JP5656368B2 - Dentifrice - Google Patents

Description

  The present invention relates to a dentifrice containing a xanthine derivative and a binder.

  It is known that xanthine derivatives such as caffeine have a central nervous excitability and can improve drowsiness and also have a masking effect on sweetness, and are used for the purpose of obtaining a refreshing aftertaste without causing a sweet taste. For example, Patent Documents 1 and 2 disclose oral compositions and foods containing caffeine from the viewpoint of masking the sweetness of sweeteners. In addition, caffeine is also known to have an effect of improving irritation to mucous membranes by essential oil components such as menthol, camphor, and borneol (for example, Patent Document 3).

  However, although the solubility of caffeine in water is 15% by mass at 80 ° C., it is as low as about 2% by mass at room temperature (20 ° C.), and the solubility varies greatly depending on the temperature. There is a problem of end up. On the other hand, Patent Document 4 describes an eye drop containing 0.0001 to 10% by mass of aminoethylsulfonic acid and 0.4 to 10% by mass of caffeine. On the other hand, Patent Document 5 contains 0.5 to 15% by weight of caffeine and contains a mixture of alcohol and water in a weight ratio of 5 to 200 times that of caffeine, thereby dissolving caffeine. A percutaneous absorption preparation with improved properties is described.

JP-A-8-245350 Japanese Patent Laid-Open No. 9-238641 JP 2001-302518 A JP 2002-37735 A JP-A-10-53527

The present inventor anticipated the drowsiness improving action, sweetness masking action and refreshing agent irritation improving action of xanthine derivatives such as caffeine, and started studies for blending them into a dentifrice. However, the dentifrice is different from the eye drops such as Patent Documents 3 and 4, and requires appropriate viscosity and shape retention from the viewpoint of retaining the dentifrice-containing component on the tooth surface and gum surface for a predetermined time. Therefore, a binder is blended. And when the viscosity of the composition is improved by blending a xanthine derivative and a binder, the xanthine derivative has a new problem that the solubility in water decreases and the crystals precipitate when the viscosity increases. There was found. It has also been found that xanthine derivatives have the effect of increasing the viscosity of dentifrices.
Accordingly, an object of the present invention is to provide a stable dentifrice that contains a xanthine derivative and a binder and does not precipitate crystals of the xanthine derivative.

  Therefore, the present inventor has made various studies to obtain a dentifrice having a dampness-improving effect and a sweetness-masking effect, in which the xanthine derivative is stably blended in a dissolved state and has an appropriate viscosity. It has been found that such a problem can be solved when the binder is blended at a certain ratio.

That is, the present invention includes the following components (A), (B), (C) and (D):
(A) A xanthine derivative selected from the group consisting of caffeine, theophylline, theobromine and salts thereof 0.1 to 1.5% by mass
(B) 35-60 mass% of water
(C) Glycerin 0.1 to 35% by mass
(D) Binder 0.2-4% by mass
And a dentifrice with a mass ratio ((B + C) / A) of the sum of the component (B) and component (C) to the component (A) of 50 to 700.

  The dentifrice of the present invention contains a xanthine derivative and a binder, and can effectively suppress crystallization of the xanthine derivative while having an appropriate viscosity and shape retention.

The dentifrice of the present invention comprises the above component (A) xanthine derivative selected from the group consisting of caffeine, theophylline, theobromine and salts thereof, component (B) water, component (C) glycerin, and component (D). It is obtained by blending a binder.
The component (A) xanthine derivative in the dentifrice of the present invention is caffeine, theophylline, theobromine or a salt thereof, and among these, caffeine is preferable. Caffeine includes anhydrous caffeine and caffeine hydrate.
Caffeine is the chemical name 3,7-dihydro-1,3,7-trimethyl-1H-purine-2,6-dione (1,3,7-trimethylxanthine), for example from Shiratori Pharmaceutical Co., Ltd. It is sold under the brand name of anhydrous caffeine.
The compounding amount of the component (A) in the dentifrice of the present invention is 0.1 to 1.5% by mass from the viewpoint of sufficiently exerting the effects of the xanthine derivative such as drowsiness improvement, sweetness masking, and improvement of the stimulation of the refreshing agent. It is preferably 0.2 to 1.2% by mass, more preferably 0.5 to 1% by mass.

The dentifrice of the present invention contains 35 to 60% by mass of component (B) water and 0.1 to 35% by mass of component (C) glycerin. The blending amount of the component (C) is further preferably 30% by mass or less, and is suitable when blending 1% by mass or more and further 3% by mass or more from the viewpoint of suppressing crystal precipitation of the component (A).
The total amount of the component (B) and the component (C) is (B + C) / (A) in the mass ratio of 50 to 700 with respect to the component (A) from the viewpoint of suppressing crystallization of the component (A). And preferably 500 or less, particularly 100 or less. Furthermore, the mass of the component (B) and the component (C) / 3 is a mass ratio with respect to the component (A), and (B + C / 3) / (A) is 45 to 500, and further 48 to 300, It is suitable especially when it is 51-100. In the dentifrice of the present invention, the component (E) sugar and sugar alcohol can be blended, but when the component (E) is blended, the amount necessary to dissolve the component (E) from the total moisture. The mass excluding water (F) is defined as the mass of the component (B) water. The amount of water (F) necessary for dissolving the component (E) is the mass necessary for dissolving the component (E) at 20 ° C. If the component (E) is, for example, sorbitol, sorbitol water ( 30% of water in 70%) is the component (F), and is not included in the component (B).

The moisture content of the dentifrice can be calculated from the blended moisture content and the moisture content in the blended component, but can be measured, for example, with a Karl Fischer moisture meter. As the Karl Fischer moisture meter, for example, a trace moisture measuring device (Hiranuma Sangyo) can be used. In this apparatus, 5 g of dentifrice is taken and suspended in 25 g of anhydrous methanol, and 0.02 g of this suspension is fractionated and the amount of water can be measured. And when the dentifrice contains the sugar alcohol and / or sugar of the component (E), the water (F) necessary for dissolving the component (E) at 20 ° C. from the measured water mass. The mass excluding the weight is the component (B) water.
35-75 mass% is preferable and, as for the sum total (B + F) of the moisture content of a dentifrice, 40-70 mass% is more preferable.

  The dentifrice of the present invention contains a binder of component (D). As the binder of component (D), sodium alginate, sodium carboxymethyl cellulose, carrageenan, xanthan gum, sodium polyacrylate, hydroxyethyl cellulose, hydroxypropyl cellulose, pectin, tragacanth gum, gum arabic, guar gum, caraya gum, locust bean gum, gellan gum It is preferable to blend any one or more of tamarind gum, psyllium seed gum, polyvinyl alcohol, sodium chondroitin sulfate, and a methoxyethylene maleic anhydride copolymer. The compounding amount of the component (D) binder is 0.2 to 4% by mass, preferably 0.5 to 2%, from the viewpoint of suppressing the crystallization of the component (A) and the viscosity and shape retention as a dentifrice. % By mass.

Component (E) sugar and / or sugar alcohol can be mix | blended with the dentifrice of this invention. Component (E) is a sugar and / or sugar alcohol 50~80g soluble in water solution 100g at 20 ° C., the dentifrice of the present invention as component (E), 60～80G dissolved in water solution 100g It is suitable when blending sugar and / or sugar alcohol, and particularly when blending sugar alcohol. The sugar and / or sugar alcohol component (E), sorbitol to 72g dissolved in water solution 100g at 20 ° C., xylitol to 66g dissolved, maltitol, trehalose to 68.9g dissolved mentioned to 60g dissolved, Sorbitol is preferred from the viewpoint of the moisturizing effect. The amount of component (E) is preferably 0% by mass or more, more preferably 2% by mass or more, preferably 30% by mass or less, and more preferably 20% by mass or less from the balance with the total amount of moisture. .

The dentifrice of the present invention can further contain a polyhydric alcohol (other than glycerin). Examples of the polyhydric alcohol include propylene glycol, trimethylene glycol, 1,2-butanediol, 1,3-butanediol, dipropylene glycol, polyethylene glycol and the like, and polyethylene glycol and propylene glycol are preferable. The polyhydric alcohol is not blended or can be blended more than 0% by mass, preferably 2% by mass or more, and 8% by mass or less, more preferably 6% by mass or less from the viewpoint of feeling of use such as taste and stickiness. Are preferred.
Furthermore, the dentifrice of the present invention can contain a monohydric alcohol such as ethanol, but it is preferably 5% by mass or less, more preferably 2% by mass or less, particularly from the viewpoint of taste and irritation. It is preferable that it is 1 mass% or less.

  The dentifrice of the present invention can be a gel or paste toothpaste, but the viscosity at 25 ° C. is preferably 1000 to 5000 dPa · s, and more preferably 1500 to 4000 dPa · s from the viewpoint of use feeling. Further, a dentifrice having a viscosity of 1500 to 4000 dPa · s at a temperature of 25 ° C. after being stored for one week or more after production is preferable. Are preferred.

The dentifrice of the present invention can further contain a sugar alcohol excluding component (E) as long as the effects of the present invention are not impaired. The sugar alcohols excluding component (E), the dissolved amount of the water solution of 100g at 20 ° C. is a small sugar alcohols than 50 g, for example, erythritol, lactitol, palatinit, mannitol.
The dentifrice of the present invention contains other ingredients that can be used for oral use, such as abrasives, foaming agents, fluorine ion supply compounds, sweeteners, flavors, pH adjusters, preservatives, various medicinal ingredients, You may mix | blend suitably in the range which does not inhibit the objective of this invention.

  As the abrasive, within the range that does not impair the usability of the present invention, silica-based abrasives such as hydrous silica, anhydrous silica, silica gel, precipitated silica, silica gel, aluminosilicate, zirconosilicate, gluconosilicate, etc. Calcium diphosphate dihydrate and anhydrous, calcium pyrophosphate, calcium carbonate, alumina, aluminum hydroxide, magnesium acetate, tribasic magnesium phosphate, zeolite and the like can be used. In particular, from the viewpoint of sufficient cleaning effect and usability, it is preferable to use hydrous silica, anhydrous silica, calcium hydrogen phosphate dihydrate, calcium hydrogen phosphate anhydrate, alumina, aluminum hydroxide, calcium carbonate, zeolite. preferable. The content of the abrasive is preferably 5 to 20% by mass, and particularly preferably 7 to 15% by mass, in the dentifrice of the present invention, from the viewpoint of obtaining a sufficient cleaning effect and good usability.

  Foaming agents include anionic, nonionic, cationic, and amphoteric surfactants. As these surfactants, only one surfactant may be used from among anionic, nonionic, and cationic surfactants. However, when two or more surfactants are used, any one of them is used. The surfactant is preferably 0.1% by mass or less. In addition, when only one surfactant is used from among the above-mentioned surfactants, for example, when an anionic surfactant is contained, an anionic surfactant having a plurality of compositions can be used. In the case of using these surfactants, a surfactant having a plurality of compositions can be used for each surfactant.

Examples of the anionic surfactant include acyl amino acid salts such as sodium acyl glutamate and acyl sarcosine sodium, alkyl phosphates such as sodium alkyl phosphate, alkyl sulfate salts, higher fatty acid sulfonated monoglyceride salts, fatty acid esters of isethionic acid. Salt, N-methyl long chain acyl taurine sodium salt, polyoxyethylene monoalkyl phosphate. The hydrophobic alkyl group and acyl group in these anionic surfactants preferably have 6 to 18 carbon atoms, particularly 10 to 14 carbon atoms. The salt is preferably a sodium salt. As the anionic surfactant, an alkyl sulfate ester salt is particularly preferable from the viewpoint of good foamability and availability at low cost.
The anionic surfactant is preferably contained in the dentifrice of the present invention in an amount of 0 to 5% by mass, and more preferably 0 to 2% by mass.

  Examples of the fluoride ion supply compound include sodium fluoride, tin fluoride, ammonium fluoride, potassium fluoride, lithium fluoride, sodium monofluorophosphate, potassium monofluorophosphate, and ammonium fluoride.

  Examples of the sweetening agent include saccharin sodium, aspartame, thaumatin, acesulfame potassium, stevioside, stevia extract, paramethoxycinnamic aldehyde, neohesperidyl dihydrochalcone, and perilartin.

  As a flavoring agent, 1-menthol, carvone, anethole, eugenol, limonene, peppermint oil, spearmint oil, ocimen, n-amyl alcohol, citronellol, α-terpineol, methyl salicylate, methyl acetate, citronol acetate, cineol, 1 , 8-cineole, linalool, ethyl linalool, crocodile, thymol, lemon oil, orange oil, sage oil, rosemary oil, cinnamon oil, pimento oil, perilla oil, clove oil, eucalyptus oil, hatsuka oil, anise oil, winter green Oil etc. are mentioned.

  Various medicinal ingredients include anti-inflammatory agents such as allantochlorohydroxyaluminum, azulene, glycyrrhetinic acid, epidihydrocholesterin, α-bisabolol, glycyrrhizic acid and salts thereof; phenolic compounds such as hinokitiol; tranexamic acid, epsilon aminocaproic acid, etc. Α-tocopherol, α-tocopherol acetate (dl-form, d-form) and salts thereof; copper compounds such as copper chlorophyllin sodium and copper gluconate; salts such as sodium chloride and potassium nitrate; dextranase, mutanase, Enzymes such as amylase and lysozyme chloride; extracts such as sugarcane, duck, clove, urgon, safflower; aluminum lactate, strontium chloride, berberine, hydroxamic acid and its derivatives, sodium tripolyphosphate Zeolite, dihydrocholesterol, and zinc citrate.

  In the following test examples and examples,% means mass%. Moreover, the prescription shown by the table means the mass% of each component.

Test example 1
Test solutions 1 to 8 were prepared according to the formulation in Table 1. Test solutions 2, 5, and 6 were prepared by adding 1% binder to an aqueous solution containing 2% caffeine. The viscosities of test solutions 2 to 5 were measured using a helipath viscometer (TVB-10R, manufactured by Toki Sangyo Co., Ltd.) immediately after preparation without dissolving the binder at 60 ° C. and cooling time. The temperature was measured under the measurement conditions of 40 ° C., rotor C, 50 r / min, and 1 minute. The test solution was stored at 20 ° C. for 7 days, and the crystal state after 4 and 7 days was confirmed. The degree of crystallization was evaluated according to the following criteria.
0: Neither crystals nor solids are confirmed 1: Slight crystals are confirmed (amount that can be counted)
2: Solid is confirmed and the liquid is cloudy. 3: It can be seen that there are crystals. 4: The crystals are layered. 5: The crystals are covered.

  As shown in Table 1, it was confirmed that the viscosity of the test liquid 2 containing caffeine was higher than that of the test liquid 3 not containing caffeine. Moreover, the test liquids 2, 4 to 6 containing the binder were confirmed to produce crystals or solids after storage. Test solution 7 containing glycerin had high caffeine solubility, but crystals were confirmed after storage. On the other hand, crystals were not confirmed in Test Solution 8 in which glycerin and a binder were blended.

Test example 2
Test solutions 9 to 15 were prepared according to the formulation in Table 2. In the same manner as in Test Example 1, the sample was stored at 20 ° C. for 7 days, and the degree of crystallization after 4 days and after 7 days was evaluated in the same manner as in Test Example 1.

As shown in Table 2, the test solution 9 containing sorbitol, the test solution 10 containing xylitol, and the test solution 12 containing trehalose confirmed crystals after storage at 20 ° C. for 7 days. Test solution 11 containing erythritol solubility of 36g in water solution 100g at 20 ° C. In contrast crystals after storage 7 days was observed. On the other hand, crystals were confirmed in the test solution 13 containing polyethylene glycol after storage. On the other hand, in the test solutions 14 and 15 containing sorbitol, a binder and glycerin, no crystal was observed after storage even though the amount of water relative to caffeine was smaller than that of the test solution 9.

Examples 1-8, Comparative Examples 1-2
According to the formulation shown in Table 3, the dentifrices of Examples 1 to 8 and Comparative Examples 1 and 2 were prepared. The viscosity of the dentifrice was measured using a helipath type viscometer at a measurement temperature of 25 ° C. and measurement conditions of rotor C, 50 r / min for 1 minute. The viscosity and the presence or absence of crystals after 1 week when the dentifrice was stored at 25 ° C were evaluated for the presence or absence of crystals after 1 month and 2 months after storage at 5 ° C.
Evaluation of crystals 0: No acicular crystals 1: With acicular crystals

  As shown in Table 3, Example 1 which contains a binder and the total weight of glycerin and water (excluding water necessary for dissolving sorbitol at 20 ° C.) is 50 times or more of caffeine No crystals were confirmed for -8 after storage at 25 ° C for 1 week and after storage at 5 ° C for 1 week. On the other hand, Comparative Examples 1 and 2 containing 40% of water (excluding water contained in the sorbitol solution) but having a total amount of glycerin and water smaller than 48 times that of caffeine are 1 at 25 ° C. Crystals were confirmed after weekly storage, and when stored at 5 ° C., crystals were confirmed after one month and two months. In addition, when stored at 5 ° C., crystals were not confirmed in Examples 7 and 8 after 1 month, but crystals were confirmed after 2 months, and Examples 1 to 6 were crystals after 2 months. It was not confirmed. In Comparative Examples 1 and 2, crystals were formed after one week, and the viscosity increased more than twice, but Examples 3 to 6 had a viscosity immediately after production of the dentifrice and a viscosity after one week. The difference is 600 dPa · s or less, and it is considered that the effect of suppressing crystal formation is high.

Claims (3)

The following components (A), (B), (C) and (D):
(A) Caffeine 0.2-1.5 mass%
(B) 35-60 mass% of water
(C) Glycerin 0.1 to 35% by mass
(D) Binder selected from carboxymethylcellulose, sodium carboxymethylcellulose, xanthan gum and carrageenan 0.2-4% by mass
The mass ratio ((B + C) / A) of the sum of component (B) and component (C) to component (A) is 50 to 500,
The viscosity at 25 ° C. is 1000 to 5000 dPa · s,
(E) The content of sugar and / or sugar alcohol selected from sorbitol, xylitol and trehalose is 0 to 20% by mass,
In the case where the component (E) is contained, the dentifrice further contains (F) water necessary for dissolving the component (E) at 20 ° C. in addition to the water of the component (B) . The dentifrice according to claim 1, wherein a sugar and / or sugar alcohol selected from the component (E) sorbitol, xylitol and trehalose, and (F) water in an amount necessary for dissolving the component (E) at 20 ° C are blended. Agent.   Furthermore, the dentifrice of Claim 1 or 2 containing a polyhydric alcohol.