JP2021066667A - Oral composition - Google Patents

Abstract

To provide means that can suppress a rise in viscosity of an oral composition containing a thickener, aluminium lactate, and silica even if it is stored.SOLUTION: The present disclosure provides an oral composition containing a thickener, aluminium lactate, silica and hydroxy apatite particles.SELECTED DRAWING: None

Description

The present disclosure relates to oral compositions and the like, and more particularly to oral compositions and the like containing aluminum lactate and silica.

Since aluminum lactate is a medicinal ingredient for preventing hyperesthesia, it is added to the oral composition in anticipation of the effect. Further, silica is blended in an oral composition as a tooth abrasive and the like.

Japanese Unexamined Patent Publication No. 5-155745

The present inventors significantly increase the viscosity of an oral composition containing a thickener, aluminum lactate, and silica when it is stored (particularly when it is stored at a relatively high temperature, for example, about 40 to 60 ° C.). I found out to do. This temperature is a temperature that is sufficiently possible in the distribution of oral composition products (particularly in the summer), and from the viewpoint of keeping the quality of the products constant, such a time course during transportation or storage. The increase in viscosity is not preferable.

Therefore, the present inventors have investigated a method capable of suppressing an increase in viscosity over time for an oral composition containing a thickener, aluminum lactate, and silica. As a result, it has been found that by further adding hydroxyapatite particles to the oral composition, it is possible to efficiently suppress the increase in viscosity of the oral composition (particularly, the increase in viscosity with time). Then, based on the findings, further studies were carried out.

The present disclosure includes, for example, the subjects described in the following sections.
Item 1.
Oral composition containing thickener, aluminum lactate, silica, and hydroxyapatite particles.
Item 2.
Item 2. The oral composition according to Item 1, wherein the thickener is at least one selected from the group consisting of alginic acid or a salt thereof, hydroxyalkyl cellulose, carboxyalkyl cellulose or a salt thereof, xanthan gum, and carrageenan.
Item 3.
Item 2. The oral composition according to Item 1, wherein the thickener is carboxymethyl cellulose or a salt thereof.
Item 4.
Item 2. The oral composition according to any one of Items 1 to 3, wherein the viscosity at 30 ° C. is 400 Pa · s or less.
Item A.
A method for suppressing an increase in viscosity of an oral composition over time, which comprises further blending hydroxyapatite particles in the preparation of an oral composition containing a thickener, aluminum lactate, and silica.

Provided is an oral composition containing a thickener, aluminum lactate, and silica, and suppressing an increase in viscosity during storage.

It is a graph which shows the value calculated by subtracting the viscosity value immediately after preparation from the viscosity value measured after storing each oral composition at 55 degreeC for 6 days.

Hereinafter, each embodiment included in the present disclosure will be described in more detail. The present disclosure preferably includes, but is not limited to, an oral composition, particularly an oral composition containing a thickener, aluminum lactate, and silica, and the present disclosure is described herein. Includes everything disclosed and recognizable to those skilled in the art.

The oral compositions included in the present disclosure contain hydroxyapatite particles in addition to thickeners, aluminum lactate, and silica. In addition, in this specification, the said oral composition may be referred to as "the oral composition of this disclosure".

As the hydroxyapatite particles, hydroxyapatite particles known in the field of oral composition can be used. Further, hydroxyapatite particles prepared by a known method or a method easily conceived from a known method can also be used. Furthermore, a commercially available hydroxyapatite product can be purchased and used. For example, it can be purchased from Tomita Pharmaceutical Co., Ltd. and used.

The median diameter (d50) of the hydroxyapatite particles is not particularly limited, but is preferably 5 μm or less, more preferably 4.5 μm or less. The lower limit of the median diameter is not particularly limited, and examples thereof include 1 μm or more, 2 μm or more, or 3 μm or more. More specifically, for example, 1 to 5 μm can be mentioned. The median diameter is a value measured by a laser diffraction / scattering method. More specifically, it is a value measured by a dry particle size distribution measurement using a laser diffraction type particle size distribution measuring device.

The hydroxyapatite particles are prepared by, for example, a method for producing hydroxyapatite particles, which comprises a step of mixing an aqueous solution of an alkali phosphate salt having a pH of 4 or more and less than 7 and a calcium hydroxide slurry and reacting them at 35 to 85 ° C. can do.

The alkali salt of phosphoric acid is not particularly limited and includes hydrates and anhydrides. Examples of the alkali phosphate salt include sodium dihydrogen phosphate, disodium hydrogen phosphate, trisodium phosphate, tetrasodium pyrophosphate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate, tripotassium phosphate and the like. , Preferred are sodium phosphate salts such as sodium dihydrogen phosphate, disodium hydrogen phosphate, trisodium phosphate and the like, and more preferably sodium dihydrogen phosphate.

The concentration of the alkali phosphate salt in the aqueous solution of the alkali phosphate salt is not particularly limited, and is, for example, 3 to 50% by mass. The concentration is preferably 3 to 30% by mass, more preferably 5 to 20% by mass, and even more preferably 7 to 15% by mass.

The pH of the aqueous alkali salt solution is preferably 4 or more and less than 7. The pH is more preferably 5 to 6.5. As will be described later, when the pH of the aqueous solution of the alkali phosphate is relatively low (for example, when the pH is 4 or more and less than 5), an anhydride is used as the alkali phosphate and the reaction temperature is relatively high. For example, it is desirable to set it at 65 to 85 ° C., preferably 70 to 85 ° C., and more preferably 75 to 85 ° C.

Where the calcium hydroxide slurry has oxalic acid reactivity, the calcium hydroxide slurry is preferably a calcium hydroxide slurry having a specific reactivity with oxalic acid.

Reactivity to oxalic acid can be expressed, for example, by the following definition:
Oxalic acid reactivity: 50 g of calcium hydroxide slurry prepared at a concentration of 5% by mass and maintained at 25 ± 1 ° C., and 40 g of an aqueous oxalic acid solution having a concentration of 0.5 mol / liter maintained at 25 ± 1 ° C. Is added all at once, and the time (minutes) until the pH reaches 7.0 after the addition.

The specific reactivity with oxalic acid is preferably 1 to 40 minutes, more preferably 5 to 30 minutes, still more preferably 10 to 20 minutes, as defined above.

The BET specific surface area of the calcium hydroxide slurry is preferably 5 m ² / g or more, more preferably 6 m ² / g or more. The upper limit of the BET specific surface area is not particularly limited, but is, for example, 20 m ² / g, 15 m ² / g, and 10 m ² / g.

A calcium hydroxide slurry having high oxalic acid reactivity (for example, having reactivity with the above-mentioned specific oxalic acid) can be typically obtained by grinding the calcium hydroxide slurry. The oxalic acid reactivity can be further enhanced (the time defined above is shortened) by the grinding treatment. The grinding process is performed using, for example, a bead mill. The conditions for the grinding treatment are not particularly limited, and for example, conditions according to the method described in JP-A-2017-036176 can be adopted.

The calcium hydroxide slurry can be prepared, for example, by reacting water with quicklime (calcium oxide) obtained by calcining limestone. For example, a calcium hydroxide slurry can be prepared by calcining limestone in a kiln at about 1000 ° C. to produce quicklime, adding about 10 times the amount of hot water to the quicklime and stirring for 30 minutes. it can.

The solid content concentration of the calcium hydroxide slurry is not particularly limited, but is, for example, 1 to 30% by mass, preferably 3 to 20% by mass, more preferably 5 to 15% by mass, and further preferably 6 to 12% by mass.

The amount ratio of the aqueous alkali salt solution to the calcium hydroxide slurry is not particularly limited as long as the ratio can produce hydroxyapatite particles. The amount ratio is adjusted so that the Ca / P molar ratio is preferably 0.3 to 0.7, more preferably 0.4 to 0.6, and even more preferably 0.45 to 0.55. Is desirable.

The mode in which the aqueous solution of the alkali salt phosphate and the calcium hydroxide slurry are mixed is not particularly limited. For example, an embodiment in which a calcium hydroxide slurry is added to a reaction vessel containing an aqueous alkali salt phosphate solution (Aspect 1), an embodiment in which an aqueous alkali salt phosphate solution is added to a reaction vessel containing a calcium hydroxide slurry (Aspect 2), and phosphoric acid. An embodiment (aspect 3) in which an aqueous alkali salt solution and a calcium hydroxide slurry are added to the reaction vessel at the same time can be mentioned. Among these, aspect 1 is preferable. At the time of the above addition to the reaction vessel, the liquid in the reaction vessel is usually stirred.

It is desirable that the above addition to the reaction vessel be carried out over a certain period of time. The time from the start of addition to the end of addition is, for example, 10 to 90 minutes, preferably 20 to 60 minutes, and more preferably 20 to 40 minutes.

The reaction is usually carried out under stirring. The reaction temperature is 35-85 ° C. The reaction temperature is preferably 40 to 75 ° C, more preferably 45 to 70 ° C, still more preferably 50 to 70 ° C, still more preferably 55 to 65 ° C. The reaction temperature is relatively high when the pH of the aqueous solution of the alkali phosphate solution is relatively low (for example, when the pH is 4 or more and less than 5), for example, 65 to 85 ° C, preferably 70 to 85 ° C, more preferably 75. ~ 85 ° C. Reaction time (time to start after all the aqueous alkali salt solution and calcium hydroxide slurry are mixed, time to start from the time when the addition of the aqueous alkali phosphate solution and calcium hydroxide slurry is completed in the above embodiments 1 to 3). ) Is, for example, 10 to 180 minutes, preferably 20 to 120 minutes, more preferably 40 to 90 minutes, still more preferably 50 to 70 minutes.

The hydroxyapatite particles produced by the above steps are subjected to a purification treatment, if necessary. Examples of the purification treatment include filtration treatment, washing treatment and the like. Further, if necessary, it can be subjected to a drying treatment.

The hydroxyapatite particles can be contained in the oral composition, for example, in an amount of about 1 to 10% by mass. The upper or lower limit of the content ratio range is, for example, 1.5, 2, 2.5, 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, 7, 7.5. , 8, 8.5, 9, or 9.5% by mass. For example, the range is more preferably 2 to 8% by mass or 3 to 7% by mass.

Further, aluminum lactate is preferably contained in the oral composition of the present disclosure in an amount of 0.05 to 3% by mass. The upper or lower limit of the range is, for example, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1, 1.1. , 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2, 2.1, 2.2, 2.3, 2.4 , 2.5, 2.6, 2.7, 2.8, or 2.9% by mass. For example, the range may be 0.1 to 2.7% by mass or 0.2 to 2.5% by mass.

Although not particularly limited, the mass ratio of the hydroxyapatite particles and aluminum lactate contained in the oral composition is preferably about 0.2 to 0.6 aluminum lactate with respect to the hydroxyapatite particles 1. The upper or lower limit of the range may be 0.25, 0.3, 0.35, 4, 0.45, 0.5, or 0.55, for example 0.25 to 0.55 or 0. More preferably about 3 to 0.5.

As the thickener contained in the oral composition of the present disclosure, a known thickener used in the field of oral composition can be used. Examples of such thickeners include alginic acid or a salt thereof, hydroxyalkyl cellulose, carboxyalkyl cellulose or a salt thereof, xanthan gum, gellan gum, tragant gum, carrageenan, arabia gum, carrageenan, dextrin, polyvinyl alcohol, polyvinylpyrrolidone, and thickening silica. , Bee gum, O- [2-hydroxy-3- (trimethylammonio) propyl] hydroxyethyl cellulose chloride, polyalginic acid or a salt thereof, agar and the like.

Among these, alginic acid or a salt thereof, hydroxyalkyl cellulose, carboxyalkyl cellulose or a salt thereof, xanthan gum, carrageenan are preferable.

As the salt of alginic acid, an alkali metal salt of alginic acid is preferable, and more specifically, a potassium salt and a sodium salt are preferable. Sodium alginate is particularly preferable.

As the alkyl of the hydroxyalkyl cellulose, an alkyl having 1 to 4 carbon atoms (1, 2, 3, or 4) is preferable. Specific examples of the hydroxyalkyl cellulose include hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose and the like.

As the alkyl of the carboxyalkyl cellulose, an alkyl having 1 to 4 carbon atoms (1, 2, 3, or 4) is preferable. Specific examples of the hydroxyalkyl cellulose include carboxymethyl cellulose and carboxymethyl ethyl cellulose. Further, as the salt of carboxyalkyl cellulose, an alkali metal salt is preferable, and more specifically, a potassium salt or a sodium salt is preferable.

As the salt of polyacrylic acid, a sodium salt or a potassium salt can be preferably exemplified.

The thickener may be used alone or in combination of two or more. Further, the thickener can be contained in, for example, about 0.5 to 5% by mass in the oral composition, and the upper limit or the lower limit of the range is, for example, 1, 1.5, 2, 2.5, 3, 3 It can be 5, 4, or 4.5% by mass. For example, the range can be 1 to 3% by mass or 1 to 2.5% by mass.

As the silica contained in the oral composition of the present disclosure, known silica used in the field of oral composition can be used. For example, precipitated silica can be used. Moreover, silica for polishing can be used. Although not particularly limited, the silica is preferably silica having an average particle size of 2 to 20 μm. The average particle size is a value measured by a laser diffraction / scattering method. Further, the silica preferably has a pH (5aq. Sol.) Of, for example, about 5.5 to 7.5 or about 6 to 7. The pH (5 aq. Sol.) Is the pH at which 5 g of silica is dispersed in 95 mL of purified water. Further, the silica preferably has an oil absorption amount (cc / 100 g) of, for example, about 10 to 500 or 20 to 400. The silica can be contained in the oral composition, for example, in an amount of about 1 to 30% by mass. The upper or lower limit of the content ratio range is, for example, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21. , 22, 23, 24, 25, 26, 27, 28, or 29% by mass. For example, the range is more preferably 2 to 25% by mass or 3 to 20% by mass.

The oral composition of the present disclosure does not cause a significant increase in viscosity even when stored at a relatively high temperature (for example, about 40 to 60 ° C.). In particular, when stored at 55 ° C. for 6 days, the difference in viscosity (Pa · s) before and after storage is preferably 300 or less in absolute value, and 250 or less, 200 or less, 150 or less in absolute value. , Or 100 or less is more preferable.

In the present specification, the viscosity of the composition is determined by keeping the composition in a constant temperature bath at 30 ° C. for 30 minutes to bring the composition to 30 ° C., and then using a B-type viscometer (manufactured by Brookfield, spindle TF, rotation speed). : 10 rpm / 1 minute).

The oral composition of the present disclosure preferably has a viscosity of 400 Pa · s or less at 30 ° C. regardless of the time since preparation, storage conditions (particularly storage temperature), and the like. In other words, the oral composition of the present disclosure preferably has a viscosity at 30 ° C. of 400 Pa · s or less, whether immediately after preparation or after storage at a relatively high temperature. Further, the viscosity may be, for example, 390, 380, 370, 360, 350, 340, 330, 320, 310, 300, 290, 280, 270, 260, or 250 Pa · s or less. The lower limit of the viscosity is not particularly limited, and examples thereof include about 10, 20, 30, 40, 50, or 60 Pa · s.

In the oral composition of the present disclosure, components other than the above that can be blended in the oral composition may be further blended alone or in combination of two or more, as long as the effect is not impaired.

For example, as a surfactant, a nonionic surfactant, an anionic surfactant or an amphoteric surfactant can be blended. Specifically, as nonionic surfactants, sugar fatty acid esters such as sucrose fatty acid ester, maltose fatty acid ester, and lactose fatty acid ester; fatty acid alkanolamides; sorbitan fatty acid ester; fatty acid monoglyceride; polyoxyethylene addition coefficient is 8 to 10. , Polyoxyethylene alkyl ether having an alkyl group having 13 to 15 carbon atoms; polyoxyethylene alkylphenyl ether having a polyoxyethylene addition coefficient of 10 to 18 and an alkyl group having 9 carbon atoms; diethyl sebacate; polyoxy Ethylene-hardened castor oil; fatty acid polyoxyethylene sorbitan and the like are exemplified. Examples of the anionic surfactant include sulfate esters such as sodium lauryl sulfate and sodium polyoxyethylene lauryl ether sulfate; sulfosuccinates such as sodium lauryl sulfosuccinate and sodium polyoxyethylene lauryl ether sulfosuccinate; sodium cocoyl sarcosin and lauroyl methyl alanine. Acylamino acid salts such as sodium; cocoyl methyl taurine sodium and the like are exemplified. Examples of the amphoteric ion surfactant include betaine acetate-type surfactants such as lauryldimethylaminoacetate betaine and coconut oil fatty acid amide propyldimethylaminoacetic acid betaine; and imidazoline-type activators such as N-cocoyl-N-carboxymethyl-N-hydroxyethylethylenediamine sodium. Activator; Amino acid type activator such as N-lauryldiaminoethylglycine and the like are exemplified. These surfactants can be blended alone or in combination of two or more. The blending amount is usually 0.1 to 5% by mass based on the total amount of the composition.

In addition, sweeteners such as saccharin sodium, acesulfame potassium, stebioside, neohesperidyl dihydrochalcone, perillartine, taumatin, aspalathylphenylalanyl methyl ester, and p-methoxycinnamic aldehyde may be blended. These can be used alone or in combination of two or more. Further, these can be blended in an amount of 0.01 to 1% by mass based on the total amount of the composition.

Further, as the wetting agent, sorbitol, glycerin, polypropylene glycol, xylit, martit, lacchit, polyoxyethylene glycol and the like can be blended alone or in combination of two or more.

As the preservative, parabens such as methylparaben, ethylparaben, propylparaben and butylparaben, sodium benzoate, phenoxyethanol, alkyldiaminoethylglycine hydrochloride and the like can be blended alone or in combination of two or more.

As a colorant, legal pigments such as Blue No. 1, Yellow No. 4, Red No. 202, and Green No. 3, mineral pigments such as ultramarine, reinforced ultramarine, and navy blue, titanium oxide, etc. are blended alone or in combination of two or more. May be good.

As the pH adjuster, citric acid, phosphoric acid, malic acid, pyrophosphate, lactic acid, tartaric acid, glycerophosphate, acetic acid, nitric acid, chemically possible salts thereof, sodium hydroxide and the like may be blended. These can be blended alone or in combination of two or more so that the pH of the composition is in the range of 4 to 8, preferably 5 to 7. For example, the blending amount of the pH adjuster is 0.01 to 2% by weight.

A bactericide may be blended as a medicinal ingredient. For example, cationic bactericides such as cetylpyridinium chloride, benzalkonium chloride, benzethonium chloride, chlorhexidine hydrochloride, chlorhexidine gluconate, amphoteric bactericides such as dodecyldiaminoethylglycine, nonionic bactericides such as triclosan and isopropylmethylphenol. Examples include hinokithiol. Furthermore, a medicinal ingredient other than the bactericide can be blended. For example, vitamin Es such as potassium nitrate, dl-α-tocopherol acetate, tocopherol succinate, or tocopherol nicotinate, sodium fluoride and the like may be blended. The medicinal ingredient can be blended alone or in combination of two or more. Since potassium nitrate is a medicinal ingredient for preventing hyperesthesia, it is particularly preferable to further add it to the oral composition of the present disclosure. In particular, when potassium nitrate is blended, it can be contained in the oral composition, for example, in an amount of about 1 to 10% by mass. The upper or lower limit of the content ratio range is, for example, 1.5, 2, 2.5, 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, 7, 7.5. , 8, 8.5, 9, or 9.5% by mass. For example, the range is more preferably 2 to 8% by mass or 3 to 7% by mass.

Further, as a base, for example, alcohols, silicon, apatite, white petrolatum, paraffin, liquid paraffin, microcrystalline wax, squalane, plastibase and the like can be added alone or in combination of two or more.

The above description of the optional component is an example, and does not limit the optional component that can be used.

In addition, in this specification, "including" also includes "consisting essentially" and "consisting of" (The term "comprising" includes "consisting essentially of" and "consisting of."). The present disclosure also includes all combinations of the constituent requirements described herein.

In addition, the various properties (property, structure, function, etc.) described for each embodiment of the present disclosure described above may be combined in any way in specifying the subject matter included in the present disclosure. That is, the present disclosure includes all subjects consisting of any combination of each combinable property described herein.

The subject matter of the present disclosure will be described in more detail below based on examples, but the subject matter of the present disclosure is not limited to these examples.

Production Example 1: Preparation of hydroxyapatite particles 10.7 mass% sodium dihydrogen phosphate / dihydrate aqueous solution and solid content concentration 8.6 mass% polished so that the Ca / P molar ratio becomes 0.5. A crushed calcium hydroxide slurry (BET specific surface area: 6.7 m ² / g oxalic acid reactivity: 15 minutes 30 seconds, JP-A-2017-036176) was prepared. An aqueous solution of sodium dihydrogen phosphate / dihydrate was placed in a stainless steel beaker and heated to 60 ° C. with stirring to maintain the stirring until the stirring was stopped. A 10% aqueous NaOH solution was added to adjust the pH to 5.5. Calcium hydroxide slurry was added thereto over 30 minutes. After completion of the addition, the mixture was further stirred for 1 hour, filtered, washed with water, and dried at 80 ° C. to obtain hydroxyapatite particles (powder).

Study example: Examination of change in viscosity of oral composition due to aluminum lactate Each component shown in Table 1 was mixed to prepare each oral composition. Caustic soda was also added to the composition containing aluminum lactate in order to adjust the pH to around 7. The numerical value of each component shown in Table 1 indicates mass%. Further, in Table 1, "Production Example 1 HAp" indicates hydroxyapatite particles obtained in the same manner as in Production Example 1, and "Commercial HAp" indicates commercially available hydroxyapatite particles (manufactured by Tomita Pharmaceutical Co., Ltd.). Further, as the "silica" in Table 1, any of five types of commercially available silica (silica a, b, c, d, e) is used, and as the "hydroxyapatite particles", Production Example 1HAp or commercially available. HAp was used or not blended. Each of these "silica" and each "hydroxyapatite particle" was combined to prepare each oral composition (see Tables 2a, 2b, and 2c). The characteristics of the five types of silica used are summarized in Table 3.

The viscosity of each of the obtained oral compositions was measured immediately after preparation. Further, a colorless transparent glass container (manufactured by Kashiwayo Glass) having a full filling amount of 83.5 mL and a body diameter of 45.5 mm is filled with 60 mL or more, and the viscosity is adjusted immediately after filling and after storage at 55 ° C. for 6 days in a dark place. It was measured. In each case, the viscosity is measured by keeping each oral composition warm for 30 minutes in a constant temperature bath at 30 ° C., and then using a B-type viscometer (Brookfield, Spindle TF, rotation speed: 10 rpm / 1 minute). It was done using. The viscosity immediately after preparation is shown in Table 2a, and the viscosity after storage at 55 ° C. for 6 days is shown in Table 2b. Further, Table 2c shows a value calculated by subtracting the viscosity value immediately after the preparation from the viscosity value after the storage. The results in Table 2c are graphed and shown in FIG.

Further, commercially available HAp was used as the hydroxyapatite particles, silica c, silica d, or silica e was used as the commercially available silica, and the amount of aluminum lactate was 0.2% by mass and the amount of 48% caustic soda was 0.1% by mass. The oral composition was prepared and stored in the same manner as above except that the storage conditions were stored at room temperature for 6 days, and the viscosity was examined. The viscosity immediately after preparation is shown in Table 4a, and the viscosity after storage at room temperature for 6 days is shown in Table 4b. Further, Table 4c shows a value calculated by subtracting the viscosity value immediately after the preparation from the viscosity value after the storage.

Claims (4)

Oral composition containing thickener, aluminum lactate, silica, and hydroxyapatite particles. The oral composition according to claim 1, wherein the thickener is at least one selected from the group consisting of alginic acid or a salt thereof, hydroxyalkyl cellulose, carboxyalkyl cellulose or a salt thereof, xanthan gum, and carrageenan. The oral composition according to claim 1, wherein the thickener is carboxymethyl cellulose or a salt thereof. The oral composition according to any one of claims 1 to 3, wherein the viscosity at 30 ° C. is 400 Pa · s or less.

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