JP3331092B2 - Toothpaste composition - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a dentifrice composition containing a capsule which can be easily broken by brushing, has a good feeling in use, and has a good product appearance.

[0002]

2. Description of the Related Art Conventionally, there have been known a large number of dentifrice compositions in which capsules containing useful ingredients such as various medicinal ingredients, flavors, and pigments are incorporated. In such a dentifrice composition, gelatin, a wax-like substance, agar using agar, etc. are used as a film-forming substance of the capsule.
Gelatin is mainly used.

[0003] Examples of those using gelatin as a film-forming substance include dentifrices in which a flavoring material is encapsulated (Japanese Patent Laid-Open No. 49-453) and toothpastes encapsulated in gelatin capsules (Japanese Patent Laid-Open No. 61-453). No. 100516), a double-capsule containing a water-soluble drug as a core, coated with a lipophilic substance (wax-like substance), and further coated with a hydrophilic substance (gelatin), and an oral composition containing the same. Japanese Unexamined Patent Publication (Kokai) No. 61-225115) and oral mucosa-adhering type bad breath inhibitor in which a bad breath preventing component is mixed with a water-soluble film such as gelatin (Japanese Patent Publication No. 5-41602).

[0004] Further, as a material using a wax-like substance as a film-forming substance, a toothpaste coated with a granulating foaming agent or defoaming agent (synthetic resin or paraffin or the like) (Japanese Patent Publication No. 58-20928). ), A double coat in which a water-soluble medicinal agent solid powder is first coated with a core-forming thermoplastic resin or a high-melting-point wax-like substance, and then coated with a high-melting-point wax-like substance having a lower melting point than the first coat layer. Toothpaste containing fine-grained capsules (Japanese Patent Publication No. 50-25011), a perfume inclusion cyclodextrin granule coated with a coating material comprising shellac, a glycerin fatty acid ester and an excipient, and a granular dentifrice base mixed. Granular dentifrice composition with changing flavor (Japanese Patent Publication No. 5-5840)
No. 4), a microcapsule containing a hydrophobic medicinal component and a chain saturated hydrocarbon represented by C _n H _{2n + 2} in a weight ratio of hydrophobic medicinal component / the chain saturated hydrocarbon ≦ 2. 1
A dentifrice composition containing at least one or more kinds (JP-A-1-275520) can be mentioned.

[0005] Further, as a document showing the possibility that agar can be used as a film-forming substance, there is disclosed a microcapsule containing a silicone oil as a core substance. Dentifrice composition that expresses
No. 9), an opaque microcapsule formed by depositing an insoluble salt as if covering the capsule membrane in a state where it is at least partially buried in the capsule membrane (Japanese Patent Publication No. 63-4858).
No. 0), an edible composition in which the core is a flavor in particulate form and the matrix encapsulating it contains an outer coating of a hydrophilic polymer containing an intense sweetener to enhance flavor and sweetness. Automatic flow granular delivery system for applying (Japanese Patent Laid-Open No. Hei 4-22255)
No. 8).

[0006] As a capsule to be incorporated into a dentifrice composition, it is required that the capsule film be broken during use and the contents released. However, in the case of capsules using gelatin as the above-mentioned film-forming substance, the film is easily broken at the time of use, but on the other hand, there is a problem that the film is easily broken at the time of manufacture and the contents leak. On the other hand, when a wax-like substance is used as the film-forming substance, it can sufficiently withstand external force at the time of manufacturing, but on the other hand, there is a problem that the film of the capsule is hardly broken by brushing with a toothbrush.

[0007] When agar is used as a film-forming substance, problems such as those when gelatin and wax-like substances are used can be improved. However, for example, as described in
The microcapsules in JP-A-5-100309 have an average particle size of 5 to 50 μm, and the opaque microcapsules in JP-B-63-48580 have an average particle size of 5 to 100 μm.
When the particle size of the capsule is small as described above, there is a problem that the capsule is easy to escape from the bristle tip of the toothbrush during brushing, so that the capsule is not easily broken. In this case, there is also a problem that the feeling of use is reduced due to the capsules remaining without being destroyed. On the other hand, if the size of the capsule is too large, the feeling of discomfort / foreign matter at the time of use is increased, and the feeling of use is reduced.

[0008]

As described above, capsules to be mixed with the dentifrice composition have a problem of not only easiness of destruction at the time of use but also the particle size. Therefore, the present invention solves the above problems, is excellent in easiness of destruction at the time of use, can be recognized in the oral cavity, and has an appropriate particle size without giving a feeling of strangeness or foreign matter It is intended to provide a dentifrice composition containing

[0009]

Means for Solving the Problems The present inventors have conducted intensive studies to achieve the above object, and as a result, produced a capsule using agar as a main component of a film-forming substance and blended it into a dentifrice composition. The present invention has been completed by finding an appropriate particle size range in such a case.

The present invention comprises agar having a jelly strength of 500 g / cm ² or more as a main component of the film-forming substance, wherein the agar has a coating rate of 1 to 30% by weight and an average particle size of 0.1 to 30% by weight.
It is intended to provide a dentifrice composition characterized by containing a capsule having a size of 3 to 3 mm and a breaking strength of 0.1 to 20 g / piece.

Hereinafter, the present invention will be described. In the present invention, a "capsule" is a product in which contents such as a medicinal ingredient, a pigment and a flavoring agent are covered with a film.

Agar is used as the main component of the film-forming substance of the capsule. The agar is preferably one having a high solubility in water, particularly one having a solubility in water at 95 ° C. under normal pressure of 3 or more, particularly 5 or more. These are preferred because the operation of forming the coating is easy.

The agar has a jelly strength of 5
It is not less than 00 g / cm ² and does not break capsules during the production of the dentifrice composition. The jelly strength was measured by applying a load to the 1.5% agar gel from above,
Are those represented by the load amount when the withstand 20 seconds per ^2, generally in the case of yarn agar is used as a food 400 g / cm ² or so, in the case of angular agar 280 g / cm
^{About 2} .

In the present invention, a hydrophilic polymer substance or a lipophilic polymer substance can be blended together with agar for the purpose of improving the usability. Examples of the hydrophilic polymer include gelatin, sodium alginate, carrageenan, carboxymethylcellulose, methylcellulose,
Hydroxyethylcellulose, hydroxypropylcellulose, hydroxypropylmethylcellulose, gum arabic, guar gum, xanthan gum, casein, pectin, albumin, polyvinyl alcohol, and the like, and as the lipophilic polymer, polyethylene,
Wax-like polymers such as polypropylene, polystyrene, polyvinyl chloride, polyacrylic acid, polymethacrylic acid, cetyl alcohol, stearyl alcohol, ethylene glycol distearate, sorbitan tristearate, ceresin, paraffin wax, polyolefin wax, beeswax and carnauba wax Substances can be mentioned. These can be used alone or in appropriate combination of two or more kinds.

When a hydrophilic polymer or a lipophilic polymer is added to the agar as a film-forming substance, the hydrophilic polymer or the lipophilic polymer is added in an amount of 1 to 100% by weight of the agar. %, Especially 1 to
The addition of 20% by weight is preferable since the feeling of use can be improved without impairing the stability of the contents and the release property in the oral cavity.

The content of the capsule is not particularly limited as long as it is a medicinal component, a flavoring agent, a coloring agent, etc., which are usually used in an oral composition such as a dentifrice. Among them, those which are lipophilic are preferred. The content can be in a desired form such as a liquid, a powder, or a gel, depending on the form of the dentifrice composition, the production method, and the like.

Examples of the medicinal component include a caries preventive agent, an antimicrobial agent, a vitamin, an enzyme and an anti-inflammatory agent.
More specifically, sodium fluoride, tin fluoride, sodium monofluorophosphate, vitamin E, vitamin C, dextranase, mutanase, sodium chloride, glycyrrhizinate, glycyrrhetinic acid, azulene, dihydrocholesterol, chlorhexidine, epichloride Dihydrocholesterol, isopropylmethylphenol, trichlorocarbanilide, triclosan, halocarban, hinokitiol, allantoin, tranexamic acid, propolis, cetylpyridinium chloride, benzethonium chloride, benzalkonium chloride, sodium copper chlorophyllin, lysozyme chloride, etc. . Flavoring agents include flavoring aldehydes, esters, alcohols, etc., and more specifically, spearmint oil, peppermint oil, clove oil, sage oil, eucalyptus oil, laurel oil, cinnamon oil, cinnamon oil , Lemon lime oil, grapefruit oil, menthol, carvone, methyl salicylate, ethyl salicylate, eugenol, camphor,
Ginger, ethyl acetate, diethyl ketone, eucalyptol, pepper, rose, isopropylmethylphenol, maltol, anethole and the like can be mentioned. Examples of the pigments include inorganic or organic pigments, and more specifically, inorganic pigments such as cobalt blue, cobalt green, yellow iron oxide, titanium oxide, mica, zinc powder, aluminum powder, blue No. 1, red Lake pigments such as tar pigments such as No. 2, copper chlorophyll, β-
Examples thereof include carotene and hinokitiol iron complex salts.

As the contents of the capsule, fats and oils, waxes, hydrocarbons, higher fatty acids, higher alcohols, esters, essential oils, silicone oils and the like are further compounded as excipients. be able to.

Examples of fats and oils include natural fats and oils such as soybean oil, bran oil, jojoba oil, avocado oil, almond oil, olive oil, cocoa butter, sesame oil, persic oil, castor oil, coconut oil, mink oil, beef tallow, lard, etc. Or hardened oils obtained by hydrogenating these natural fats and oils and synthetic triglycerides such as glyceride myristic acid, glyceride 2-ethylhexanoate, glyceride tricaprylate, and glyceride tricaprate. Examples of the waxes include carnauba wax, whale wax, beeswax, and lanolin. As hydrocarbons, liquid paraffin,
Examples include petrolatum, paraffin, microcrystalline wax, ceresin, squalane, pristane, and the like. Examples of higher fatty acids include lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, oleic acid, linoleic acid, linolenic acid, lanolinic acid and isostearic acid. Examples of higher alcohols include lauryl alcohol, cetyl alcohol, stearyl alcohol, oleyl alcohol, lanolin alcohol, cholesterol, 2-hexyldecanol, and the like. Examples of the esters include cetyl octoate, myristyl lactate, cetyl lactate, isopropyl myristate, myristyl myristate, isopropyl palmitate, isopropyl adipate, butyl stearate, decyl oleate, and the like. Essential oils include peppermint oil, jasmine oil, camphor oil, hinoki oil, spruce oil, ryu oil, turpentine oil, cauliflower oil, helgamot oil, tangerine oil, shobu oil, pine oil, lavender oil, bay oil, glove oil, Hiba oil, rose oil, eucalyptus oil, lemon oil, peppermint oil, rose oil, sage oil and the like can be mentioned. Examples of silicones include dimethylpolysiloxane and the like.

The method for producing the capsule is not particularly limited, and known production methods, for example, a chemical method such as an interfacial polymerization method and a curing in liquid coating method, and a physicochemical method such as a coacervate method. Although a physical method such as a fluidized bed method can be applied, a double nozzle dropping method is particularly preferable.

The capsule used in the present invention has an average particle size of 0.3 to 3 mm, particularly 0.5 to 3 mm, and more preferably 0.6 to 3 mm.
Preferably it is 2 mm. When the average particle size is less than 0.3 mm, the particles are hardly broken by brushing, the feeling in use is reduced, and the appearance is impaired. On the other hand, when the average particle size exceeds 3 mm, the feeling of use is significantly reduced, and the appearance is impaired. Since the film-forming substance of this capsule is agar, when the dentifrice base is added after the preparation of the capsule, it slightly swells, but the average particle size after the swelling needs to be in the above range.

The capsule has a breaking strength of 0.1 to 20 g per piece, particularly 1 to 20 g, and more preferably 1 to 20 g.
It is preferable that the amount is 0 g because the leakage of the contents is prevented during production and storage of the dentifrice composition, and the contents can be easily broken and the contents can be released during use. In addition, this breaking strength is indicated by the amount of load when one capsule taken out from the dentifrice composition is continuously applied from above and the capsule (coating) is broken. The breaking strength in the present invention was measured with a compression tester KES-F3 (manufactured by Kato Iron Works) at a speed of 50 seconds / mm.

The coating rate of agar in the capsule is 1 to 3
It is preferably 0% by weight, particularly preferably 1 to 15% by weight, and more preferably 5 to 15% by weight, since a suitable destructive property is imparted during use and the contents can be easily released. In addition, the coating ratio is represented by the weight percentage of agar relative to the total weight of the capsule.

The content of the capsule in the dentifrice composition of the present invention is preferably 0.1 to 10% by weight, and particularly preferably 0.1 to 10% by weight.
The content of 5 to 5% by weight is preferable because effects such as medicinal ingredients can be appropriately exhibited, the feeling in use is good, and the appearance is beautiful.

In addition to the above-mentioned components, the dentifrice composition of the present invention also contains oral vehicles generally used in oral preparations such as dentifrices, for example, abrasives, binders, surfactants, wetting agents, flavors, sweeteners. Ingredients, preservatives, water and the like can be added.

Among these, abrasives include dibasic calcium phosphate, tribasic calcium phosphate, insoluble sodium metaphosphate, silica, aluminum hydroxide, magnesium phosphate, calcium carbonate, calcium pyrophosphate, zeolite, composite aluminosilicate, magnesium carbonate,
Bengala, calcium sulfate and the like can be mentioned. Examples of the binder include sodium carboxymethyl cellulose, sodium polyacrylate, hydroxyethyl cellulose, thickening silica, montmorillonite, carrageenan, sodium alginate, guar gum, xanthan gum, pectin and the like. Furthermore, the surfactant is not particularly limited as long as it is generally used in dentifrice compositions, and acyl amino acid salts such as sodium acylglutamate and sodium acylsarcosine, alkyl sulfate salts such as sodium lauryl sulfate, and the like. Ionic surfactants, sucrose fatty acid esters, sorbitan fatty acid esters, polyoxyethylene
Examples include nonionic surfactants such as polyoxypropylene block copolymers.

The amounts of these oral vehicles are, for example, 1 to 75% by weight of an abrasive, 5% by weight or less of a binder,
In particular, it is preferable to add 0.1 to 5% by weight, more preferably 0.5 to 5% by weight, 1 to 40% by weight of a surfactant, and 10 to 85% by weight of a wetting agent and water in total. it can.

The dentifrice composition of the present invention can be formed into a desired form such as toothpaste, powdered toothpaste, liquid dentifrice, etc., but the agar forming the capsule film is transparent (colored or colorless and transparent depending on the pigment to be mixed). ), The dentifrice composition itself, except for the capsule, is also made transparent, thereby further enhancing the aesthetic appearance by synergy between the transparency of the capsule and the transparency of the entire composition containing the same. Can be. When the dentifrice composition is thus transparent, the transparency is preferably 3 mm or more, particularly preferably 5 mm or more. The method for measuring the transparency is based on the method described in Examples.

[0029]

The dentifrice composition of the present invention contains agar as a film-forming substance as a main component and has an average particle size of 0.3 to 3%.
Contains capsules that are mm. Therefore, at the time of use, the capsule is easily broken by brushing, and the contents such as medicinal ingredients can be released and permeated into the oral cavity locally. In addition, since the capsules are easily broken and have an appropriate particle size, the feeling of discomfort and foreign matter in the oral cavity during use is small, and the feeling of use is excellent. Furthermore, since the size of the capsule is such that its presence can be visually confirmed, it is possible to give the user a sense of security and an expectation due to the development of medicinal effects, etc., while hesitating to use. It does not give such a foreign-body sensation (discomfort). In addition, the dentifrice composition of the present invention has very little leakage of contents during production and storage, and has high component stability.

[0030]

EXAMPLES The present invention will be described in more detail with reference to the following Examples, but it should not be construed that the invention is limited thereto.

Production Example 1 Capsules were produced according to the following formulation and production method. The agar is trade name UP-37 (solubility 10, jelly strength 700)
g / cm ² ; manufactured by Ina Food Industry Co., Ltd.).

(Capsule formulation) Coating solution formulation: Agar 5% by weight Purified water 95% by weight Content solution formulation: Tri (caprylic acid / caprylic acid) glycerin ^{* 1} 40% by weight β-glycyrrhetinic acid 50% by weight Ethanol 10% by weight % * 1: Coconado MT, manufactured by Kao Corporation, a triglyceride of a mixture of caprylic acid and capric acid

(Capsule Preparation Method) Capsules were prepared by a double nozzle dropping method. However, the nozzle diameter of the content liquid was 0.8 mm, the nozzle diameter of the coating liquid was 1.0 mm, the temperature of the coating tank and the coating line was set at 75 ° C., and the temperature of the cooling liquid was set at 25 ° C.

The capsule thus obtained had an average particle size of 1 mm and a coating ratio of 10.2% by weight. The particle size was measured with a caliper, and the coating ratio was determined by measuring the total weight of one capsule, then breaking the capsule, and measuring the weight of only the coated portion. Each value is an average value of 20 pieces. The same measurement was performed in the following Production Examples. Also, destroy one of the capsules and
-Glycyrrhetinic acid was extracted with a 0.0025 M aqueous solution of phosphoric acid-methanol (75 v / v%), and the amount thereof was determined using high performance liquid chromatography (L-6000, manufactured by Hitachi, Ltd.). Met.

Production Example 2 A capsule was produced by the following formulation and the same production method as in Production Example 1.

(Capsule formulation) Coating solution formulation: agar (same as in Production Example 1) 10% by weight Purified water 90% by weight Content solution formulation: tri (caprylic acid / capric acid) glycerin 40% by weight β-glycyrrhetinic acid 50% by weight Ethanol 10% by weight

The capsule thus obtained had an average particle size of 1 mm and a coating ratio of 36.2%. When one of the capsules was broken and the amount of β-glycyrrhetinic acid in the capsule was quantified in the same manner as in Production Example 1, the amount was 31.
It was 9% by weight.

Production Example 3 Capsules were produced in the same manner as in Production Example 1 and according to the production method of Production Example 1. However, the nozzle diameter of the content liquid is 0.
The nozzle diameter of the coating liquid was 0.35 mm. The capsule thus obtained has an average particle size of 0.35 m.
m, and the coating ratio was 10.8%. The amount of β-glycyrrhetinic acid in this capsule was determined in the same manner as in Production Example 1 to be 44.6% by weight.

Comparative Production Example 1 Among the capsules produced in Production Example 3, those having a particle size of less than 0.3 mm were screened. The capsule thus obtained had an average particle size of 0.24 mm and a coating ratio of 10.8% as in Production Example 3. The amount of β-glycyrrhetinic acid in this capsule was determined in the same manner as in Production Example 1, and it was 43.6% by weight.

Comparative Production Example 2 A capsule was produced in the same manner as in Production Example 1 and according to the production method of Production Example 1. However, the nozzle diameter of the content liquid is 2.
80 mm, and the nozzle diameter of the coating solution was 3.50 mm. The capsule thus obtained has an average particle size of 3.50 m.
m, and the coating ratio was 9.8%. Further, the amount of β-glycyrrhetinic acid in this capsule was determined in the same manner as in Production Example 1, and it was 45.1% by weight.

Examples 1 to 4 and Comparative Examples 1 and 2 Dentifrices having the compositions (in% by weight) shown in Table 1 were produced by a conventional method. With respect to these dentifrices, tests of each item shown in Table 1 were performed by the following methods. The reason why the measured value of the particle size differs from that of the above-mentioned production example is that the agar absorbed water and swelled. Table 1 shows the results.

(1) Method for Measuring Particle Size, Film Coverage, and Breaking Strength The above method was used to measure 20 capsules, and the average value was indicated.

(2) Transparency The test method will be described with reference to FIGS. First, a measuring cylinder 1 having a mark as shown in FIG.
0. Dentifrice was added. Next, while the glass tube 14 whose bottom was closed with a colorless transparent flat glass plate was sunk inside the measuring cylinder 10, the glass tube 14 was visually observed from the upper opening of the glass tube 14. The thickness a (mm) that can be clearly identified was defined as the transparency (see FIG. 2). At the time of the test, 40 W × 2 fluorescent lamps were used as a light source via a ground glass.

(3) Release amount of β-glycyrrhetinic acid (easiness of destruction) First, as shown in FIG. 3, a glass tube (teeth) having a diameter of 7 mm and a length of 80 mm was placed on an epoxy resin base (gum). By bonding and fixing, a tooth model was prepared. Next, 1g of each dentifrice
Is precisely weighed into a toothbrush and a constant load is applied on the tooth model using the scrubbing method (300 g per brush area).
Brushing (3-4 strokes per second). 1
Minutes or 3 minutes after brushing, the released β-
The amount of glycyrrhetinic acid was measured in the same manner as in Production Example 1.
The release amount was indicated by the ratio (expressed in% by weight) of this measured amount to the amount of β-glycyrrhetinic acid at the time of blending the capsule.

(4) Sensory evaluation Thirty men and women (15 persons each) between the ages of 20 and 40 years old actually used the dentifrices of the examples and comparative examples. The dentifrice was evaluated organoleptically based on the following criteria. The evaluation was performed by summing up the scores of each person and using the average value for each dentifrice. (Usability) 1 = No discomfort / feeling of foreign matter. 2 = almost no discomfort or foreign object feeling. 3 = Somewhat uncomfortable feeling / foreign body feeling. 4 = Feeling strange or foreign 5 = I feel a sense of strangeness and foreign matter strongly. (Appearance) 1 = preferred. 2 = Slightly preferred. 3 = Neither. 4 = Not very good. 5 = not preferred.

[0046]

[Table 1]

As is clear from the results in Table 1, when the average particle size of the capsule is smaller than 0.3 mm (Comparative Example 1)
Was hardly destroyed by brushing, so that the amount of released contents was small. Furthermore, the capsules which remained without being destroyed increased discomfort / foreign body sensation in the oral cavity. In addition, when the average particle size of the capsule was larger than 3 mm (Comparative Example 2), the amount of released contents was large because the capsule was easily broken by brushing. However, the feeling of incongruity / foreign matter until all capsules are destroyed, the feeling of incongruity / foreign matter due to a large amount of agar remaining even after destruction deteriorates the usability, and the product appearance is also impaired. From these results, it was confirmed that when the average particle size was out of the range of 0.3 to 3 mm, all of the products were defective. In addition, when the coating rate exceeded 30% by weight (Example 2), it was slightly less likely to be broken, and the amount of released contents was smaller than in Examples 1 and 3. In addition, it was found that when the transparency was 3 mm or more (Example 3), the user was given a particularly preferable feeling.

[Brief description of the drawings]

FIG. 1 is an explanatory diagram of a method for measuring transparency.

FIG. 2 is an explanatory diagram of a method for measuring transparency.

FIG. 3 is an explanatory diagram of a test method for measuring an amount of released contents.

──────────────────────────────────────────────────続 き Continuation of the front page Examiner Aki Nakaki (56) References JP-A-55-100309 (JP, A) JP-A-63-5011 (JP, A) JP-A-1-268622 (JP, A) JP-A-52-148635 (JP, A) (58) Fields investigated (Int. Cl. ⁷ , DB name) A61K ^7/ 00-7/50

Claims (4)

(57) [Claims] An agar having a jelly strength of 500 g / cm ² or more as a main component of a film-forming substance, wherein the agar has a coating ratio of 1 to 30% by weight and an average particle size of 0.3 to 3 m.
m, a dentifrice composition comprising a capsule having a breaking strength of 0.1 to 20 g / piece. 2. The dentifrice composition according to claim 1, wherein the capsule has an average particle size of 0.5 to 3 mm. 3. The dentifrice composition according to claim 1, wherein the capsule is produced by a double nozzle dropping method. 4. The dentifrice composition according to claim 1, wherein the dentifrice composition has a transparency of 3 mm or more.