KR100951396B1 - Dental composition for antiplaque and antigingivity - Google Patents

Abstract

The present invention relates to a toothpaste composition excellent in bad breath removal, plaque removal and antimicrobial effect, and in particular, to the toothpaste composition characterized in that the coating of the cetylpyridinium chloride to the abrasive granules, By applying cetylpyridinium chloride to the abrasive granules, it maintains cetylpyridinium chloride in a stable state during the oral application, and also increases the adhesion of cetylpyridinium chloride to the teeth to maintain efficacy. It can be expected that the stability with other components and the safety of teeth can be excellent in the effects of bad breath removal, antibacterial action and plaque suppression, and can provide a safe toothpaste composition with high stability.

Cetylpyridinium chloride, toothpaste, composition, granule, coating.

Description

Toothpaste composition excellent in bad breath removal, plaque removal and antibacterial effect {DENTAL COMPOSITION FOR ANTIPLAQUE AND ANTIGINGIVITY}

The present invention relates to a toothpaste composition excellent in bad breath removal, plaque removal and antibacterial effect, and more particularly, to a toothpaste composition to which the cetylpyridinium chloride is coated on the abrasive grains.

Bad breath is caused by the presence of food residues in the oral cavity, the presence of plaque and inflammation of the periodontal tissues in preference to the presence of sulfur-containing substances in the oral cavity, diseases of the stomach or lungs, and lack of salivary secretion. Is a problem.

Plaque, which is one of the causes of bad breath, is called plaque or plaque, and refers to a lump before it is adhered to the tooth surface by bacteria and its by-products and food residues in the oral cavity, before being calcified into a dense and microorganism such as a gel. These plaques are formed by calcareous calculus and cause inflammatory periodontal disease, which is recognized as the most important factor in oral diseases.                         

Therefore, the management of plaque and the resulting inflammation is not an exaggeration to say that it is the most essential element in oral care. The plaque test is the most important test item in the oral condition and health status, periodontal treatment is not established without plaque control.

Cetylpyridinium chloride, which has excellent inhibitory ability against plaque and is frequently used in oral fluids and dentifrices of medicines and quasi-drugs with high antibacterial activity, has recently been set as a public notice item because of its recognition of its efficacy and its excellent stability and safety [2000 standards and Test Method 2 Amendment 1].

Cetylpyridinium Chloride (hereinafter referred to as "CPC") is a cationic antimicrobial agent useful for inhibiting calculus. There is a disadvantage that is not persistent. Specifically, CPC suppresses tartar by covalently binding to bacterial membranes or saliva proteins while having a cation, and exhibits antimicrobial activity against bacteria in saliva, compared with the results of in vitro experiments. The results for gingivitis appear to be unsatisfactory [ J. Oral Rehabilitation 1985, 12, 81; J. Clinical Periodontology 1988, 15, 488]. This is because CPC has an excellent antimicrobial effect and rapidly decomposes in the oral tissues even though they adhere quickly to the oral tissues, and the action cannot be continued for a long time. For this reason, cetylpyridinium chloride is limited in its use despite its excellent effect.

In the related art, a simple composition of a general toothpaste composition containing CPC (International Patent Publication No. 94-700051) or an example of applying CPC as a powder (Korean Journal of Periodontal Medicine 1999, 29, 1, p144) has been reported. Due to the rapid decomposition of CPC, its efficacy is not sustained, and when applied as a powder, there is a concern about adverse effects such as wear and irritation on the teeth of the CPC itself.

Therefore, there is a need for an active method considering the stability of the tooth as well as the continuous enhancement of the effect when applying the cetylpyridinium chloride excellent in the effect.

The present invention is to solve the above problems, it is to provide a toothpaste composition that can be coated on the granules of cetylpyridinium chloride to increase its stability and maximize the effect when applied to the product.

In order to achieve the above object, the present invention provides a toothpaste composition in the toothpaste composition, which is coated with cetylpyridinium chloride on the surface of the granules as an active ingredient.

In other words, by applying the coating on the surface of the granules of cetylpyridinium chloride with a coating agent, the toothpaste composition to the continuous antimicrobial action and physical properties of the granules to the toothpaste composition, thereby giving It can enhance the plaque suppression effect to the part, and it is characterized by showing bad breath removal, plaque removal and antibacterial effect.

Hereinafter, the present invention will be described in detail.

In constructing the toothpaste composition of the present invention, a feature of the present invention is to apply the coating of the surface of the granules with cetylpyridinium chloride using a coating agent.

Cetylpyridinium chloride is a cationic antimicrobial agent useful for inhibiting calculus and is characterized by fewer side effects such as tooth staining of other similar antimicrobial agents. Specifically, while having a cation, covalent bonds with bacterial membranes or saliva proteins inhibits calculus and shows antimicrobial activity against bacteria in saliva. Cetylpyridinium chloride is contained as one of the active ingredients of the toothpaste composition in the present invention, the content is preferably 0.01 to 5% by weight based on the total composition.

In the present invention, the granules serve as drug carriers to improve the stability of cetylpyridinium chloride by coating cetylpyridinium chloride on the surface thereof, and also to impart the physical properties of the granules themselves to plaque to the minute parts between the interdental teeth. It exhibits features that can enhance the inhibitory effect.

The granules should be defined in appropriate size and strength in consideration of the manufacturing process, the mouth feel of the consumer, and the stability in application in the toothpaste. Specifically, if the strength of the granules is too high, it may damage the tooth surface by imparting the teeth, and if the strength of the granules is weak, the granules may be destroyed during the toothpaste manufacturing process and lose meaning as granules. Therefore, the strength of the granules, which are not destroyed in the manufacturing process but destroyed when brushing, is suitably 150-650 g / cm 2. In addition, the size of the granules is suitable from 100 to 750 ㎛. The size is a size having a good feeling without feeling a foreign object in use.

In addition, the granules are beneficial to abrasives, and precipitated calcium carbonate, silica, zeolite, clad silicon dioxide and calcium phosphate anhydride may be used as possible abrasives that are granulated and distributed.

The granules are contained as an active ingredient of the toothpaste composition in the present invention, wherein the content is preferably 0.1 to 10% by weight based on the total composition.

The coating of the present invention is carried out using a coating agent, and the coating agent is used to coat cetylpyridinium chloride on the surface of the granules, which is stably contained in the dentifrice composition to easily release cetylpyridinium chloride when applied in the oral cavity. Preferred are materials that can be and easily destroyed in the oral cavity. In the present invention, as a water-soluble high molecular material, a substance that is poorly used in pharmaceutical applications with high stability is used, and specifically, polyethylene glycol, methyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, ethyl cellulose, hydroxy cellulose, polyvinyl alcohol , At least one selected from the group consisting of polyvinylpyrrolidone and other waxes. In addition, saliva and substances that can be degraded by enzymes present in saliva can also be used.

The method of coating the surface of granules with cetylpyridinium chloride using a coating agent can use all conventional methods known in the art. For example, there is a coating method using a fluidized bed granulator and a coating method using a deposition method. In the coating method using the induction layer granulator, the coating agent and the granules are mixed, and the granules are floated using the fluidized bed granulator. After coating, the solvent is removed through a drying process, and then filtered through a suitable sieve to completely remove the solvent and evenly distribute the solvent. In addition, the coating method using the deeping method should be given the appropriate concentration and conditions in consideration of the properties of the deposition solvent and granules when immersing the granules.

In addition, the toothpaste composition of the present invention contains the herbal extract in addition to the toothpaste composition containing cetylpyridinium chloride and granules as an active ingredient. The herbal extracts are tea tree oil, tea extract, chamomile, ratania, myrr and pine needle extract. The herbal extracts contain flavonoids to show the efficacy of anti-inflammatory and blood circulation, and further include them in the toothpaste composition, thereby providing synergistic activity to the desired efficacy in the present invention. The content of the herbal extract is preferably 0.01 to 10 parts by weight based on 100% by weight of the toothpaste composition.

In addition, the toothpaste composition of the present invention usually contains a caking additive, a humectant, a foaming agent, a sweetener and a flavoring component. In particular, in the present invention, by using the granules as polishing granules, it is possible to reduce or not use the amount of abrasives usually included.

Abrasives are to maintain the cleaning and gloss of teeth, dicalcium phosphate dihydrate and anhydride, dicalcium phosphate, calcium carbonate, calcium pyrophosphate, aluminum hydroxide, silicic anhydride, aluminum silicate, insoluble sodium metaphosphate, tertiary It contains one or more selected from magnesium phosphate, magnesium carbonate calcium sulfate, methyl polymethacrylate, and other synthetic resins.

The binder serves to prevent the solid powder component and the liquid component from being separated, and is essential for the ointment toothpaste, and any water-soluble polymer may be used. Specifically, sodium carboxymethylcellulose synthesized from cellulose of trees, carrageenans extracted from seaweeds and xanthan gum carboples obtained from microorganisms and mixtures thereof may be used.

Moisturizing agents use sorbitol, glycerin, concentrated glycerin, xylitol, ethylene glycol, propylene glycol, polyethylene glycol, polypropylene glycol and mixtures thereof.

Foaming agent enhances the feeling of use of the product, helps cleansing action, and facilitates the dissolution of foreign substances in the oral cavity by speeding up the dispersion and penetration of other active ingredients and reducing the interfacial tension. As the foaming agent, sodium lauryl sulfate, an anionic surfactant, is mainly used, and a copolymer of polyoxyethylene polyoxypropylene (poloxamer), polyoxyethylene cured castor oil, poly Oxyethylene sorbitan fatty acid ester and the like can be used.

In addition, it may contain other active ingredients, typically fluoride, sodium fluoride, sodium fluoride phosphate may be used alone or mixed as a fluorine ion source. For the purpose of preventing periodontal disease, water-soluble salts such as sodium chloride or sodium bicarbonate with high osmotic pressure, aminocapronic acid, allantoin, and allantoin derivatives having hemostatic action and various vitamins can be used simultaneously.                     

Other toothpaste compositions of the present invention are used for flavoring, sweetening, food coloring and flavoring to improve the feeling, metol, anetol, eucalyptol, thymol, peppermint oil, spearmint oil, sage, methyl salicylate and Fruit extracts can be used.

Conventional toothpaste compositions consist of the following ratios.

Ingredient Content ratio (weight ratio) abrasive 10 to 60 Moisturizer 20 to 75 Binder 0.5 to 10 Foam 1 to 3 water 4-50 Active ingredient of the present invention 2 to 6 Preservative               0.2 to 1.2 Sweetener incense

Hereinafter, the present invention will be described in detail with reference to examples.

However, the following examples are merely to illustrate the invention, but the content of the present invention is not limited by the following examples.

Preparation Examples 1 to 4 Coating of Cetylpyridinium Chloride on Granules

The granules were SiO ₂ (Sorbosil BFG50, Ineos, UK), and the solvent was used as a water: ethanol mixed solvent or water through several preliminary experiments, and the coating method was a coating method using a fluidized bed granulator. Specific components and contents are shown in Table 2 below.

Preparation Example 1 Production Example 2 Production Example 3 Preparation Example 4 Type of granule SiO ₂ SiO ₂ SiO ₂ SiO ₂ HPMC (%) ^* 5 5 5 5 CPC (%) ^** 2 2 2 2 menstruum water water Water: Ethanol (8: 2) Water: Ethanol (8: 2) CPC (%) / granule (g) 0.05 0.1 0.05 0.1 yield(%) 99.8 100.1 98.2 99.2  *: HPMC stands for (Hydroxypropyl methylcellulose) **: CPC stands for cetylpyridinium chloride.

Coating conditions were operated as follows.

Fluid bed granulator was used FIFUND FIF200, coating was carried out under the following conditions.

<Operating Bed Assembly Condition>

(1) Start dust collector before work

(2) Mixing time: 20 minutes at 60 ° C (raw material drying in parallel)

(3) Out Let Damp: granule start 1 stage → after 3 stage

(4) In Let Damp: granule start 3 steps → after 6 steps

(5) Spray rate: 400 to 500 ml / min (average = 450 ml / min)

(6) Drying temperature: 70 → 65 ℃

(7) soup temperature: 3 kg / ㎠

(8) Steam pressure: 3 kg / ㎠

(9) Compressed air source: 6 ㎏ / ㎠

(10) Spray air pressure: 4 kg / ㎠

As shown in Table 2 , the coating yields a difference in the concentration of cetylpyridinium chloride contained in the granules, and as a result, a high yield of 99.3% was obtained, and no difference was found between solvents. It is also good and the particle size is composed of 100 ~ 700 ㎛.

<Examples 1-2> Preparation of the toothpaste composition of this invention

Binder and other additives were previously dispersed in the humectant, and weakly active ingredients such as an abrasive and an anti-tartar was added, followed by stirring for about 30 minutes.

Finally, the foaming agent and the flavoring agent were added, followed by stirring for 20 minutes in a vacuum to prepare a toothpaste composition of the present invention.

In addition, in order to compare the toothpaste composition of the present invention in the same way to prepare a conventional toothpaste composition was used as a comparative example.

Each added component and composition ratio are as Table 3 below.

<Comparative Examples 1 to 3> Preparation of Toothpaste Composition

As shown in Table 3 below, each added component was prepared in the same manner as in the above Example according to the composition ratio.

Component and Composition Ratio (wt%) ingredient Example 1 Example 2 Comparative Example 1 Comparative Example 2 Comparative Example 3 Colloidal silicon dioxide 10 10 10 10 10 Sodium monofluorophosphate 0.76 0.76 0.76 0.76 0.76 Carboxymethylcellulose Sodium 0.6 0.6 0.6 0.6 0.6 Sodium Lauryl Sulfate 2.0 2.0 2.0 2.0 2.0 Concentrated glycerin 3.0 3.0 3.0 3.0 3.0 Sorbitol liquid (70% liquid) 63.5 63.5 63.5 63.5 63.5 Saccharin Sodium 0.2 0.2 0.2 0.2 0.2 Incremental Silica 8 8 8 8 8 Methyl paraben 0.2 0.2 0.2 0.2 0.2 Titanium dioxide 0.3 0.3 0.3 0.3 0.3 Spices 0.8 0.8 0.8 0.8 0.8 Preparation Example 1 One - - - - Production Example 2 - One - - - Cetylpyridinium Chloride - - 0.05 0.1 - water Remainder Remainder Remainder Remainder Remainder

Experimental Example 1 Stability Experiment of Toothpaste Composition

Experiments were conducted to confirm the stability of the dentifrice compositions prepared by the examples and comparative examples.

Each toothpaste composition was stored in a thermostat at 30 ° C., 40 ° C. and 50 ° C. for 12 weeks, and then the physical stability of the toothpaste composition was observed. The results are shown in Table 4 below.

Temperature Example 1 Example 2 Comparative Example 1 Comparative Example 2 Comparative Example 3 0 ℃ stability stability stability stability stability 30 ℃ stability stability stability stability stability 40 ℃ stability stability 10 weeks later After 8 weeks bleaching and separation stability 50 ℃ stability stability 9 weeks later After 7 weeks stability

As shown in Table 4 , Examples 1 and 2 of the present invention shows a stable at a temperature of 0 ~ 50 ℃, in the comparative example after 7 weeks decolorization and the phenomenon that the powder and liquid components of the composition is separated It can be seen that. However, in the case of Comparative Example 3, it is shown that it is stable. Through this, it can be seen that the toothpaste composition containing cetylpyridinium chloride itself is less stable than the toothpaste composition containing no cetylpyridinium chloride (Comparative Example 3), and coated the granules with cetylpyridinium chloride as in the present invention. When included, it can be seen that the stability of the toothpaste composition is improved.

Experimental Example 2 Measurement of PCR and RDA

In order to determine the cleaning ability and polishing power of the toothpaste composition of the present invention, the conventional fat cleaning ratio (PCR) and radioactive dentine abrasion (RDA) values were measured. The results are shown in Table 5 below.

Example 1 Example 2 Comparative Example 1 Comparative Example 2 Comparative Example 3 PCR 115 126 95 108 80 RDA 72 80 77 74 75

As shown in Table 5 , the PCR values were high in Examples 1 and 2 of the present invention, and the RDA values showed all similar values. This means that the granules contain better cleaning power rather than higher polishing power, that is, the granules transfer cetylpyridinium chloride to the interdental area, thereby increasing the cleaning power of the transferred cetylpyridinium chloride rather than the abrasiveness of the granule itself. do.

Experimental Example 3 MIC Measurement

MIC measurement was carried out to determine the antimicrobial activity against the fungus and causative agent of periodontal disease on the toothpaste composition of the present invention.

Brain heart infusion agar (BHIA) containing CPC concentration was used to evaluate the antimicrobial activity by agar medium dilution method. The periodontal pathogens were cultured for 5 days at 37 ° C. and 5% CO _{2. For} caries, they were cultured at 37 ° C. for 2 days under aerobic conditions. MIC).

In addition, the antibacterial activity was evaluated by agar medium dilution method using BHIA containing Example 1 and Comparative Example 3 by concentration. The test concentration was diluted twice from the 50-fold dilution concentration (10 ㎍ / ㎖) of the test toothpaste was carried out in a total dilution concentration of 10 steps.

The results are shown in Table 6 below.

(1) Test bacteria

① Periodontal pathogens: Actionbacilus Actinomycetemcomitans ATCC 29522, Fusobacterium nucleatum ATCC 25586.

② caries cause: Streptococcus mutans ATCC 25175, Actinomyces viscosus ATCC 158987.

(2) medium used

Blood agar medium (blood agar base + final volume 5% blood) BHI agar

Measurement of MIC (Minimum Inhibitory Concentration) (Unit: ㎍ / ㎖) Test bacteria MIC Example 1 (dilution factor) Comparative Example 3 (dilution factor) A. Actinomycetemcomitans 8 100 100 F. nucleatum 2 400 100 Streptococcus mutans 0.5 800 400 Actinomyces viscosus 2 800 400

As shown in Table 6 , the MIC for showing the antimicrobial activity to each test bacterium was found to be 0.5 ~ 8 ㎍ / ㎖, Example 1 of the present invention compared to Comparative Example 3 in the experimental strain, respectively, on average 2 times The degree of antimicrobial activity is shown, and it can be seen that the elution of cetylpyridinium chloride in the cetylpyridinium chloride coated granules contained in the toothpaste composition of the present invention is smooth and shows excellent antimicrobial activity.

Experimental Example 4 Measurement of Bad Breath Removal Effect of Toothpaste Composition

In order to find out the effect of removing bad breath on the toothpaste composition, we recruited about 60 clinical subjects who perceived bad breath as usual, and then ate the same meal. Quantification.

Weak or very strong people with bad breath were excluded from the test subjects and each group was divided into 10 groups to adjust the average value to be similar between each group. The next day, after confirming the reproducibility of the experimental value, the same meal and snacks were eaten, and after 1 hour, the initial bad breath was measured, and after each hour, each group was brushed with the same method and time. Was measured. Differences in the Harimetta value before and after brushing were obtained and the mean value was compared for each group. The results are shown in Table 7 .

Example 1 Example 2 Comparative Example 1 Comparative Example 2 Comparative Example 3 Difference before and after brushing 230 258 130 185 90

As shown in Table 7 , it was found that the toothpaste compositions of Comparative Examples 1 and 2 containing the toothpaste composition and cetylpyridinium chloride of the present invention had an excellent bad breath effect. In particular, it was confirmed that the toothpaste composition of the present invention exhibited a more bad breath effect than those containing generally cetylpyridinium chloride (Comparative Examples 1 and 2).

Experimental Example 5 Plaque Test PCR

Plaque test is the most important test item for oral condition and health condition, and periodontal treatment is not established without plaque control.

Since it was difficult to visually determine the adherence state of the plaque, the staining was performed. The dye was mainly erythrosin-based, and the dye was applied to the surface of the teeth by moistening the dye solution in a cotton ball. After brushing, the adhesion surface of the stained plaque was calculated. O'Leary's Plaque Control Record (PCR), which is commonly used in daily clinical practice as an index indicating plaque adhesion, divided the tooth surface into four sides (buccal, lingual, mesial, and distal) and calculated the number of stained surfaces. (President of Periodontal Science, Nam Yong Ok). The results are shown in Table 8 below.

Example 1 Example 2 Comparative Example 1 Comparative Example 2 Comparative Example 3 PCR Pack 15 20 10 15 5

As shown in Table 8 , it was found that the toothpaste composition of Comparative Examples 1 and 2 containing the toothpaste composition of the present invention and cetylpyridinium chloride has an excellent bad breath effect.

As described above, the toothpaste composition of the present invention is coated by applying the cetylpyridinium chloride to the abrasive granules, thereby maintaining the cetylpyridinium chloride in a stable state during the oral application, and also of cetylpyridinium chloride Not only to maintain the efficacy by increasing the adhesion, but also can be expected to be stable with other components and the safety of the teeth can be excellent in the effects of bad breath removal, antibacterial action and plaque suppression, and can provide a safe toothpaste composition with high stability. In addition, the toothpaste composition of the present invention provides synergistic activity to the desired efficacy by adding several kinds of herbal extracts complexed to the toothpaste composition with the efficacy of anti-inflammatory and blood promotion.

Claims (7)

In the toothpaste composition, at least one water-soluble type selected from the group consisting of polyethylene glycol, methyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, ethyl cellulose, hydroxy cellulose, polyvinyl alcohol, polyvinylpyrrolidone and waxes Toothpaste composition using the polymer as a coating agent coated with cetylpyridinium chloride on the surface of the abrasive granules as an active ingredient. The toothpaste composition according to claim 1, wherein the polishing granules are polishing granules selected from the group consisting of precipitated calcium carbonate, silica, zeolite, clad silicon dioxide and calcium phosphate anhydride. The dentifrice composition according to claim 1, wherein the content of cetylpyridinium chloride is 0.01 to 5% by weight based on the total composition. The dentifrice composition according to claim 1, wherein the content of the granules is 0.1 to 10% by weight based on the total composition. The dentifrice composition of claim 2 wherein the granules have a particle size of 100-750 μm and have a strength of 150-650 g / cm 2. delete The method of claim 1, wherein the toothpaste composition further comprises selected from the group consisting of tea tree oil (Tea tree oil), bovine extract, Chamomile, Ratania, Myrr and pine needle extract Toothpaste composition, characterized in that.