JPH0558404B2 - - Google Patents

Description

[Detailed description of the invention]

FIELD OF THE INVENTION The present invention relates to a granular dentifrice composition that changes in flavor, and more particularly to a granular dentifrice composition that allows a user to recognize the appropriate usage time based on the change in flavor. Prior Art Although toothpaste compositions originally have sufficient oral cleaning and disease prevention functions,
Improper use, especially insufficient usage time, often results in the product not achieving its full potential. In order to avoid such insufficient use of dentifrice compositions, dentifrice compositions have already been proposed that inform the user of the appropriate usage time by changing their color or changing the amount of foam. However, among such dentifrice compositions, it is difficult to find one that is satisfactory in terms of the degree of change in color tone and amount of foam, the time required for change, the safety of the pigments used, etc. Furthermore, if the color change is due to a change in the amount of foam, it may be necessary to stop using the product and repeat the check to determine if the usage time is sufficient.
There is a drawback that defoaming reduces the desire to use the product. The present inventors have conducted extensive studies in order to obtain a dentifrice composition that eliminates these drawbacks and can clearly indicate the appropriate usage time to the user. As a result, the desired dentifrice composition can be obtained by granulating cyclodextrin containing a flavoring agent and combining the granules obtained by coating the cyclodextrin with a certain kind of coating substance with a granular dentifrice base. They discovered this and completed the present invention. DISCLOSURE OF THE INVENTION The present invention provides a granular dentifrice composition with variable flavor, which is prepared by mixing flavor-inclusive cyclodextrin granules coated with a coating material consisting of shellac, glycerin fatty acid ester, and an excipient, and a granular dentifrice base. This is what we provide. In the dentifrice composition of the present invention, during use, after a certain period of time, for example, after at least 60 seconds, the flavor is released from the flavor-enclosing cyclodextrin granules, and the flavor changes.
As a result, the appropriate usage time will be displayed,
There is no need to interrupt use and repeat confirmation, and
There are no disadvantages such as a decrease in the desire to use the product due to de-wrapping. The fragrance-included cyclodextrin granules in the dentifrice composition of the present invention are obtained by granulating cyclodextrin containing a fragrance and coating the granules with the coating material. The fragrance is not particularly limited and may be any fragrance suitable for the purpose of the present invention, such as cinnamon oil, clove oil, caraway oil, peppermint oil, spearmint oil,
Coriander oil, rosemary oil, eucalyptus oil, cardamom oil, anise oil,
Natural essential oils such as orange oil, lemon oil, cedarwood oil, geranium oil, lime oil, mace oil, bergamot oil, diasmine oil, lavender oil, wine wreath oil, sage oil, thyme oil, laurel oil, menthol, Benzyl alcohol, ethyl alcohol, cineole, phenylpropyl alcohol, butyl alcohol, isopropyl alcohol, borneol, phenethyl alcohol, linalool, propylene glycol, geraniol, α-terpineol, phenethyl alcohol, hexanol, octyl alcohol,
Alcohols such as propyl alcohol, aldehydes such as cinnamic aldehyde, benzaldehyde, butanal, anisaldehyde, octanal, decanal, 2-methylundecanal, trans-2-hexenal, and citral, thymol, isoeugenol, vanillin, bourbonal, etc. Phenols, diasmine, diethyl ketone, menthone, ethyl amyl ketone, camphor, butanone, ethyl maltol, carvone,
Ketones such as methyl nonyl ketone, α-, β-, γ-ionone, nootkatone, methyl dihydrodiasmonate, maltol, furaneol, methyl propyl ketone, methyl n-amyl ketone, methyl heptyl ketone, methyl octyl ketone, ethyl capro ate, methyl butyrate, ethyl caprylate, cinnamyl acetate, allyl caproate, isoamyl caproate, ethyl lactate, benzyl benzoate, methyl cinnamate, ethyl phenyl acetate, benzyl salicylate, methyl N-methyl anthranilate, Menthyl acetate, methyl salicylate, butyl acetate, ethyl propionate,
Ethyl acetate, ethyl acetoacetate, menthyl formate, linalyl caproate, methyl acetate, isoamyl acetate, ethyl isobutyrate, ethyl butyrate, geranyl propionate, cinnamyl propionate, benzyl butyrate, isoamyl butyrate, Esters such as benzyl isobutyrate, isoamyl isovalerate, geranyl isovalerate, ethyl levulinate, methyl β-methylthiopropionate, ethyl benzoate, other menthofuran, linalool oxide, γ-decalactone,
Included are limonene, anethole, citral diethylacetal, rose oxide, 1,8-cyonele, 2-methylpyrazine, γ-heptylbutyrolactone, γ-amylbutyrolactone, allyl hexanoate, ethyl methylphenylglycidate, and the like. The cyclodextrin used for inclusion of these fragrances is usually β-cyclodextrin, but
α- or γ-cyclodextrins can also be used. Inclusion of a fragrance with a cyclodextrin can be carried out according to a known method. For example, water may be added to a mixture of a cyclodextrin and a fragrance, shaken for a day and night, and then the solid matter may be filtered and dried.
Although the ratio of cyclodextrin and perfume can be selected as appropriate, it is usually appropriate to use about 5 to 30 parts by weight of perfume per 100 parts by weight of β-cyclodextrin. Cyclodextrin containing a fragrance is a powder, and in the present invention, it is prepared using a binder or a binder and an excipient by a conventional method to a particle size (average particle size of about 0.1 mm or more) that can be coated with a coating material. Granulate into granules. The binders and excipients used may be conventional ones. For example, the binders include hydroxyethylcellulose, hydroxypropylmethylcellulose, methylcellulose, ethylcellulose, sodium carboxymethylcellulose, polyvinylpyrrolidone, polyvinyl alcohol, polyvinyl acetate, polyethylene glycol,
Examples include starches, dextrin, gum arabic, gum tragacanth, guar gum, carrageenan, sodium alginate, gelatin, and gluten. Examples of excipients include saccharides such as sorbitate and lactose, starches such as corn starch and potato starch, calcium sulfate, silicic anhydride, and calcium phosphate. These binders and excipients may be used alone or in combination of two or more, and the amount used is not particularly limited.
Usually, per 100 parts by weight of fragrance clathrate dextrin,
The total amount is about 10 to 500 parts by weight. The coating materials used for coating are basically:
It is a mixture of shellac, glycerin fatty acid ester and excipients. The shellac may be any refined shellac or white shellac. Examples of glycerin fatty acid esters include glyceryl monostearate, glyceryl monooleate, glyceryl distearate, glyceryl dioleate, and mixtures thereof. Further, as excipients, there may be mentioned the same excipients as those exemplified in the above-mentioned granulation of cyclodextrin clathrated with fragrance, and they may be used alone or in combination of two or more kinds. In order to make the user aware of the appropriate usage time, for example, 60 seconds or more, the weight ratio of shellac:glycerin fatty acid ester:excipient in the coating material is preferably 10:0.1 to 4.0:10 to 30. shall be. If the ratio of glycerin fatty acid ester to shellac is too high, the release of the clathrate flavoring agent will be too rapid during tooth brushing, while if it is low, it will cause caking of the granules and will also result in solid granules that cannot be disintegrated by normal brushing. Therefore, the above ratio is preferable. Furthermore, when the ratio of excipient to shellac exceeds the above range, the coating with the coating material becomes very brittle and immediately disintegrates when brushed during tooth brushing, resulting in granules that release the clathrate fragrance; The above proportions are preferred since the release of the flavoring agent from the base is very slow and the change in flavor becomes unclear, making it unsuitable for the purposes of the present invention. If desired, the coating material may contain suitable amounts of other additives, such as colorants. The coating of the cyclodextrin granules containing a fragrance can be carried out according to a conventional method, for example, while spraying an ethanol solution of shellac and glycerin fatty acid ester at an appropriate concentration onto the granules at 30 to 40°C, at the same time. Coating is carried out by adding an appropriate amount of excipient, and after completion of spraying, drying at 50°C yields the desired coated granules. The thickness of the coating material to be applied also influences the release of the clathrate fragrance, i.e. the recognition of the appropriate usage time, and the proportion of the coating material based on the total amount of coated granules obtained is 10-40% by weight. It is preferable to make it thick. If the thickness of the coating material is too thin, it will not be uniformly coated, the thin areas will break down quickly, and the clathrate will be released too quickly.
On the other hand, if it is too thick, the release of the clathrate perfume will not occur in a given time. The average particle size of the coated perfume cyclodextrin granules is preferably 0.7 mm or less, and if it exceeds 0.7 mm, a foreign body sensation is likely to occur in the oral cavity. The dentifrice composition of the present invention is obtained by mixing the thus obtained coated granules with a granular dentifrice base. The granular dentifrice base is made by granulating the ingredients used in ordinary dentifrice compositions by a conventional method using the binders and excipients described above, for example, with an average particle size of 0.3.
~1.0mm granules. These ingredients include:
Calcium carbonate, dicalcium phosphate (dihydrate, anhydride), silicic anhydride, aluminum hydroxide,
Abrasives such as alumina, calcium pyrophosphate, aluminum silicate, insoluble sodium metaphosphate, magnesium phosphate, magnesium carbonate and mixtures thereof, sodium lauryl sulfate,
Examples include foaming agents such as sodium lauroyl sarcosinate, sucrose fatty acid esters, and mixtures thereof, sweeteners such as saccharin, stevioside, glycyrrhizin, and aspartame, other fungicides, preservatives, fragrances, colorants, and various medicinal ingredients. Further, in order to flavor and odor the base itself, a flavoring agent having a different flavor from the flavoring agent included in the cyclodextrin is also used. The blending amounts of these components can be appropriately selected according to ordinary dentifrice compositions. The mixing ratio of the coated flavor inclusion cyclodextrin granules and the granular toothpaste base is not particularly limited, and can be arbitrarily mixed at a ratio such that the concentration of the inclusion flavor released in the oral cavity is equal to or higher than a threshold value. Usually, the weight ratio of granular toothpaste base to coated encapsulated flavoring granules is preferably 10:0.5 to 3. EXAMPLES Next, the present invention will be explained in more detail with reference to reference examples and examples. In addition, "department" means
All terms refer to parts by weight. Reference Example 1 A fragrance was prepared according to the following recipe. Ingredients Weight % Menthol 40 Peppermint oil 40 Carvone 5 Anethole 7 Orange oil 3 Lemon oil 2 Clove oil 1 Benzyl alcohol 0.1 Ethyl amyl ketone 0.9 Ethyl butyrate 0.1 Linalyl caproate 0.9 Obtained fragrance 2.34 parts and β-cyclodextrin 23.40 parts 150 parts by volume of water was added to the mixture, and the mixture was shaken overnight. Then, the mixture was suction-filtered, and the filtered solid was dried with air at 45° C. for 24 hours to obtain fragrance inclusion cyclodextrin powder. This powder was mixed with 49.41 parts of corn starch and 1.60 parts of hydroxypropyl cellulose (5%
(Used as an aqueous solution) and then granulated with 30 to 40
Coated flavor-included cyclodextrin granules (coating) coated with 7.5 parts of shellac, 0.75 parts of glyceryl monostearate (used as a solution in 50 parts by volume of ethanol) and 15 parts of corn starch and having an average particle size of 0.30 to 0.59 mm at Substance content 23.25%,
Ceramics: Glycerin fatty acid ester: Excipient =
10:1:20). Reference Example 2 A fragrance was prepared according to the following recipe. Ingredients Weight% Menthol 30 Peppermint oil 10 Carvone 10 Spearmint oil 30 Anethole 10 Lime oil 3 Lemon oil 3 Mace oil 1 Bergamot oil 2 Isoamyl valerate 0.5 Isoamyl acetate 0.5 2.5 parts of the fragrance obtained in the same manner as Reference Example 1, β-
Cyclodextrin 25 parts, corn starch 54.5 parts
part and hydroxypropyl methylcellulose 2
cyclodextrin granules containing fragrance were obtained. The granules were coated with 5 parts of shellac, 1 part of glyceryl distearate and 10 parts of calcium carbonate to form coated perfume-inclusion cyclodextrin granules with an average particle size of 0.30 to 0.59 mm (coating substance content 16
%, shellac: glycerin fatty acid ester: excipient = 10:2:20). Reference example 3 According to the following recipe, the average particle size is 0.30 using the usual method.
A granular toothpaste base of ~0.59 mm was prepared. Ingredients Weight % Dicalcium phosphate 70.06 Sodium lauryl sulfate 2.00 D-sorbit 14.00 Corn starch 11.00 Hydroxypropyl cellulose 0.50 Sodium saccharin 0.20 Bactericides and preservatives 0.10 Flavor 1.30 Sodium monofluorophosphate 0.84 The composition of the flavor is as follows. Ingredients Weight% Menthol 35.0 Peppermint oil 50.0 Carvone 1.0 Anethole 5.0 Cinnamon oil 3.0 Coriander oil 3.0 Diasmone 0.5 Menthyl acetate 0.5 Methyl saliciate 1.0 Thymol 1.0 Reference example 4 Similar to Reference example 3, granules with an average particle size of 0.59 to 0.84 mm A toothpaste base was prepared. Reference example 5 According to the following recipe, the average particle size is 0.30 using the usual method.
A granular toothpaste base of ~0.59 mm was prepared. Ingredients Weight % Calcium carbonate 81.10 Sodium N-lauroylsarcosine 0.50 Sodium myristyl sulfate 1.30 Lactose 15.00 Hydroxypropyl methylcellulose 0.40 Sodium saccharin 0.20 Bactericide and preservative 0.10 Flavor 1.40 The composition of the flavor is as follows. Ingredients Weight% Menthol 25.0 Peppermint oil 10.0 Carvone 10.0 Spearmint oil 40.0 Anethole 10.0 Eucalyptus oil 1.0 Clove oil 1.0 Cedarwood oil 1.0 Ethyl alcohol 1.0 Camphor 0.2 Ethyl acetate 0.8 Examples 1 to 6 Coated packages obtained in Reference Examples 1 and 2 The flavoring granules and the granular dentifrice bases obtained in Reference Examples 3 to 5 were mixed in the proportions (weight ratio) shown in Table 1 below to obtain a desired granular dentifrice composition. Table 1 also shows the results of evaluating the resulting dentifrice compositions regarding the average time (seconds) required for a change in flavor to be recognized in the oral cavity and the presence or absence of foreign body sensation.

[Table] As described above, the dentifrice composition of the present invention is
During use, it is possible to indicate the appropriate use time by a clear change in flavor, there is no need to interrupt use and repeat confirmation, and there is no drawback such as a decrease in the desire to use due to defoaming.

Claims (1)

[Scope of Claims] 1. Flavor-changing granules characterized by mixing flavor-included cyclodextrin granules coated with a coating substance consisting of shellac, glycerin fatty acid ester, and excipients with a granular toothpaste base. shaped dentifrice composition. 2. The dentifrice composition according to item 1 above, wherein the weight ratio of shellac: glycerin fatty acid ester: excipient is 10:0.1 to 4.0:10 to 30. 3. The dentifrice composition according to item 1 above, wherein the proportion of the coating material in the coated flavor-inclusion cyclodextrin granules is 10 to 40% by weight. 4. The dentifrice composition according to item 1 above, wherein the average particle size of the coated cyclodextrin granules containing flavor is 0.7 mm or less.