JP6087144B2 - Dentifrice composition - Google Patents

Description

  The present invention relates to a dentifrice composition.

  Conventionally, oral compositions such as dentifrice compositions have been blended with cetylpyridinium chloride having a high bactericidal activity in order to suppress stain adhesion in the oral cavity or to suppress plaque formation. For example, Patent Document 1 discloses an oral composition that can enhance the adsorption effect of cetylpyridinium chloride on teeth and suppress the adhesion of stain by using a specific compound having a hydroxyl group such as thymol and isopropylmethylphenol. Things are disclosed. Moreover, in the composition for oral cavity described in Patent Document 2, the adsorption of cetylpyridinium chloride to teeth is promoted by containing a specific monohydric alcohol. Furthermore, Patent Document 3 discloses a composition for oral cavity in which a polyoxyethylene / polyoxypropylene block polymer is used in combination, and this composition can stabilize the antibacterial activity of cetylpyridinium chloride.

  On the other hand, in general, toothpaste compositions are blended with various powders as an abrasive to improve cleaning feeling by brushing with a toothbrush or the like. In any of the above compositions, such an abrasive is blended. Yes.

JP 2011-201861 A JP 2011-173873 A JP-A-4-202121

  However, it is useful for the present inventors to use calcium carbonate as an abrasive powder in order to improve the cleaning feeling with the feeling that the teeth are smooth after brushing with a toothbrush using a dentifrice composition. Although it discovered that there existed, it became clear that content of cetyl pyridinium chloride will fall when these abrasive powders are mix | blended with the said composition.

  The present invention, while using cetylpyridinium chloride and calcium carbonate together, is excellent in storage stability of cetylpyridinium chloride, brushing with a toothbrush, etc. The present invention relates to a dentifrice composition that provides a clean feel that does not leave powder in the oral cavity.

  Accordingly, the present inventors can provide a good cleaning feeling and improve the storage stability of cetylpyridinium chloride by using a specific amount of calcium carbonate and abrasive silica in combination while containing a specific amount of cetylpyridinium chloride. We have found a dentifrice composition that can be used.

That is, the present invention includes the following components (A), (B), (C) and (D):
(A) Cetylpyridinium chloride 0.005 mass% to 0.5 mass% (B) Calcium carbonate 5 mass% to 20 mass% (C) Abrasive silica (D) Contains water and has a pH of 8.2. The present invention relates to a dentifrice composition in a tube container, which is 9 or less and the total content of the component (B) and the component (C) is 10% by mass or more and 30% by mass or less.

According to the dentifrice composition of the present invention, it is possible to obtain a clean feel that the teeth are slippery after brushing with a toothbrush or the like, while preventing the powder from remaining in the oral cavity, and the residual amount of cetylpyridinium chloride is reduced. Can be effectively suppressed, and excellent antibacterial activity can be sufficiently exhibited.
In addition, when the tooth surface is touched with the tongue, it is possible to smoothly slide the tongue without feeling the presence of an adhering substance and the surface of the tooth is well cleaned. It feels like a clean feeling. Further, in the present invention, the clean feeling means that the dentifrice composition feels attached to the entire mucous membrane or tooth surface in the oral cavity after tooth brushing, or is contained in the adhering dentifrice composition. It means that there is no residual feeling that feels powdery depending on the body.

Hereinafter, the present invention will be described in detail.
The dentifrice composition of this invention contains 0.005 mass% or more and 0.5 mass% or less of cetyl pyridinium chloride (A). Content of a component (A) is 0.005 mass% or more in the dentifrice composition of this invention from a viewpoint of hold | maintaining the outstanding bactericidal activity, Preferably it is 0.01 mass% or more. Content of a component (A) is 0.5 mass% or less in the dentifrice composition of this invention from a viewpoint which ensures a storage stability, and a viewpoint which ensures favorable flavor, Preferably it is 0.1. It is at most 0.05% by mass, more preferably at most 0.05% by mass. Moreover, content of a component (A) is 0.005-0.5 mass%, Preferably it is 0.01-0.1 mass%, More preferably, it is 0.01-0.05 mass%. It is.

  The dentifrice composition of the present invention contains 5% by mass or more and 20% by mass or less of calcium carbonate (B). By containing the component (B) in such an amount, the performance as an abrasive can be sufficiently exerted to provide a good cleaning feeling, and the storage stability of the component (A) is effectively enhanced, and The tube container containing the dentifrice composition can be prevented from swelling.

  As a calcium carbonate of a component (B), 1 type or 2 types chosen from heavy calcium carbonate and light calcium carbonate are preferable. Generally, heavy calcium carbonate is used as the calcium carbonate contained in the dentifrice composition as an abrasive powder. Heavy calcium carbonate is a white powder that is obtained by pulverizing and purifying limestone and shells that contain calcium carbonate, and is a highly abrasive powder that is commercially available as calcium carbonate. It is also used as a food additive.

  In the dentifrice composition of the present invention, when heavy calcium carbonate is used as the component (B), the average particle size of the heavy calcium carbonate is preferably 0.1 μm or more from the viewpoint of providing a good cleaning feeling, More preferably, it is 1 μm or more. The average particle diameter of heavy calcium carbonate is preferably 50 μm or less, more preferably 10 μm or less, from the viewpoint of ensuring good dispersibility in the oral cavity and usability. The average particle diameter can be measured with a laser diffraction / scattering particle size distribution measuring apparatus.

  In general, light calcium carbonate is used as the calcium carbonate that is the raw material of the granules contained in the dentifrice composition. Light calcium carbonate is obtained by reacting carbon dioxide with lime milk in which slaked lime is dispersed in water, and high abrasiveness can be exhibited by using granules produced therefrom. Such granules can be obtained by combining light calcium carbonate with organic binders or inorganic binders and components such as water-insoluble fibers, or other components as necessary. It can be obtained by aggregating or complexing calcium.

In the dentifrice composition of the present invention, when light calcium carbonate is used as component (B), it is preferable to use granules produced from light calcium carbonate. That is, the dentifrice composition of this invention can contain the granule containing at least one part of the said component (B). By containing such granules, when applied to the oral cavity, the components (B) contained therein are gradually released as the granules disintegrate, and the storage stability of the components (A) is improved over a long period of time. An excellent polishing property can be applied while being held.
The average particle size of granules produced from light calcium carbonate that can be used in the dentifrice composition of the present invention is preferably 100 μm or more, more preferably 150 μm or more, from the viewpoint of providing a good cleaning feeling. Is 300 μm or less, more preferably 250 μm or less.

  In the dentifrice composition of the present invention, it is more preferable to use heavy calcium carbonate as the component (B) from the viewpoint of providing a better cleaning feeling.

  The content of the component (B) is 5% by mass in the dentifrice composition of the present invention from the viewpoint of ensuring a good cleaning feeling and from preventing the tube container containing the dentifrice composition from swelling. It is above, Preferably it is 7 mass% or more. The content of the component (B) is in the dentifrice composition of the present invention from the viewpoint of maintaining the high storage stability of the component (A) and preventing the residual feeling of the dentifrice composition in the oral cavity after brushing. Furthermore, it is 20 mass% or less, Preferably it is 18 mass% or less. Moreover, content of a component (B) is 5-20 mass% in the dentifrice composition of this invention, Preferably it is 7-18 mass%. In addition, when using light calcium carbonate as a component (B) and containing the granule manufactured from this, from the quantity of the light calcium carbonate contained in a granule, content of a component (B) and the component (B) mentioned later And the total content of the component (C) is converted and contained in the dentifrice composition of the present invention in such an amount that a predetermined value is obtained.

  The dentifrice composition of the present invention contains abrasive silica (C). By containing this component (C), the component (A) is sufficiently exerted as an abrasive in combination with the component (B) whose total content with the component (C) described later is in a specific range. It is possible to effectively suppress the remaining amount from being lowered while maintaining the storage stability of the resin. Component (C) has an oil absorption of silica of preferably 50 to 150 mL / 100 g, more preferably 70 to 130 mL / 100 g from the viewpoint of sufficiently exerting the action as an abrasive, and RDA value (Radioactive) Dentine Abrasion values) is preferably 80 to 230, more preferably 100 to 180, and even more preferably 120 to 150. The amount of oil absorption indicates the amount of oil that can be supported by silica, and the measurement method is specified by the method of JIS K5101-13-2 (established in 2004) according to the amount of oil absorbed in the boiled sea bream. Value. The RDA value can be measured by a tooth brushing RDA test method (Hefferren, Journal of Dental Research 1976, No: 7, 8 p. 563-573). The average particle size of the component (C) is preferably 1 to 25 μm, more preferably 2 to 20 μm, and still more preferably from the viewpoint of providing a good feeling of use while enhancing the smooth feel of teeth. 3 to 15 μm.

  Specific examples of commercially available components (C) include sorbosyl AC77 (PQ Corporation) (oil absorption: 129 mL / 100 g, RDA value: 125), thixosyl TX73 (rhodia) (oil absorption: 111 mL / 100 g, RDA value) : 100), sorbosyl AC33 (PQ Corporation) (oil absorption: 65 mL / 100 g, RDA value: 180), Zeordent 124 (Huber) (oil absorption: 70 mL / 100 g, RDA value: 150).

  In the dentifrice composition of the present invention, the total content of the component (B) and the component (C) is 10% by mass or more and 30% by mass or less. When the total content of the component (B) and the component (C) is within such a range, these components combine with each other to provide an excellent abrasiveness and provide a feel that is smooth on the teeth. A clear feel that the dentifrice composition is difficult to remain is obtained, the storage stability of the component (A) is maintained well, the decrease in the residual amount is suppressed, and the antibacterial activity can be sufficiently exhibited. The total content of the component (B) and the component (C) is 10% by mass or more and preferably 12% by mass or more in the dentifrice composition of the present invention from the viewpoint of exhibiting excellent polishing properties. . The total content of the component (B) and the component (C) is 30% by mass or less in the dentifrice composition of the present invention from the viewpoint of favorably maintaining the storage stability of the component (A), preferably It is 25 mass% or less, More preferably, it is 20 mass% or less. Moreover, the total content of the component (B) and the component (C) is 10 to 30% by mass in the dentifrice composition of the present invention, preferably 12 to 25% by mass, more preferably 12 to 20%. % By mass.

  In the dentifrice composition of the present invention, the mass ratio of the component (B) to the component (C) ((B) / (C)) is a residual that feels good cleaning and feels powdery in the oral cavity after use. From the viewpoint of suppressing the feeling, it is preferably 0.8 or more, more preferably 1 or more, and further preferably 1.5 or more. From the same viewpoint, the mass ratio of the component (B) to the component (C) ((B) / (C)) is preferably 4 or less, more preferably 3 or less. Moreover, the mass ratio ((B) / (C)) of the component (B) and the component (C) is preferably 0.8 to 4, more preferably 1 to 3, and further preferably 1.5. ~ 3.

The dentifrice composition of the present invention contains water (D). By containing this component (D), the dispersibility in the oral cavity of the dentifrice composition of this invention can be improved, and a favorable usability | use_condition can be brought about. The content of the component (D) is preferably 20% by mass in the dentifrice composition of the present invention from the viewpoint of enhancing dispersibility and suppressing the residual feeling of feeling powdery in the oral cavity after use. It is above, More preferably, it is 25 mass% or more, More preferably, it is 30 mass% or more. The content of the component (D) is preferably 60% by mass in the dentifrice composition of the present invention from the viewpoint of ensuring the shape retention of the dentifrice composition while having good dispersibility and improving the feeling of use. % Or less, more preferably 50% by mass or less, and still more preferably 45% by mass or less. Moreover, content of a component (D) becomes like this in the dentifrice composition of this invention, Preferably it is 20-60 mass%, More preferably, it is 25-50 mass%, More preferably, it is 30-45 mass%. is there. Here, the content of water in the dentifrice composition of the present invention includes water contained in a blending component such as a sorbitol liquid and water blended separately.
In addition, although the water content in a dentifrice composition can also be computed by calculation from the water content mix | blended and the water content in the mix | blended component, it can measure with a Karl Fischer moisture meter, for example. As the Karl Fischer moisture meter, for example, a trace moisture measuring device (Hiranuma Sangyo) can be used. In this device, 5 g of the toothpaste composition can be taken and suspended in 25 g of anhydrous methanol, and 0.02 g of this suspension can be collected to measure the amount of water.

  In the dentifrice composition of the present invention, the mass ratio of component (B) to component (D) ((B) / (D)) disperses component (B) well in the oral cavity and improves the feeling of cleaning. From a viewpoint and the viewpoint which suppresses the residual feeling which feels powderiness in the oral cavity after use, Preferably it is 0.1 or more, More preferably, it is 0.15 or more. The mass ratio of component (B) to component (D) ((B) / (D)) ensures the shape retention of the dentifrice composition while having good dispersibility, from the viewpoint of improving the feeling of use. , Preferably it is 1 or less, More preferably, it is 0.6 or less, More preferably, it is 0.5 or less. Moreover, the mass ratio ((B) / (D)) of the component (B) and the component (D) is preferably 0.1 to 1, more preferably 0.1 to 0.6, and still more preferably. Is 0.15 to 0.5.

  The dentifrice composition of the present invention preferably further contains a binder. Examples of the binder include sodium alginate, sodium carboxymethylcellulose, carrageenan, xanthan gum, sodium polyacrylate, hydroxyethylcellulose, hydroxypropylcellulose, pectin, tragacanth gum, gum arabic, guar gum, caraya gum, locust bean gum, gellan gum, tamarind gum, One type or two or more types selected from psyllium seed gum, polyvinyl alcohol, sodium chondroitin sulfate, and a methoxyethylene maleic anhydride copolymer are included. Especially, 1 type or 2 types or more chosen from sodium carboxymethylcellulose, a carrageenan, and a xanthan gum is preferable from a viewpoint of providing a favorable usability | use_condition. The content of the binder is preferably 0.05 to 3% by mass, more preferably 0.1 to 2% by mass, and further preferably 0.4 to 1 in the dentifrice composition of the present invention. 0.5% by mass.

  The dentifrice composition of the present invention has a viewpoint of ensuring the storage stability of the component (A), and when the dentifrice composition of the present invention is filled in a tube container, for example, the swelling in the container is caused by reaction with the component (B). From the viewpoint of effectively preventing the occurrence, the content of the pH adjuster comprising an acid is preferably 0.01% by mass or less, more preferably 0.001% by mass or less, or the pH adjustment comprising an acid. It is preferable not to contain an agent. Examples of the pH adjuster comprising an acid include organic acids such as acetic acid, fumaric acid, malic acid, lactic acid, gluconic acid and tartaric acid; and inorganic acids such as condensed phosphoric acid, phytic acid, hydrochloric acid and sulfuric acid.

  In the dentifrice composition of the present invention, in addition to the above components, an abrasive other than calcium carbonate; an anionic surfactant such as sodium lauryl sulfate; sorbitan fatty acid ester, glycerin fatty acid ester, Nonionic surfactants such as polyglycerin fatty acid esters and sucrose fatty acid esters; wetting agents such as glycerin and polyethylene glycol; fragrances such as menthol and anethole; sweeteners such as sodium saccharin and sucralose; preservatives: other than cetylpyridinium chloride Medicinal components and the like can be included as necessary.

The pH at 25 ° C. of the dentifrice composition of the present invention is a tube from the viewpoint of enhancing the storage stability of the component (A), and after filling the tube container with the dentifrice composition of the present invention and storing it until use. From the viewpoint of effectively preventing the occurrence of blistering of the container, it is 8.2 or more, more preferably 8.3 or more. The pH at 25 ° C. of the dentifrice composition of the present invention is preferably 9 or less, more preferably 8. from the viewpoint of securing a good taste and feeling of use and enhancing the storage stability of the component (A). It is 8 or less, more preferably 8.6 or less. Moreover, the pH at 25 ° C. of the dentifrice composition of the present invention is preferably 8.2 to 9, more preferably 8.2 to 8.8, and further preferably 8.3 to 8.6. .
The pH of the dentifrice composition of the present invention is a value measured using a pH electrode. Specifically, it is adjusted to an aqueous solution diluted with distilled water to a concentration of 10% by mass by adding distilled water. Means the measured value.

  In order to adjust the pH of the dentifrice composition of the present invention to the above range, it is preferable to use a pH adjuster other than a pH adjuster comprising an acid, such as a hydroxide such as sodium hydroxide, Examples thereof include one or more selected from ammonia or aqueous ammonia, lower alkanolamines, basic amino acids such as arginine and lysine.

  The form of the dentifrice composition of the present invention can be a toothpaste composition or a gel-like dentifrice composition depending on the intended use. In addition, the tube container filled with such a dentifrice composition has a thickness and flexibility capable of discharging the composition as a content when the body portion of the container body is pressed. The material preferably has a plurality of resin layers (multilayer resin layers), may have an aluminum layer as an intermediate layer, and the innermost layer is preferably low-density polyethylene. The tube container preferably has a shoulder portion in which one end portion of the cylindrical body portion is fused and the other end portion is integrally provided with a discharge port. In addition, it is preferable from a viewpoint provided with the softness | flexibility which a shoulder part and a discharge outlet are polyethylene, and it is easy to discharge to the last by pressing the trunk | drum part of a container main body. Examples of the resin constituting the resin layer of the body portion of the container body include low density polyethylene, high density polyethylene, polyethylene terephthalate, polypropylene, polyvinyl chloride, polylactic acid, polystyrene, and ethylene-vinyl alcohol copolymer (EVOH resin). In view of ease of extrusion, those having a polyethylene layer are preferable. The tube container filled with the dentifrice composition of the present invention can extrude and discharge the dentifrice composition filled by pressing the body part of the container body, so that carbon dioxide gas is contained in the filled dentifrice composition. When it occurs, it is considered that the body part of the container body will easily swell.

In relation to the above-described embodiment, the present invention further discloses the following preferred compositions.
[1] The following components (A), (B), (C) and (D):
(A) Cetylpyridinium chloride 0.005% by mass or more and 0.5% by mass or less (B) Calcium carbonate 5% by mass or more and 20% by mass or less (C) Abrasive silica (D) Contains water and component (B) And the component (C) total content is 10 mass% or more and 30 mass% or less, and the dentifrice composition with a tube container whose pH is 8.2 or more and 9 or less.
[2] The mass ratio ((B) / (C)) between the component (B) and the component (C) is preferably 0.8 or more, more preferably 1 or more, and further preferably 1.5 or more. The dentifrice composition in a tube container according to the above [1], which is preferably 4 or less, more preferably 3 or less.
[3] The content of component (A) is preferably 0.01% by mass or more, preferably 0.1% by mass or less, and more preferably 0.05% by mass or less. [2] A dentifrice composition in a tube container.

[4] The dentifrice composition in a tube container according to any one of the above [1] to [3], wherein the content of the component (B) is preferably 7% by mass or more, and preferably 18% by mass or less.
[5] Component (B) is preferably an average particle size of 0.1 μm or more, more preferably an average particle size of 1 μm or more, preferably an average particle size of 50 μm or less, more preferably an average particle size of 10 μm or less. The dentifrice composition in a tube container according to any one of the above [1] to [4], which is a heavy calcium carbonate.
[6] The dentifrice composition in a tube container according to any one of the above [1] to [5], wherein at least a part of the component (B) is light calcium carbonate preferably contained in granules having an average particle size of 100 μm or more and 300 μm or less. .

[7] The amount of oil absorption of the component (C) is preferably 50 to 150 mL / 100 g, more preferably 70 to 130 mL / 100 g, [1] to [6] The dentifrice composition in any one of the above tube containers .
[8] The RDA value of component (C) is preferably 80 to 230, more preferably 100 to 180, and still more preferably 120 to 150, any one of the above [1] to [7] tubes Dentifrice composition in a container.
[9] The average particle size of the component (C) is preferably 1 to 25 μm, more preferably 2 to 20 μm, and further preferably 3 to 15 μm, any one of the above [1] to [8] Dentifrice composition in a tube container.

[10] The total content of the component (B) and the component (C) is preferably 12% by mass or more, preferably 25% by mass or less, and more preferably 20% by mass or less. [9] The dentifrice composition in any one of the tube containers.
[11] The content of component (D) is preferably 20% by mass or more, more preferably 25% by mass or more, still more preferably 30% by mass or more, and preferably 60% by mass or less. More preferably, it is 50 mass% or less, More preferably, it is 45 mass% or less The said dentifrice composition with a tube container in any one of said [1]-[10].
[12] The mass ratio of component (B) to component (D) ((B) / (D)) is preferably 0.1 or more, more preferably 0.15 or more, and preferably 1 or less. Yes, more preferably 0.6 or less, and even more preferably 0.5 or less, the dentifrice composition in a tube container according to any one of the above [1] to [11].

[13] More preferably, it contains a binder, and the content of the binder is preferably 0.05 to 3% by mass, more preferably 0.1 to 2% by mass, and still more preferably. The dentifrice composition in a tube container according to any one of the above [1] to [12], which is 0.4 to 1.5% by mass.
[14] The dentifrice composition in any one of the above [1] to [13], further comprising one or more binders selected from sodium carboxymethylcellulose, carrageenan and xanthan gum.
[15] The content of the pH adjuster comprising an acid is preferably 0.01% by mass or less, more preferably 0.001% by mass or less, or preferably no acid-containing pH adjuster is contained. The dentifrice composition in a tube container according to any one of the above [1] to [14].
[16] The tube container according to any one of [1] to [15] above, wherein the pH at 25 ° C. is preferably 8.3 or more, preferably 8.8 or less, and more preferably 8.6 or less. Dentifrice composition.
[17] The above [1] to [16], in which the tube container preferably has a body thickness of the container body of 120 to 250 μm, preferably includes a multilayer resin layer, and preferably includes a polyethylene layer. The dentifrice composition in any one tube container.

  Hereinafter, the present invention will be specifically described based on examples. In addition, unless otherwise indicated in a table | surface, content of each component shows the mass%.

[Production Example 1: Production of granule 1 (calcium carbonate granule)]
Light calcium carbonate 75% by mass (average particle size 2-5 μm), colloidal silica 20% by mass (Snowtex SK Nissan Chemical Co., Ltd.), cellulose 5% by mass (KC Flock W-400 g, Nippon Paper Chemicals Co., Ltd.) and water are mixed The slurry was made into a water slurry and spray granulated with a spray granulator at an air blowing temperature of 200 ° C and an exhaust air temperature of 80 to 90 ° C. The obtained granules were classified with a sieve of 90 μm / 500 μm (particle diameter 90 to 500 μm) to obtain granules having an average particle diameter of 250 μm. The granules after spray drying were used for the production of a dentifrice composition. The resulting granules have a dry disintegration strength of 10 g / piece. The disintegration strength is an average value obtained by measuring 10 to 20 granules having a particle size (180 to 200 μm) using a micro compression tester (Shimadzu Corporation, MCTM-500).

[Production Example 2: Production of granule 2 (zinc-containing granule)]
Light calcium carbonate 95% by mass (average primary particle size: 0.05 μm) and zinc oxide 5% by mass were mixed, and zinc-containing granules having a zinc concentration of 5% by mass were produced by a rolling granulator. Specifically, light calcium carbonate and zinc oxide were mixed in the apparatus (Newgramachine SEG850 type), and granulated by adding 15 parts by mass of purified water to 100 parts by mass of the powder during granulation. After completion of the granulation step, it was produced by drying for 20 to 30 minutes with a dryer (rotary kiln). The obtained zinc-containing granules were classified by sieving to obtain granules having an average particle diameter of 200 μm. The dried granule was used for the production of a dentifrice composition.

[Examples 1 to 3, Comparative Examples 1 to 5]
According to the prescription shown in Tables 1-2, after obtaining the dentifrice composition using the granule 1 or the granule 2 as needed, each measurement and evaluation were performed according to the following methods and criteria. The results are shown in Tables 1-2.

<PH>
Distilled water was added to each composition to prepare an aqueous solution diluted to a concentration at which the dentifrice composition was 10% by mass, and the pH of the composition at 25 ° C. was measured using a pH electrode.

<< Evaluation of storage stability of cetylpyridinium chloride: Measurement of residual ratio >>
50 g of each prepared dentifrice composition was filled in a tube container having a capacity of 50 g, sealed with a lid, and then Example 1 and Comparative Example 1 were stored in a constant temperature bath at 40 ° C. for 3 months. Comparative Examples 2 to 5 were stored in a thermostat at 50 ° C. for 1 month. In the tube container used, the body portion of the container main body, the innermost layer is linear low density polyethylene, and the outermost layer is provided with a printing layer (including varnish), and the printing layer / low density polyethylene 50 μm / adhesive / It consisted of a multilayer resin layer comprising an aluminum layer in the intermediate layer, which was composed of high density polyethylene 80 μm / adhesive / aluminum 12 μm / adhesive / polyethylene terephthalate 12 μm / adhesive / linear low density polyethylene 100 μm. Moreover, the tube container was provided with the shoulder part which is integrally provided with the discharge port, and the shoulder part and the discharge port were made of polyethylene. About the dentifrice composition after a preservation | save, according to the method shown below, content of each component, the swelling of a container, and the feeling of cleaning were evaluated. The results are shown in Tables 1-2.

《Cetylpyridinium chloride remaining rate》
The residual amount of component (A) cetylpyridinium chloride after storage was measured by HPLC (high performance liquid chromatography), and the mass ratio of the content to cetylpyridinium chloride before storage was defined as the residual rate.
<Measurement conditions for HPLC (High Performance Liquid Chromatography)>
Apparatus: Hitachi High-Performance Liquid Chromatogram La chromaElite
Column: CAPCELL PAK SCX UG80 (4.6 × 100mm, 5μm) (Manufacturer: Shiseido)
Column temperature: 40 ° C
Mobile phase: 0.05 mol / L sodium perchlorate-containing methanol / water mixture (methanol: water = 3: 1)
Flow rate: 1.2mL / Min
Sample injection volume: 20 μL
Measurement wavelength: 260 nm

<< Evaluation of swelling of tube container >>
A tube container with a dentifrice composition (total length 110 cm, width of the sealed end of the container body 4 cm) filled with 50 g of each dentifrice composition in a tube container of 50 g capacity, sealed with a lid, The tube container is gently put into a container (110.5 cm × 8.5 cm, a box-shaped container with an opening of 5.5 cm in height) filled with the top surface. When filling the dentifrice composition into the tube container, air is prevented from being mixed in. The tube container sinks and there is no portion protruding from the water surface. By introducing the tube container, the overflowed water was collected and the mass was measured. The difference between the mass of the water after storage and the mass of the water before storage was defined as the swelling of the tube container after storage.

《Evaluation of cleaning feeling and residual feeling》
1 g of each dentifrice composition is discharged from a tube container and applied to a toothbrush. After brushing for 2 minutes by three specialist panelists, the oral cavity is rinsed with water, and then the feel of touching the tooth surface with the tongue and the oral cavity The touch was evaluated according to the following evaluation criteria. Tables 1 and 2 show the results of the three-person discussion.
3: There is a good cleaning feeling that the tooth surface is smooth, and there is no feeling that the dentifrice composition adheres to the oral cavity or a residual feeling that remains powdery.
2: The tooth surface is not so smooth, and there is a slight residual feeling that the toothpaste composition is adhered to the oral cavity and the powdery texture remains.
1: The tooth surface is smooth, but there is a residual feeling that the dentifrice composition and powder adhere to the oral cavity.

  As shown in Table 1, although Example 1 uses calcium carbonate as the component (B), the stability of cetylpyridinium chloride is good, whereas Comparative Example 1 having a high pH shows that after storage of cetylpyridinium chloride. It was observed that the content was decreasing. As shown in Table 2, in Comparative Examples 2, 3 and 4 having a pH of 8 or 8.1, it was confirmed that the tube container swelled, and the abrasive powders of the component (B) and the component (C) Despite the small amount, a residual feeling was felt as if powder remained in the oral cavity. In contrast, Examples 2 and 3 containing specific amounts of calcium carbonate and abrasive silica not only effectively prevented a decrease in the residual amount of cetylpyridinium chloride after storage, In spite of the large amount, it was confirmed that adhesion of the composition and residual powder were not felt in the oral cavity, and swelling of the tube container after storage was also suppressed. In addition, although the comparative example 5 which contains a component (B) fully has prevented the swelling of the tube container after a preservation | save, it was confirmed that the adhesion of a composition and the residue of powder | flour remain in an oral cavity.

Claims (9)

The following components (A), (B), (C) and (D):
(A) Cetylpyridinium chloride 0.005 mass% or more and 0.5 mass% or less (B) Calcium carbonate 5 mass% or more and 20 mass% or less (C) Oil absorption is 50-150 mL / 100g, and an average particle diameter is 1 containing <br/> a is abrasive silica (D) water 25 wt% to 60 wt% or less ～25Myuemu, and component (B) and component (C) the total content of more than 10% by weight to 20% by weight of A dentifrice composition in a tube container, wherein the mass ratio of component (B) to component (C) ((B) / (C)) is from 0.8 to 4, and the pH is from 8.2 to 9 (However, a dentifrice composition containing ascorbic acid phosphate or a salt thereof is excluded) . The dentifrice composition of Claim 1 whose mass ratio ((B) / (C)) of a component (B) and a component (C) is 1.5 or more and 3 or less.   The dentifrice composition of Claim 1 or 2 whose mass ratio ((B) / (D)) of a component (B) and a component (D) is 0.1 or more and 1 or less.   The dentifrice composition of any one of Claims 1-3 containing the granule containing at least one part of a component (B).   The dentifrice composition of any one of Claims 1-4 containing a binder.   The dentifrice composition according to any one of claims 1 to 5, wherein the content of the pH adjuster comprising an acid is 0.01% by mass or less, or the pH adjuster comprising an acid is not contained. The RDA value of a component ( C ) is 80-230, The dentifrice composition of any one of Claims 1-6.   The dentifrice composition according to any one of claims 1 to 7, wherein the component (B) is heavy calcium carbonate having an average particle size of 0.1 µm to 50 µm.   The dentifrice composition according to any one of claims 1 to 7, wherein at least a part of the component (B) is light calcium carbonate contained in granules having an average particle size of 100 µm to 300 µm.