JP6236773B2 - Opaque dentifrice composition - Google Patents

Description

  The present invention relates to an opaque dentifrice composition in which granules are dispersed and blended, which improves the cleanability of tooth gaps and is excellent in the effect of suppressing discoloration of the dentifrice over time.

  In general, dentifrice compositions have improved cleaning power by blending abrasives, but methods have also been proposed to further improve the cleaning power and effect by dispersing and blending granules.

The technique which mix | blends a granule as a means to raise the cleaning power of a dentifrice composition is proposed by patent documents 1-4.
In Patent Document 1 (Japanese Patent Laid-Open No. 1-299211), when a granule having a certain particle size and strength is blended, the granule can be recognized in the mouth, and an effect can be obtained and the polishing power can be obtained without damaging the teeth. It has been shown that it can be enhanced. In Patent Document 2 (Japanese Patent No. 4702561), a dentifrice composition having an appropriate polishing force and feeling of use by blending heavy calcium carbonate, disintegration strength, inorganic granules having a specific average particle size and a water-soluble polymer substance. Things are disclosed.
Furthermore, in Patent Document 3 (Japanese Patent Application Laid-Open No. 2011-121916), by combining a granule having a particle diameter of 20 to 500 μm and carboxymethyl cellulose having a low etherification degree, the tooth surface has excellent microfouling removal ability. Dentifrice compositions have been proposed.

  On the other hand, it is known to add an aesthetic effect by adding colored granules to a dentifrice composition, and Patent Documents 1 and 3 also describe that granules can contain a colorant. Patent Document 4 (Japanese Patent Publication No. 2002-526393) discloses that colored silica particles are blended in order to give a beautiful appearance to a transparent liquid dentifrice gel. Patent Document 5 (Japanese Patent Laid-Open No. 2010-138132) discloses a technique for suppressing discoloration due to high-temperature storage.

JP-A-1-299211 Japanese Patent No. 4702561 JP 2011-121916 A JP 2002-526393 A JP 2010-138132 A

  However, the conventional dentifrice compositions have room for improvement in terms of cleanability of the gap between the teeth and the stability of the appearance after long-term storage at high temperatures.

  The present invention has been made in view of the above circumstances, and is an opaque dentifrice in which granules are dispersed and blended, with improved cleaning properties, particularly cleaning of gaps between teeth, and excellent anti-discoloration effect of the dentifrice over time. An object is to provide a composition.

  As a result of intensive studies to achieve the above object, the present inventors have determined that the colored granule (A) having an average particle diameter of 150 to 400 μm and 90% by mass or more of particles having a particle diameter of 600 μm or less is 0.00. 5 to 5% by mass and 3 to 60% by mass of the abrasive (B) having an average particle size of 120 μm or less, and shows the blending ratio of the colored granules (A) and the abrasive (B) / The opaque dentifrice composition (A) having a mass ratio of 2 to 70 improves the cleaning property, particularly the cleaning property of the tooth gap (the gap existing between the teeth), and is excellent in the effect of removing colored stains. The present inventors have found that the dentifrice preparation is excellent in the effect of suppressing discoloration over time. Moreover, the favorable usability | use_condition which is harmless for gingiva was obtained.

As described above, when a granule is blended in a dentifrice composition and stored for a long period of time, the dentifrice discolors. In particular, in a dentifrice composition, the white paste turns yellow, but the abrasive (B) is contained. When the colored granules (A) having a specific average particle size and particle size were dispersed and blended with the opaque dentifrice composition, the dentifrice surprisingly showed the effect of suppressing discoloration over time, and was stored for a long time at a high temperature. The discoloration of the dentifrice could be suppressed, and the effect of removing colored stains could be improved. In the present invention, the combination of the colored granules (A) gives a remarkable effect that cannot be predicted from the aesthetic effects of the conventional colored granules. It is something that cannot be achieved with suitable colored granules.
In the present invention, the colored granule (A) is preferably a granulated product colored with a cold-colored organic pigment selected from blue, green, and purple, and the abrasive (B) is calcium carbonate-based or A silica-based abrasive is preferred.

Therefore, the present invention provides an abrasive having an average particle diameter of 200 to 350 μm and 1 to 5 mass% of colored granules (A) having 90% by mass or more of particles having a particle diameter of 400 μm or less and an average particle diameter of 120 μm or less. (B) contains 3 to 40% by mass, and (B) / (A) indicating the blending ratio of the colored granules (A) and the abrasive (B) is 2 to 40 as a mass ratio, The colored granule (A) is a cold-colored system in which the granulated product comprising a water-insoluble material composed of one or more selected from zeolite, silica, calcium carbonate and aluminum oxide is selected from blue, green and purple An opaque dentifrice composition characterized by being a colored granule colored with an organic pigment of

  According to the present invention, it is possible to provide an opaque dentifrice composition in which granules are dispersed and blended, in which the cleaning property, particularly the cleaning property of a tooth gap is improved and the dentifrice has an excellent effect of suppressing discoloration over time. it can.

  The present invention will be described in further detail below. The dentifrice composition of the present invention contains colored granules (A) and an abrasive (B) and has an opaque appearance.

  The colored granules (A) are dispersed and blended in the dentifrice composition to provide an effect of improving the cleaning property and an effect of suppressing the color change of the dentifrice over time. The colored granules (A) are composed of a granulated product and a pigment coloring the granulated product, and a granulated product colored with a pigment is used.

  Here, the granulated product of the colored granules (A) may be any material that can be blended in the dentifrice composition, and an appropriate water-insoluble material can be used. In particular, those containing one or more water-insoluble materials selected from zeolite, silica, calcium carbonate and aluminum oxide are suitable for imparting cleaning properties, more preferably zeolite, silica, carbonic acid. A granulated product which is calcium and particularly contains zeolite and silica as constituent components is preferable.

Furthermore, in addition to the above materials, the granulated product may be added with known components that can be usually blended into the granule, and specific examples include a fragrance component, other excipients, and medicinal components. These optional components can be added as long as the effects of the present invention are not impaired.
In addition, the said granulated material can be prepared by granulating the component of a raw material by a normal method.

  In the colored granule (A), the pigment for coloring the granulated product is preferably a cold-colored pigment, and may be organic or inorganic as long as it can be blended into the dentifrice composition. Of these, organic dyes are preferred.

  As the cold dye, those having an absorption maximum in the range of 560 to 730 nm when dissolved in a solvent, particularly chloroform, 1-chloronaphthalene or ethanol, and measuring the visible absorption spectrum in the range of 400 to 800 nm are preferable. Can be used. Examples of the cold-colored dye having an absorption maximum in this range include a cold-colored organic dye selected from blue, green, and purple, and blue-based organic dyes are particularly preferable.

Specific examples of such a cold color pigment include blue 201, blue 204, green 202, purple 201 and the like. Of these, blue 201 and blue 204 are preferable. The above pigments may be used alone or in combination of two or more in terms of effect expression.
Further, as the pigment, yellow and red pigments may be added in addition to the cold pigment as long as the colored granules (A) exhibit a cold color appearance.

The colored granule (A) is preferably a colored granule colored with a cold color pigment. In this case, if the color granule (A) is colored in a cold color having an absorption maximum in the above range with the cold color pigment, The aspect can be adjusted as appropriate. The color of the colored granules (A) is, for example, blue, green, grass color, light green, dark green, blue green, light blue, light blue green, light blue, purple, light blue purple, etc., among which blue, green, especially blue It is preferable from the point of discoloration suppression and cleaning property provision.
In addition, in the non-colored granule, for example, the granule showing a white appearance without color, the discoloration suppressing effect is not recognized even when used in combination with the abrasive (B), and the object of the present invention is not achieved.

  The amount of the pigment used is preferably 0.01 to 0.2% (mass%, the same shall apply hereinafter), more preferably 0.02 to 0.1%, based on the entire granulated product of the colored granules (A). It is. It is effective for discoloration suppression to be 0.01% or more. 0.2% or less is preferable to give a good appearance of the preparation.

  The average particle diameter (d50) of the colored granules (A) is 150 to 400 μm, preferably 200 to 350 μm. When the average particle size is less than 150 μm, the cleaning property of the tooth gap is poor. If it exceeds 400 μm, discoloration of the dentifrice cannot be suppressed.

  The colored granule (A) has a particle size (d90) of 90% or more of particles of 600 μm or less, preferably 400 μm or less. If the particle size is larger than 600 μm, discoloration of the dentifrice cannot be suppressed.

The average particle diameter (d50) and the particle diameter (d90) of 90% or more of the particles are values obtained by the granule particle size distribution measurement method described below.
Granule Size Distribution Measurement Method Granule size distribution was measured with Nikkiso Co., Ltd. Microtrac Series MT3300, and water was used as a dispersion solvent for the granules. When the cumulative curve was determined with the total volume of the granule population as 100%, the particle diameter (μm) at the point where the cumulative curve was 50% and 90% was the average particle diameter (d50), and 90% or more of the particles The particle diameter (d90) was used.

The colored granules (A) are preferably disintegrating granules, and the average disintegration strength is preferably 10 to 100 g / piece, more preferably 15 to 50 g / piece. The higher the average disintegration strength is, the higher the cleaning property is.
The average disintegration strength of the granules is determined by measuring automatically breaking strength for each of 30 granules by using a rheometer (Sun Rheometer CR-200D manufactured by Sun Science Co., Ltd.). It is the average value of the values measured for the load when the granules disintegrate.

  The compounding quantity of a granule (A) is 0.5 to 5% of the whole composition, Preferably it is 1 to 5%, More preferably, it is 1 to 3%. If it is less than 0.5%, it is inferior to the cleaning property of the tooth gap and the discoloration suppressing effect of the dentifrice. If it exceeds 5%, the appearance deteriorates.

The abrasive (B) has an average particle size of 120 μm or less, preferably 50 μm or less, more preferably 3 to 20 μm. The average particle diameter is a value measured by the microtrack method in the same manner as described above.
Examples of the abrasive (B) include calcium carbonate abrasives such as light calcium carbonate and heavy calcium carbonate, silica abrasives such as silica gel, precipitated silica and zirconosilicate, dibasic calcium phosphate dihydrate, Phosphoric acid type abrasives such as calcium diphosphate anhydrate, calcium pyrophosphate, aluminum hydroxide, polymethyl methacrylate, insoluble calcium metaphosphate, magnesium carbonate, tertiary magnesium phosphate, zirconium silicate, hydroxyapatite, synthetic resin abrasive, etc. Among them, calcium carbonate-based abrasives, silica-based abrasives, especially calcium carbonate-based abrasives are preferable because they can provide cleaning properties and discoloration-suppressing effects without harm to the gums.

  The compounding quantity of an abrasive | polishing agent (B) is 3 to 60% of the whole composition, Preferably it is 3 to 40%, More preferably, it is 10 to 40%. If it is less than 3%, the cleaning property of the tooth gap is inferior. When it exceeds 60%, the balance as a preparation is deteriorated.

  In this invention, (B) / (A) which shows the mixture ratio of a coloring granule (A) and an abrasive | polishing agent (B) is 2-70 as mass ratio, Preferably it is 2-40, More preferably, it is 4 ~ 40. When the ratio of (B) / (A) is within the above range, it is excellent in the cleanability of the tooth gap and the discoloration-suppressing effect of the dentifrice. When it exceeds, it is inferior to the discoloration inhibitory effect of a dentifrice. Moreover, the cleaning property of the teeth is lowered.

  The dentifrice composition of the present invention has an opaque appearance. Here, “opaque” is determined to be opaque by the following evaluation method.

Evaluation method of opaque appearance The evaluation method of opaque appearance is to draw two 2mm-thick black vinyl tapes with a thickness of 30mm on the back of a transparent glass plate with a light transmittance of 100%. A sample dentifrice was placed on the surface, an acrylic plate having a thickness of 1 mm was placed on both ends, and pressed from above with another glass plate to form a film. When the black line was not visible when visually observed from 30 cm above, it was determined to be opaque.

  The dentifrice composition of the present invention can be suitably prepared as a paste-form or gel-form preparation having an opaque appearance, for example, a toothpaste, a liquid dentifrice, and in particular, a toothpaste, and its production method is in a dosage form. The corresponding ordinary method can be adopted. In this case, appropriate known components other than the colored granules (A) and the abrasive (B) can be blended according to the purpose of the composition, dosage form, and the like. For example, in the case of a toothpaste, a thickening agent such as thickening silica, sodium carboxymethylcellulose, a sugar alcohol such as sorbit, a polyhydric alcohol such as propylene glycol, a surfactant such as sodium lauryl sulfate, If necessary, sweeteners such as preservatives and sodium saccharin, active ingredients such as coloring agents, fragrances and fluorides can be blended, and these components and water can be mixed to produce. These optional components may be blended in a normal amount if necessary, but the binder is preferably 3 to 15%, the thickener is 10 to 40%, and the surfactant is preferably 0.1 to 3%. .

  In addition, the dentifrice composition of the present invention may further contain a water-insoluble powder other than these in addition to the colored granules (A) and the abrasive (B), for example, thickening as a binder. 3-15% of silica can be blended, but it does not need to contain water-insoluble powder other than colored granules (A) and abrasives (B), or colored granules (A), abrasives (B) and thickening silica. . Further, uncolored granules, particularly uncolored granules having the same average particle diameter (d50) and particle diameter (d90) as the colored granules (A) may not be blended.

  In the dentifrice composition of the present invention, the dentifrice base color is, for example, white, pale yellow to yellow, pale blue to blue, pale green to green, pale red to red, pale orange to orange, pale pink to pink. However, the dispersion of the colored granules (A) can be visually recognized, and the dispersion of the abrasive (B) is difficult to visually recognize, particularly the color of the dentifrice base and the abrasive (B). The colors are preferably the same, and the dentifrice base color is more preferably white.

  In the present invention, in particular, a white toothpaste base, 1 to 3% of colored granules (A) having an average particle size of 200 to 350 μm and 90% or more of particles having a particle size of 400 μm or less, a calcium carbonate type A toothpaste composition in which 10 to 40% of the abrasive (B) is dispersed and blended in such a range that (B) / (A) is 4 to 40 as the mass ratio, and the colored granules (A) Is a granulated product colored with a blue, green or purple organic pigment, and is a disintegrating granule having an average disintegration strength of 15 to 50 g / piece, and a calcium carbonate-based abrasive (B) Is an average particle diameter of 3 to 20 μm, which is excellent for cleaning the gaps in the teeth and suppressing discoloration of the dentifrice, and is particularly desirable for providing the effects of the present invention.

EXAMPLES Hereinafter, although an Example and a comparative example are shown and this invention is demonstrated concretely, this invention is not restrict | limited to the following Example. In the following examples, “%” means “% by mass” unless otherwise specified.
The average particle size (d50) of the granules and the particle size (d90) of 90% or more of the particles are values obtained by the same particle size distribution measurement method as described above, and the average disintegration strength is the same as that described above. It is a value measured by a method using a meter. The average particle size of the abrasive is also a value measured in the same manner as described above.

[Examples and Comparative Examples]
Colored granules (A) shown in Table 1 were prepared by coloring the granules prepared by the following method.
Using the colored granules (A), abrasives (B-1) and (B-2), toothpastes having the compositions shown in Tables 2 and 3 were prepared by conventional methods and evaluated by the following methods. The results are shown in Tables 2 and 3.
The obtained dentifrice base color was white, and the dentifrices in each example in the table were evaluated in the same manner by the evaluation method for opaque appearance described above, and all had an opaque appearance.
The average particle diameter (d50) and particle diameter (d90) of the used colored granules (A) are as shown in Tables 2 and 3. The details of the raw materials used other than the colored granules (A) are as follows, and the other raw materials used were those conforming to the Quasi-drug raw material standard 2006.

Preparation of colored granules (A):
Using the raw materials shown in Table 1, colored granules (A) were prepared by the production method (sintering method) shown below.
Each raw material shown in Table 1 was mixed in the granulation vessel, granulated and dried for 30 minutes, and baked at 100 ° C. for 20 minutes. Thereafter, the particle size was appropriately adjusted using a sieve to produce colored granules (A).

  When the absorption spectrum in the range of 400 to 800 nm was measured for the obtained colored granules (A) using the following solvent, the absorption maximum wavelength was a value shown in Table 1. The average disintegration strength of the colored granules (A) was in the range of 10 to 100 g / piece.

＊１：ゼオライト（コスモ社製）
＊２：無水ケイ酸（ローディア社製 ＴＩＸＯＳＩＬ４３）
＊３：青色２０１号（癸巳化成社製）
＊４：緑色２０２号（癸巳化成社製）

* 1: Zeolite (Cosmo)
* 2: Silica anhydride (TIXOSIL43, Rhodia)
* 3: Blue No. 201 (Made by Kasei Kasei)
* 4: Green No. 202 (Made by Kasei Kasei)

Details of raw materials used Abrasive (B-1);
Calcium carbonate abrasive, product name Heavy calcium carbonate, Calfine,
Average particle size: 5.0 μm
Abrasive (B-2);
Silica-based abrasive, trade name NIPGEL AY-002, manufactured by Tosoh Silica Corporation,
Average particle size: 90 μm
White granules (comparative product);
Uncolored granules (prepared product) consisting of 90% zeolite and 10% silicic anhydride
Average particle diameter (d50): 290 μm, particle diameter (d90): 400 μm
Average disintegration strength is in the range of 10-100 g / piece

Evaluation method-1: Cleanability of tooth-to-tooth gap A white seal is applied to a portion other than the gap on the surface of an untreated hydroxyapatite pellet having a gap of 1 mm in width and 1 mm in depth, and the color of the gap is a reference color Was measured with a color difference meter, and the value was defined as L0. This pellet (in a state where the seal was peeled off and not stuck) was immersed in saliva at 37 ° C. for 30 minutes, and then washed with ion-exchanged water to remove surface moisture. The following three types of immersion liquids are prepared with a remineralization liquid in which 0.74 mM calcium ion, 2.59 mM phosphate ion, and 50 mM NaCl are mixed, and 0.5% albumin relime is added to the previous pellet. After repetitively soaking for 1 hour in a recalcification solution → 3% Japanese tea + 1% coffee + 1% black tea remineralization solution → 0.6% ammonium iron citrate re-mineralization solution after air drying at room temperature for 1 day Then, it was washed with running water and air-dried again, and a white seal was applied to a portion other than the gap on the surface of the colored pellet, the color of the gap was measured, and the value was L1. The surface of this colored pellet (in a state where the seal was peeled off and not stuck) was brushed 1,500 times with a toothbrush on which 1 g of the prepared dentifrice was placed, and then lightly washed with running water and dried. Again, a white seal was applied to a portion other than the gap on the surface of the pellet, the color of the gap was measured, and the value was L2.
The colored stain removal rate was calculated by the following formula, and the average value of 10 times was evaluated according to the following evaluation criteria, and the cleanability of the tooth-to-tooth gap was judged from this evaluation result.
Colored stain removal rate (%) = [(L1-L2) / (L1-L0)] × 100
Evaluation criteria ◎: Average value 70% or more ○: Average value 60% or more and less than 70% △: Average value 50% or more and less than 60% ×: Average value less than 50%

Evaluation method-2: Discoloration of dentifrice Evaluation was carried out on 20 general panelists. The prepared dentifrice was stored in a tube container and stored at 60 ° C. for 1 month, and then placed on a toothbrush, and the discoloration of the paste was determined based on the following criteria. The product immediately after production in Comparative Example 4 was used as a control, and the discoloration of the paste over time due to storage was evaluated.
Judgment criteria 5: No discoloration 4: Little discoloration 3: Neither discoloration 2: Discoloration 1: Very discoloration The average score of the points evaluated based on the above criteria is calculated and evaluated according to the following criteria Evaluation criteria A: Average point is 4.0 points or higher. ○: Average point is 3.0 points or higher and lower than 4.0 points. Δ: Average point is 2.0 points or higher and lower than 3.0 points. Less than 0

Claims (8)

1 to 5% by mass of colored granules (A) having an average particle size of 200 to 350 μm and 90% by mass or more of particles having a particle size of 400 μm or less, and 3 to 3% of an abrasive (B) having an average particle size of 120 μm or less. 40 mass%, (B) / (A) which shows the compounding ratio of a colored granule (A) and an abrasive | polishing agent (B) is 2-40 as mass ratio, The said colored granule (A) However, a granulated product composed of one or more water-insoluble materials selected from zeolite, silica, calcium carbonate and aluminum oxide is colored with a cold organic dye selected from blue, green and purple. An opaque dentifrice composition characterized by being colored granules. Colored granules (A) is a blue-based granulation of the does not dissolve in water, greenish and claim 1 dentifrice composition according those colored with organic dyes cold colors selected from purplish. The dentifrice according to claim 1 or 2, wherein the cold-colored organic pigment selected from blue, green and purple is at least one selected from blue 201, blue 204, green 202 and purple 201. Composition. The colored granule (A) is a granulated product composed of one or more water-insoluble materials selected from zeolite and silica and colored with a cold- colored organic dye selected from blue, green and purple The dentifrice composition according to any one of claims 1 to 3 . The dentifrice composition according to any one of claims 1 to 4 , wherein the colored granules (A) are disintegrating granules and have an average disintegration strength of 10 to 100 g / piece. The dentifrice composition according to any one of claims 1 to 5 , wherein the abrasive (B) is a calcium carbonate-based or silica-based abrasive. The dentifrice composition according to any one of claims 1 to 6 , wherein the dentifrice base has a white color, and the colored granules (A) and the abrasive (B) are dispersed in the dentifrice base. The dentifrice composition according to any one of claims 1 to 7 , which is a toothpaste.