless otherwise specified, % described herein may be understood to mean % by weight.

[Manufacture of film-type toothpaste]

Film toothpastes of Examples and Comparative Examples having the following composition were prepared.

Examples and Comparative Examples were prepared in the following way.

In Examples 1, 3 and 4, toothpastes were prepared by the solvent casting method. Example 2 prepared toothpaste by the extrusion method. The extrusion method was prepared by referring to Asian Journal of Pharmaceutical Sciences 10 (2015) 292-305.

Comparative Example 1-3 was produced by the solvent casting method. In Comparative Examples 2 and 3, the solution of each layer was thinly spread into a film and dried by applying hot air. The active layer, the intermediate layer, and the base layer were laminated in order, and the prepared film was cut into a desired shape and used. Comparative Example 4 was produced by the extrusion method.

Example 1 Example 2 Example 3 Example 4 1-Layer NaF 0.22% NaF 0.22% 3% hydrogen peroxide 3% hydrogen peroxide ZnCl ₂ 0.09% Sulfur extract 0.05% CPP 10% CPP 10% Hydrous silicic acid 10.0% DCPD 20.0% SLS 1.0% SLS 1.0% SLS 1.0% SLS 1.0% EC 8.8% EC 8.8% EC 12% EC 35% HPMC 4.4% HPMC 4.4% HPMC 8.0% HPMC 20% Polyox (WSR303) 5% Polyox (WSR303) 5% Polyox (WSR301) 2% Polyox (WSR301) 10% Glycerin 4.0% Polyox (WSRN80) 4% Glycerin 4.0% Glycerin 4.0% Castor oil 6.0% Glycerin 4.0% Castor oil 5.0% Castor oil 5.0% Ethanol, etc. to 100% Castor oil 6.0% Ethanol, etc. to 100% Ethanol, etc. to 100% thickness 500um 1000um 500um 500um Weight (1*6cm ² ) 0.5g 0.8g 0.5g 0.6g manufacturing method Solvent Casting Extrusion Solvent Casting Solvent Casting

Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 drug layer NaF 0.22% Hydrogen Peroxide 32% NaF 0.22% 3% hydrogen peroxide ZnCl ₂ 0.09% PVP 17% Sulfur extract 0.05% Hydrous silicic acid 10% Hydrous silicic acid 5.0% Glycerin 10.0% PVP 20.0% HPC 30% SLS 1.0% Span 80 3.50% Glycerin 10.0% Carbomer 1.0% water etc to 100% water etc to 100% Polyox (WSR303) 50% Polyox (WS301) 2.0% PEG 4% Glycerin 4.0% PG 3% support layer water etc to 100% [middle layer] Eudragit L 20% EC 8.8% Castor oil 5.0% HPMC 8.8% water etc to 100% HPC 2% SPAN80 5.0% Castor oil. 5.0% PG 1% SLS 1.0% DCPD 5.0% Ethanol 76.3% Incense 0.7% [Basic Layer] Hydrous silicic acid 5% Mint Flavor 0.5% Ethanol to 100% SLS 1% Poloxamers 3% Purified water to 100% thickness 500um 300um 300um 1000um Weight (1*6cm ² ) 0.8 0.2 0.2 0.8 manufacturing method Solvent Casting Solvent Casting Solvent Casting Extrusion

1) Polyox 301: Polyethylene oxide with a molecular weight of 4,000,000 Da

2) Polyox 303: Polyethylene oxide with a molecular weight of 7,000,000

3) Polyox N-80: Polyethylene oxide with a molecular weight of 200,000 Da

4) Ethyl cellulose: N-22 (N: ethoxy 48~49.5%, 22 cps)

5) Hydroxypropylmethylcellulose molecular weight less than 10,000 (6 cps)

[How to use]

The method of using the toothpaste (Example 1 and Comparative Example 1) for relieving cold teeth in Tables 1 and 2 is, after removing from the sachet packaging, the upper or lower jaw, the center of the tooth and gum border of the area where you want to improve or alleviate the cold tooth. attach it with After 10 minutes, use a toothbrush to wet the toothbrush with water, and then remove the patch by brushing.

The method of using the toothpaste (Example 3 and Comparative Example 3) for the purpose of preventing and alleviating gingivitis in Tables 1 and 2 is attached to the area where gingivitis occurs or bleeding gums, or attached to the upper or lower jaw. After attaching to the tooth boundary area, after 10 minutes, use a toothbrush to moisten the toothbrush with water, and then remove the attached toothpaste by brushing. In Tables 1 and 2, toothpaste for tooth whitening or for preventing staining and for maintaining tooth whitening effect (Examples 2 and 4, Comparative Examples 2 and 4) is used, after opening and taking out the sachet package, attached to the upper tooth alone or to the upper tooth. do. Once after curing for 10 minutes, the other time after 30 minutes, use a toothbrush to moisten the toothbrush with water, and then remove the patch by brushing. (If there is release paper, remove the release paper before attaching)

[Feeling of use survey]

First, a questionnaire was conducted on the feeling and removal power of each toothpaste for relieving pain during use. Thirty respondents applied the patches of Example 1 and Comparative Example 1 for 10 minutes per group, and then removed them by brushing their teeth. Then, each group responded to a questionnaire about the feeling of use after changing the product. In the same way, a questionnaire about the feeling during use was conducted for Example 2 and Comparative Example 3 with respect to toothpaste for the purpose of preventing and alleviating gingivitis. Thirty respondents applied the toothpaste of Example 2 and Comparative Example 3 for 10 minutes per group, and then removed it by brushing. Then, each group responded to a questionnaire about the feeling of use after changing the product. Finally, for the toothpaste for tooth whitening (Examples 3 and 4, Comparative Examples 2 and 4), each group was divided in half, each group was attached for 10 minutes and removed by brushing, one week first. The other group was allowed to use it for 1 week by attaching it for 30 minutes and removing it through brushing, and then answering the questionnaire.

[Cleanliness and detergency questionnaire]

- Based on survey response -

5: Refreshing and refreshing as if using paste toothpaste.

4: After use, both detergency and freshness are acceptable.

3: After use, either detergency or freshness is acceptable.

2: I don't want to use a separate paste toothpaste after use, but both the cleaning power and freshness are insufficient.

1: After use, it is steamy after use to the extent that I want to use paste toothpaste.

[Results of feeling of refreshment and detergency]

The results are shown in Table 3. It was confirmed that the embodiments of the present invention had excellent feeling of use and excellent detergency.

Since the abrasive is located inside the polymer matrix and the abrasive is released while the polymer is dissolved, the tooth surface can be cleaned by brushing after a certain period of time without interfering with the stabilization of the active drug ingredient.

[Questions related to comfort and foreign body sensation during use]

- Based on survey response -

5: There is no feeling of foreign matter, etc., and it is maintained very comfortably.

4: Easy to use.

3: Foreign body sensation is felt during use.

2: There is a foreign body sensation during use, and small pieces are felt in the mouth or tongue.

1: Foreign body sensation during use is very severe and it is inconvenient to use.

[Feeling of fit and feeling of foreign body during use]

The results are shown in Table 3. Embodiments of the present invention were not uncomfortable to wear, and were attached softly and flexibly when attached to the tooth surface.

In particular, these results were obtained by mixing a mixture of a hydrophilic cellulose-based polymer and a hydrophobic cellulose-based polymer with Polyox.

On the other hand, in the case of toothpaste with a three-layer structure (Comparative Example 2), the thickness was thick, and the feeling of use was not good. In addition, it was confirmed that a lot of residues were left in the removal process compared to the toothpaste of the present invention.

[Questions related to adhesion and stickiness]

- Based on survey response -

5: Strong adhesion between teeth and teeth/gums, and no stickiness on the inside of the lips

4: Adhesion to the teeth or the boundary between the teeth and gums is strong, but stickiness is felt on the inside of the lips.

3: The adhesive force of the tooth or the tooth/gum boundary is weak, but it does not feel sticky on the inside of the lips.

2: The adhesive strength of the teeth or the boundary between teeth and gums is weak, and stickiness is felt on the inside of the lips.

1: Does not adhere to teeth or tooth/gum boundary.

[Adhesive force result]

The results are shown in Table 3. It is important to ensure that the toothpaste of the present invention can be attached to the tooth surface. The toothpaste of the present invention could be stably attached to the teeth and the boundary between the gums and teeth without lifting. However, while the toothpastes of Comparative Examples 1 and 4 containing only Polyox were strongly sticky on the inside of the lips, they did not adhere well to the tooth surface with little moisture.

[Removing force questionnaire]

- Based on survey response -

5: Very convenient to remove, no tooth residue

4: Easy to remove, but leaves a little residue.

3: It is not convenient to remove, and the residue remains inconvenient.

2: Removal is inconvenient and leaves a lot of residue.

1: Removal is very inconvenient and leaves a lot of residue.

[Removal force result]

The results are shown in Table 3. Embodiments of the present invention could be easily removed from the tooth surface by brushing after a certain period of time, and did not leave residue on the tooth surface.

[Survey evaluation of clinical toothache, gingivitis improvement and tooth whitening effect in humans]

1) Test subject and method of use: Examples 1 and 2, Comparative Examples 1 and 4 are attached to the sore tooth or gum pain area for 10 minutes, and Examples 3 and 4, Comparative Examples 2 and 4 are 10 to 6 upper teeth It was attached by minutes or 30 minutes and then removed by brushing.

2) A questionnaire evaluation was conducted on a 5-point Likert scale after 1 week of use for 15 volunteers who felt cold teeth or gum pain in each group. In the case of whitening, 20 people who think their teeth are yellow and want a whitening effect in a short period of time are divided into two groups of 10 people, 10 people in Group A use it for 10 minutes each, 10 people in Group A use it for 1 week, and 10 people in Group B use it for 30 minutes first. After using it for 1 week, the following week was changed, and group A used 30 minutes for 1 week and group B used 10 minutes for 1 week, and then the questionnaire was evaluated on a 5-point Likert scale.

3) Scale standard

5 points: The effect of improving cold tooth/gum pain lasted for one month in all of the attached cold tooth/gum pain areas. The attached upper teeth were brighter than the lower teeth, and the whitening effect lasted for more than a month.

4 points: The effect of alleviating cold tooth/gum pain was clearly felt in all areas where it was attached. I definitely felt that the attached upper teeth were brighter than the lower teeth.

3 points: The effect of improving cold tooth/gum pain was clearly felt in one or more places where it was attached. Two or more of the central incisors, lateral incisors, and canines of the attached upper teeth were clearly brightened.

2 points: I felt less sensitive to cold food or gum pain after eating than before use. At least one of the central incisors, lateral incisors, and canines of the attached upper teeth was clearly brightened.

1 point: No improvement effect of cold tooth or gum pain was felt. I'm not sure if the upper teeth are brighter than the lower teeth.

Example 1 Example 2 Example 3 Example 4 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Cleansing Power 5 5 5 5 One 2 2 One removal power 5 5 5 5 5 3 4 5 adhesion 5 5 5 5 2 2 4 2 stickiness foreign body feeling 5 5 5 5 One 2 3 One sirin
improvement effect 5 - - One - - - gingivitis
improvement effect - 5 - - - - One - Whitening
tangible effect
(for 30 minutes) - 5 4 3 One Whitening
tangible effect
(for 10 minutes) 4 5 One One

[Stability of peroxide]

The inventors of the present invention conducted various experiments by adjusting the ratio of the polymer, which can be suggested as one way to overcome the instability of peroxide, which can occur when an abrasive and peroxide are mixed, and as a result, the following conclusions were obtained could

To evaluate the stability over time of peroxide during high-temperature storage, put it in a sachet, seal it, and store it in a thermostat at 50℃ to obtain the residual peroxide ratio of peroxide in the product according to the storage period. It was quantified by the peroxide titration method using sodium thiosulfate.

Stability over 50℃
(Residual peroxide ratio) Example 3 Example 4 Comparative Example 2 Comparative Example 4 Week 1 98% 98% 95% 50% Week 2 95% 95% 90% 40% Week 4 90% 90% 80% 30% week 8 90% 90% 75% 20%

As can be seen in Table 4, the peroxides included in the toothpastes of Examples 3 and 4 showed better stability over time than the toothpastes prepared by dividing the layers as in Comparative Example 2.

In addition, it was found that the stability over time of the peroxide in Comparative Example 4 made of a single layer was very poor.

That is, it was confirmed that the toothpaste of Examples 3 and 4 could be effectively used as a tooth whitening product without compromising the stability over time of the peroxide even though it was made of a single layer. The inventors of the present invention thought that these results could be obtained by the type and content of the abrasive included in the toothpastes of Examples 3 and 4 and the polymers used to make the adhesive toothpastes.

[Film toothpaste medicine Emission test method]

It was confirmed through the above experimental results that the toothpaste containing the whitening component can stably store the active agent.

Through the following experiments, the inventors of the present invention confirmed that the toothpaste of the present invention has a release rate suitable for releasing medicinal agents while remaining on the target area for a sufficient period of time even in a moist oral cavity for a certain period of time.

1. Operation and test method

The release test was tested using device 5 (paddle over disk) of the transdermal delivery system during the USP 25 drug release test. The test solution is a 0.9% sodium chloride solution, and samples are taken from Examples or Comparative Examples (each 1cm * 6cm). Pour 500mL of the test solution into the test tube and maintain the temperature of the test solution at 32 ± 0.5 °C during the drug release test. After fixing the sample on the upper surface of the disk that can be used as a sinker with double-sided tape, put it into the test tube with the side to which the sample is attached facing upward, and time the drug release from this moment. Prepare three test tubes for each sample in the same way and start the release test at the same time. When collecting the sample solution, after starting the test at a certain position (a position 1 cmm away from the wall of the test tube above the top of the blade of the paddle and the middle of the test liquid surface), 1 minute later in test tube #1, 10 minutes later in test tube #2, and 1 minute later in test tube #3 After this time, 100 mL of each sample is collected.

2. Results: Determination of the concentration of hydrogen peroxide (thiosulfate titration method)

Add 5 mL of 6N HCl, about 2 g of potassium iodide, and 1 drop of molybdenum ammonium solution (about 10% dispersion solution) to 100 mL of the sample taken in the release test and leave it in the dark for about 10 minutes. Add 3 mL of starch indicator here and titrate the free iodine with sodium thiosulfate solution.

Example 3 Example 4 Comparative Example 2 Comparative Example 4 Emissions in 1 minute less than 10% less than 10% less than 10% 75% or more Release in 10 minutes 30% or more 75% or more 20% or more Release in 20 minutes 75% or more more than 50%

As can be seen in Table 5, Comparative Example 4 prepared using polyox with a high molecular weight was observed to release more than 75% of the peroxide within 1 minute, and it was quickly dissolved in the oral cavity to achieve the desired effect. there was no In addition, when brushing, the abrasive was washed away before it functioned properly, so it could not have the desired abrasive and cleaning power.

Through the results of Examples 3 and 4 of the present invention, water-soluble polyox alone does not meet the purpose of the present invention, and low molecular weight polyethylene oxide is used together with high molecular weight polyethylene oxide to control the release rate of active ingredients I was able to get the desired result.

Claims (16)

A polymer mixture including i) polyethylene oxide or a polymer thereof, ii) a hydrophobic cellulose-based polymer and iii) a hydrophilic cellulose-based polymer and
iv) an abrasive and v) a medicinal agent,
single layer,
Film-type toothpaste, characterized in that the thickness of 400 to 1,200㎛. The film-type toothpaste according to claim 1, wherein the polymer mixture forms a film polymer matrix, and iv) the abrasive and v) the medicinal agent are included in the film polymer matrix. The method of claim 1, wherein the content ratio of i) polyethylene oxide or its polymer and ii) hydrophobic cellulose-based polymer and iii) hydrophilic cellulose-based polymer is 1:0.05 to 1:1 (weight of polyethylene oxide or its polymer: hydrophobic cellulose A film-type toothpaste, characterized in that the weight of the polymer-based polymer and the hydrophilic cellulose-based polymer. The film-type toothpaste according to claim 1, wherein i) polyethylene oxide or a polymer thereof is a single type or a mixture of two or more types of polyethylene oxide having different molecular weights. The film-type toothpaste according to claim 4, wherein the polyethylene oxide is a polyethylene oxide having a molecular weight of 3,000 to 7,000 kDa alone or a mixture with polyethylene oxide having a molecular weight of 100 kDa to 1,000 kDa. The film-type toothpaste according to claim 1, wherein the hydrophobic cellulose-based polymer is hydroxypropylmethyl cellulose phthalate, ethyl cellulose, ethyl methyl cellulose, ethyl hydroxyethyl cellulose, or a mixture thereof. The film-type toothpaste according to claim 6, wherein the ii) hydrophobic cellulose-based polymer is ethyl cellulose. The film-type toothpaste according to claim 1, wherein the iii) hydrophilic cellulose-based polymer is hydroxypropyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose, methyl cellulose, or a mixture thereof. The film-type toothpaste according to claim 8, wherein the iii) hydrophilic cellulose-based polymer is a mixture of hydroxypropyl cellulose and hydroxypropyl methyl cellulose. The film according to claim 1, wherein the mixing ratio of ii) hydrophobic cellulose-based polymer and iii) hydrophilic cellulose-based polymer is that the weight ratio of hydrophobic cellulose-based polymer: hydrophilic cellulose-based polymer is 3:1 to 1:3 brother toothpaste. The method of claim 1, iv) the abrasive is calcium pyrophosphate, hydrous silicic acid, colloidal silicon dioxide, calcium carbonate, sodium carbonate, baking soda, DCPD (dicalcium phosphate dehydrate), DCPA ((dicalcium phosphate anhydrous), alumina or any of these is a mixture,
The v) active agent is at least one selected from a tooth whitening component, a tooth decay preventing component, a calculus production inhibiting component, an anti-inflammatory component, an antibacterial component, a symptom improving or alleviating component, vitamins, minerals, and mixtures thereof. film type toothpaste. delete The film-type toothpaste according to claim 1, wherein the film-type toothpaste contains calcium pyrophosphate, colloidal silicon dioxide, or a mixture thereof as the abrasive, and peroxide as the active agent. delete delete The film-type toothpaste according to claim 1, wherein the film-type toothpaste is molded by extrusion.