WO2017109889A1

WO2017109889A1 - Composition for bleaching teeth and method for bleaching teeth

Info

Publication number: WO2017109889A1
Application number: PCT/JP2015/085990
Authority: WO
Inventors: 柴　肇一; 祐美川添; 義雄辻野
Original assignee: リジェンティス株式会社
Priority date: 2015-12-24
Filing date: 2015-12-24
Publication date: 2017-06-29
Also published as: JPWO2017109889A1

Abstract

Provided are: a composition for bleaching teeth, said composition being usable for bleaching teeth both in a dental office and at home and comprising agent I that contains a material serving as a carbonic acid source and agent II that contains a peroxide, and all of the agents constituting the composition being to be mixed together before using; and a method for bleaching teeth or dentures with the use of the composition.

Description

Teeth bleaching composition and tooth bleaching method

The present invention relates to a tooth bleaching composition characterized by containing a carbonic acid source substance and a peroxide and a method for bleaching a tooth by using the composition.

In recent years, the aesthetic dentistry field has been developed during dental practice. Specific examples include cleaning, bleaching (whitening), ceramic treatment, and laminate veneer treatment. Cleaning means removing stains (colored stains) on the tooth surface with a dedicated machine or instrument (such as an ultrasonic scaler), and bleaching (whitening) uses chemicals to bleach teeth by chemical action. That is, ceramic treatment is to make teeth white by shaving teeth and wearing white ceramic stuffing or covering. In addition, there is also a method to make the tooth color white by bonding a thin ceramic material called a laminate veneer, which is made to have the desired white on the tooth surface, with resin-based cement, mainly on the front tooth part. . Among these, for bleaching teeth (whitening), a bleaching composition containing hydrogen peroxide or urea peroxide, which is a peroxide, or a bleaching composition combining a peroxide and other components, Furthermore, various bleaching methods have been reported.

Patent Document 1 discloses a tooth bleaching composition containing titanium dioxide that generates a photocatalytic action by light irradiation, a compound that generates hydrogen peroxide in an aqueous solution, and a thickener. The amount of the compound that generates hydrogen peroxide in the bleaching agent composition is preferably 35% by mass or less, and the compounding amount of titanium dioxide is preferably 0.001 to 10% by mass. Further, platinum may be supported on titanium dioxide in order to improve the photocatalytic activity. Patent Document 1 describes that after the bleaching agent composition is applied to teeth, the application part is irradiated with light having a wavelength (300 nm or more) that can be absorbed by titanium dioxide to cause photocatalysis. There is. Examples of the light source include a heat lamp, a fluorescent lamp, a halogen lamp, a black light, a metal halide lamp, a xenon lamp, a mercury lamp, a UV lamp, an LED (light emitting diode), and a semiconductor laser.

Patent Document 2 discloses a dental bleaching composition comprising oxygen-based bleaching compounds such as peroxide, perborate, persulfate, percarbonate and perphosphate. Has been. This composition can further contain at least one selected from the group consisting of a thickener, phosphoric acid and condensed phosphoric acid, and / or can contain a compound capable of supplying hydrogen peroxide. Content of the compound which can supply the hydrogen peroxide of the said composition is 0.5 mass% or more as latent content of hydrogen peroxide. If the composition described in Patent Document 2 is used, it is not always necessary to irradiate the application part of the composition with teeth, and the teeth are bleached in a short time with a low concentration of peroxide. Can do.

Patent Document 3 discloses a tooth whitening composition comprising a chlorine dioxide precursor, an organic acid anhydride and an orally acceptable carrier. The whitening composition is a component that further enhances the benefits to the oral cavity and teeth, such as anticalculus agents such as phosphoric acid, pyrophosphoric acid, polyphosphoric acid, polyphosphonic acid, potassium nitrate, potassium citrate, potassium chloride, hydrogen carbonate. It may contain a desensitizing compound such as potassium or potassium oxalate.

Patent Document 4 includes hydrogen peroxide (A), bleach accelerators (B) such as alkali metal hydrogen carbonate, alkaline earth metal hydrogen carbonate, alkali metal hydrogen carbonate, and alkaline earth metal carbonate, and water. A tooth bleaching agent (D) comprising an aqueous solution in which three kinds of components of the sex thickener (C) are dissolved is disclosed. In this tooth bleaching agent (D), hydrogen peroxide (A), which is a bleaching agent, and a bleaching accelerator (B) coexist, so there is a concern about storage stability (inhibition of decomposition of hydrogen peroxide). There is. Patent Document 4 also describes that a bleaching acceleration effect can be obtained by irradiating visible light when using the tooth bleaching agent (D).

Patent Document 5 discloses a tooth bleaching composition containing a peroxide and a platinum nanocolloid and optionally containing condensed phosphoric acid or the like. This invention solves the problem that platinum, a platinum salt, or a compound carrying titanium (such as titanium oxide) precipitates without being completely dissolved when mixed with an oral composition by using a platinum catalyst as a platinum nanocolloid. To do.

Patent Document 6 discloses a linear or cyclic water-soluble polyphosphoric acid salt, hydroxyethylcellulose / dimethyldiallylammonium salt, polydimethyldiallylammonium salt, copolymer of dimethyldiallylammonium salt and acrylic vinyl monomer, etc. A composition for tooth whitening comprising a polymer compound of

International Publication No. WO01 / 001943 JP 2007-217323 A JP 2009-536935 A Japanese Patent No. 5615968 Japanese Patent Laid-Open No. 2015-98487 JP 2008-201704 A

As described above, various compositions for tooth bleaching have been proposed. However, it has not been proposed that it has excellent bleaching effect and its durability, and has no or little irritation when the composition is contained in the oral cavity.

The present inventors are a tooth bleaching composition and a bleaching method using the same, which can effectively remove stains such as pigment adhering to the tooth, and the whiteness of the tooth lasts for a long time after the removal. In order to obtain a tooth bleaching composition and a bleaching method, investigations were repeated. Moreover, the composition which is excellent in the bleaching effect but has little or no irritation was also examined. As a result of such studies, the present invention has been completed.

That is, the present invention provides a tooth bleaching composition comprising a preparation I containing a carbonic acid source substance and a preparation II containing a peroxide, and a mixture of all the preparations constituting the composition. The present invention relates to a bleaching composition. Since the carbonic acid source substance and the peroxide are mixed immediately before use, the tooth bleaching composition of the present invention is not limited to the two-part type, and may be composed of three or more parts. The present invention includes a requirement that “all the preparations constituting the composition are mixed and used”.

The tooth bleaching composition may further contain condensed phosphoric acid, a salt thereof, or a solvate thereof. That is, the preparation I or II may contain condensed phosphoric acid, a salt thereof, or a solvate thereof, or, in addition to the preparations I and II, a third preparation (formulation III) exists, The third preparation may contain condensed phosphoric acid, a salt thereof, or a solvate thereof.

The tooth bleaching composition converts the carbonic acid source material, that is, a compound capable of generating carbonate ions, to 0 in terms of the mass of the —C (═O) —O— moiety in the chemical formula of the carbonic acid source material. It is preferably contained in an amount of 2 to 20.0% by mass.

The tooth bleaching composition may contain the peroxide in an amount of 0.5 to 30.0% by mass in terms of the mass of the —O—O— moiety in the chemical formula of the peroxide. preferable.

The tooth bleaching composition preferably contains the condensed phosphoric acid, a salt thereof or a solvate thereof in an amount of 0.1 to 30.0% by mass.

In the tooth bleaching composition, a preparation other than the preparation II may further contain a platinum nanocolloid. That is, the preparation I may contain platinum nanocolloid, or, in addition to the preparations I and II, there is a third preparation (formulation III), and the third preparation contains platinum nanocolloid. May be included. The amount of the platinum nanocolloid is preferably 2 × 10 ⁻⁷ to 2 × 10 ⁻⁴ mass% in terms of the amount of platinum in the total amount of the tooth bleaching composition.

The tooth bleaching composition of the present invention includes the following embodiments:
(1) A composition for tooth bleaching comprising a preparation I containing a carbonic acid source substance and a peroxide excluding hydrogen peroxide, preferably a preparation II containing an inorganic peroxide other than hydrogen peroxide. A composition for bleaching teeth, using a mixture of all the preparations constituting the product;
(2) A tooth bleaching composition comprising a preparation I containing a carbonic acid source substance and a preparation II containing a peroxide, wherein the peroxide is represented by —O—O— in the chemical formula of the peroxide. Converted to the mass of the part, it is 1.5 to 6.5% by mass, preferably 2.0 to 6.0% by mass, more preferably 2.5 to 5.5% by mass. A tooth bleaching composition containing and using all the preparations constituting the composition; and (3) a tooth bleaching composition comprising ammonium carbonate, ammonium bicarbonate, and carbamate, and A tooth comprising: a preparation I containing at least one carbonic acid source substance selected from the group consisting of these solvates; and a preparation II containing a peroxide, wherein all preparations constituting the composition are mixed and used. Bleaching composition.

The present invention also includes the use of any of the above-described tooth bleaching compositions, a step of mixing all the preparations constituting the composition, a step of applying the obtained mixture to the teeth, and a constant amount. The present invention relates to a method for bleaching a tooth, including a step of removing a mixture applied after a lapse of time from the tooth.

After the mixture is applied to the teeth, a step of irradiating the application portion with light having a wavelength in the visible or infrared region or laser light having a long wavelength may be performed.

Furthermore, the present invention includes the use of any of the above-described tooth bleaching compositions, the step of mixing all the preparations constituting the composition, and a certain amount of the obtained mixture into the oral cavity. Or a method of bleaching a tooth, including a step of contacting a tooth surface using a container and discharging after lapse of a predetermined time or rinsing the oral cavity.

In addition, the present invention includes using any of the above-described tooth bleaching compositions, mixing all the preparations constituting the composition, and immersing the denture in the obtained mixture, The present invention relates to a method for bleaching a denture, which includes a step of taking out the denture from the mixture after a predetermined time has elapsed.

The present invention provides a tooth bleaching composition that exhibits an excellent bleaching effect and that lasts for a long period of time, and a tooth or denture bleaching method using the composition. Further, the tooth bleaching composition of the present invention containing condensed phosphoric acid, a salt thereof or a solvate thereof exhibits a higher bleaching effect.

In the tooth bleaching composition of the present invention, the bleaching effect is enhanced by the action of the carbonic acid source substance on the peroxide. Therefore, the bleaching effect is excellent even when the peroxide concentration is low, and the peroxide. Especially in the embodiment where the concentration of is low, it does not cause hypersensitivity or irritation to the gingiva.

In the tooth bleaching composition of the present invention that also contains platinum nanocolloid as a catalyst, platinum functions to promote peroxide radical generation. Since the generated radicals sterilize bacteria that cause periodontal disease, not only bleaching action but also treatment and prevention of periodontal disease can be expected.

FIG. 1 is a graph showing the methylene blue degradation over time by the tooth bleaching composition of the present invention in terms of absorbance. FIG. 2 is a graph showing the degradation rate of methylene blue over time by the tooth bleaching composition of the present invention. FIG. 3 is a graph showing the degradation of methylene blue over time by the tooth bleaching composition of the present invention in terms of absorbance. FIG. 4 is a graph showing the degradation rate of methylene blue over time by the tooth bleaching composition of the present invention.

Hereinafter, the present invention will be specifically described.

The tooth bleaching composition in the present invention includes a bleaching composition used for tooth bleaching in dentistry, a bleaching composition used for tooth bleaching at home, and a denture bleaching composition.

The tooth bleaching composition of the present invention comprises at least two preparations. The main component of Formulation I is a carbonic acid source material, and the main component of Formulation II is a peroxide. Other formulations such as Formulations I and II that make up the tooth bleaching composition of the present invention, and Formulation III, if present, are also used in admixture. Substances that react with each other should not coexist in a single formulation. In addition, preparations containing substances that react with each other should not be mixed until just before use. The form at the time of use is a mixture in which all preparations are mixed.

“Carbonate source substance” is a water-soluble chemical substance and means “a compound that generates carbonate ions when ionized in an aqueous solution”. Examples of the “carbonic acid source material” include alkali carbonates such as lithium carbonate, potassium carbonate, and sodium carbonate; alkaline earth metal carbonates such as calcium carbonate; alkali metal carbonates such as sodium bicarbonate and potassium bicarbonate Ammonium carbonate; ammonium bicarbonate; and carbamates such as ammonium carbamate; and solvates (eg, hydrates) and pharmaceutically acceptable addition salts thereof. It is preferable to use at least one selected from the group consisting of ammonium carbonate, ammonium hydrogen carbonate, and carbamates such as ammonium carbamate as the carbonic acid source material. Among these, ammonium carbonate and ammonium carbamate are particularly preferable.

The carbonic acid source material used in the tooth bleaching composition of the present invention has a —C (═O) —O— moiety in its chemical formula. The amount of the carbonic acid source material is preferably 0.2 to 20.0% by mass and more preferably 0.25 to 15.0% by mass in terms of the mass of the —C (═O) —O— moiety. It is.

“Peroxide” means an organic compound having a peroxide structure (—O—O—) or a percarboxylic acid structure (—C (═O) —O—O—) and a peroxide ion (O ₂ ²⁻ ). An inorganic compound containing Peroxides generate hydroperoxy radicals, hydroxyl radicals or oxygen radicals in aqueous solutions.

In the present invention, organic peroxides can be used, examples of which are diacetyl peroxide, dipropyl peroxide, dibutyl peroxide, dicaproyl peroxide, dilauryl peroxide, benzoyl peroxide, p, p′-dichlorobenzoyl. And peroxides, p, p'-dimethoxybenzoyl peroxide, p, p'-dimethylbenzoyl peroxide and p, p'-dinitrodibenzoyl peroxide, and pharmaceutically acceptable salts and solvates thereof. Examples of inorganic peroxides include hydrogen peroxide, hydrogen peroxide, urea peroxide (carbamide peroxide: CO (NH ₂ ) · H ₂ O ₂ ), calcium peroxide, magnesium peroxide, ammonium persulfate, Examples include potassium persulfate, potassium chlorate, potassium bromate, potassium perphosphate, perborate and percarbonate, and pharmaceutically acceptable addition salts and solvates thereof. As the peroxide, it is preferable to use hydrogen peroxide, urea peroxide, and peroxides that generate hydrogen peroxide, hydroperoxy radicals, hydroxyl radicals or oxygen radicals in an aqueous solution (for example, in the oral cavity). It is more preferable to use urea oxide and a peroxide that generates a hydroperoxy radical, a hydroxyl radical or an oxygen radical in an aqueous solution, and urea peroxide is particularly preferable.

Among the inorganic peroxides described above, in whitening (office whitening) mainly performed in a dental clinic, it is common to use a composition containing 35% by mass of hydrogen peroxide. In home whitening, it is common to use a composition containing 10 to 22% by weight of urea peroxide. Urea peroxide decomposes into hydrogen peroxide and exhibits a bleaching effect. Therefore, the bleaching action proceeds more slowly than hydrogen peroxide.

The tooth bleaching composition of the present invention preferably contains 0.5 to 30.0% by mass of a peroxide in terms of the mass of the —O—O— moiety in the chemical formula of the peroxide. More preferably, it is contained in an amount of 1.0 to 20.0% by mass, and further preferably 2.0 to 15.0% by mass. In addition, the tooth bleaching composition of the present invention having a particularly low irritation peroxide content is converted to the mass of the —O—O— moiety in the chemical formula of the peroxide. Preferably, it is contained in an amount of 1.5 to 6.5% by mass, more preferably in an amount of 2.0 to 6.0% by mass, and still more preferably in an amount of 2.5 to 5.5% by mass. .

Formulation I may consist of only a carbonic acid source substance, or alcohols and polymer compounds that do not adversely affect the tooth bleaching composition of the present invention (for example, Carbopol 940 Rubrizol (USA)) In addition, components such as a chelating agent, a stabilizer, and water may be included. Formulation II may consist only of peroxides, alcohols and polymer compounds that do not decompose peroxides (for example, Carbopol 940 Rubrizol (USA)), stabilizers, water, etc. May be included. In addition, the tooth bleaching composition of the present invention may contain Formulation III and Formulation IV. In this case, Formulation III and IV may be water or a buffer solution, or alcohol together with them. Or a polymer compound, a chelating agent, a stabilizer, and the like. Each preparation constituting the tooth bleaching composition of the present invention contains, as necessary, a thickener, a surfactant, a sweetener, an antiseptic, an active ingredient such as vitamins and minerals, a coloring agent, a fragrance, a refreshing agent, and the like. You may do.

The tooth bleaching composition of the present invention may further contain condensed phosphoric acid, a salt thereof, or a solvate thereof. Condensed phosphoric acid, a salt thereof, or a solvate thereof may be contained in any preparation.

“Condensed phosphoric acid” refers to a polymer in which two or more phosphoric acid (PO ₄ ) tetrahedra share an oxygen atom, or oxo acids thereof. "Condensed phosphoric acid" includes "polyphosphoric acid" having a linear structure, "metaphosphoric acid" having a cyclic structure or an extremely long linear structure, and "ultraphosphoric acid" having a highly branched (network) structure Is included. Furthermore, “polyphosphoric acid” includes “long-chain polyphosphoric acid”, “medium-chain polyphosphoric acid”, and “short-chain polyphosphoric acid”. Among them, short-chain polyphosphate has no antibacterial action like long-chain polyphosphate, and has effects related to FGF (cell growth factor) stabilization and functional growth like medium-chain polyphosphate. Although there is no particular effect, the removal of pigments (stains) deposited on tooth enamel and dentin physicochemically in a narrow molecular weight range and the effect of preventing deposition are recognized.

“Condensed phosphoric acid salt” means a pharmaceutically acceptable salt of condensed phosphoric acid. The salt is preferably an alkali metal salt, and more preferably a sodium salt. The salt includes not only anhydrous salts but also hydrated salts. These salts, for example, ionize in an aqueous solution and function similarly to condensed phosphoric acid. “These solvates” include solvates of condensed phosphoric acid and solvates of salts of condensed phosphoric acid, for example, hydrates.

In the condensed phosphoric acid, polyphosphoric acid can be expressed as HO [—PO ₃ H—] _n H. Polyphosphoric acid may also be represented as H _{n + 2} (P _n O _{3n + 1} ). Salts of metaphosphoric _{_{_{acid, M n + 2 (P n}}} O 3n + 1), or _(MPO ₃₎ sometimes expressed as _m.

Examples of “linear polyphosphoric acid or salt thereof” include pyrophosphoric acid having a polymerization degree (n) of 2, pyrophosphoric acid sodium, potassium pyrophosphate, tripolyphosphoric acid having n = 3, sodium tripolyphosphate, potassium tripolyphosphate, Examples include n = 4 tetrapolyphosphoric acid, sodium tetrapolyphosphate, and potassium tetrapolyphosphate. Examples of “metaphosphoric acid or a salt thereof” having a high degree of polymerization include metaphosphoric acid, sodium metaphosphate, and potassium metaphosphate.

The tooth bleaching composition of the present invention preferably contains condensed phosphoric acid, a salt thereof or a solvate thereof in an amount of 0.1 to 30.0% by mass, and 0.2 to 20.0% by mass. % Is more preferable, and it is particularly preferable that the content is 0.3 to 15.0% by mass.

Among the “condensed phosphoric acid or salts thereof” used in the present invention, ultraphosphoric acid or a salt thereof having a highly branched (network-like) structure is preferable. A preferred example of ultraphosphoric acid is ultraphosphoric acid having an average degree of polymerization of phosphoric acid of 5 to 25. Moreover, 7 or more and 20 or less may be sufficient as the average phosphoric acid polymerization degree of ultraphosphoric acid, and 7 or more and 15 or less may be sufficient as it. When ultraphosphoric acid having an average phosphoric acid polymerization degree of 7 or more and 15 or less is used, a particularly high bleaching effect can be obtained due to a synergistic effect with the peroxide.

The tooth bleaching composition of the present invention may further contain a platinum nanocolloid. Since platinum nanocolloid acts as a catalyst, it is contained in a preparation (other than preparation II) that does not contain peroxide. The amount is preferably 2 × 10 ⁻⁷ to 2 × 10 ⁻⁴ mass% in terms of “platinum” in the total amount of the tooth bleaching composition of the present invention, and 2 × 10 ⁻⁶ to 1 ×. 10 ⁻⁴ mass% is more preferable, and 1 × 10 ⁻⁵ to 6 × 10 ⁻⁵ mass% is particularly preferable.

Platinum nanocolloids are fine particles in which platinum is processed to a size of several nanometers to tens of nanometers in diameter. The platinum nanocolloid has an average particle diameter of, for example, 1 nm to 50 nm, preferably 1 nm to 10 nm, more preferably 1 nm to 5 nm, particularly preferably 1.5 nm to 2.5 nm. Further, the particle diameter of platinum nanocolloid of 90% or more is, for example, in the range of 0.1 to 10 nm, preferably 1 nm to 10 nm, more preferably 1 nm to 5 nm, and particularly preferably 1 nm to 3 nm. In the present invention, a platinum nanocolloid having an average particle size of 1 nm to 5 nm and a particle size of 90% or more of the platinum nanocolloid in the range of 0.1 to 10 nm is preferable. When platinum nanocolloid having a narrow particle size distribution is used, the platinum nanocolloid can be uniformly dispersed in the tooth bleaching composition or in the preparation constituting the composition.

As the platinum nanocolloid, a platinum nanocolloid dispersion containing sodium polyacrylate is preferably used. A polyacrylate is a colloid protective agent that improves the solvophilicity of platinum by coordinating with platinum. Therefore, the platinum nanocolloid is maintained in a uniformly dispersed state without aggregation. The R value of the platinum nanocolloid dispersion is preferably 80 to 180, more preferably 90 to 170, and particularly preferably 100 to 150. Here, the “R value” indicates “number of moles of colloid protective agent / number of moles of platinum”. When the R value is 80 to 180, the platinum nanocolloid can be maintained in a dispersed state for a long time even in an ionic solution containing cations.

Platinum platinum colloid has a large surface area of platinum, so it functions as a catalyst to enhance the bleaching effect in a small amount. Also, platinum serves to promote peroxide radical generation. As a result, the generated radicals sterilize bacteria and the like that cause periodontal disease, so that not only bleaching action but also treatment and prevention of periodontal disease can be expected. The platinum nanocolloid dispersion liquid can be prepared by a known method.

The tooth bleaching composition of the present invention is preferably such that the mixture obtained by mixing all the constituent preparations exhibits a pH value of 6-8. The tooth bleaching composition of the present invention exhibits an excellent bleaching effect even when the pH during use is neutral. Moreover, since the pH is neutral, the tooth bleaching composition of the present invention is less irritating to the gums in the oral cavity during use.

Each preparation of the tooth bleaching composition of the present invention can be produced by stirring the components contained in the preparation by a conventional method, and each preparation is enclosed in a packaging container.

The invention also relates to a method for bleaching the following teeth or dentures:
Including using the composition for tooth bleaching of the present invention, a step of mixing all preparations constituting the composition, a step of applying the obtained mixture to teeth, and a mixture applied after a certain period of time. Tooth bleaching method (1) including a step of removing from the tooth;
Including using the composition for tooth bleaching of the present invention, mixing all the preparations constituting the composition, and a certain amount of the obtained mixture in the oral cavity or using a container A method of bleaching teeth (2), comprising the step of contacting the tooth surface and exhaling after lapse of a predetermined time or rinsing the oral cavity; and using the tooth bleaching composition of the present invention, and constituting the composition A method for bleaching dentures (3), comprising a step of mixing all the preparations to be performed, and a step of immersing the denture in the obtained mixture and taking out the denture from the mixture after a predetermined time has elapsed.

In the step of mixing all the preparations constituting the tooth bleaching composition of the present invention, when the composition is composed of, for example, three kinds of preparations, the three kinds of preparations may be mixed at once just before use. Alternatively, two kinds of specific preparations may be mixed in advance, and the remaining one kind of preparation may be mixed with a mixture of the two kinds of preparation immediately before use.

The form of the mixture obtained by mixing all the preparations constituting the tooth bleaching composition is not particularly limited. The form is, for example, liquid (solution, dispersion, etc.), gel, or cream.

In the tooth bleaching method (1), for example, a liquid, gel or cream mixture is applied to the teeth using a brush, a brush, or a cloth wound around a finger. At this time, when a mouthpiece, a dental tray, or the like is used, since the preparation adheres to the tooth surface, a higher bleaching effect can be expected. Thereafter, it is allowed to stand for a certain time, for example, 5 minutes to 24 hours, preferably 20 minutes to 12 hours, more preferably 30 minutes to 2 hours. The applied mixture is then removed from the teeth by gargling or other conventional methods.

During this standing, a step of irradiating the coated portion with light having a wavelength in the visible or infrared region or laser light having a long wavelength may be performed. As the visible light to be irradiated, for example, light having a wavelength of 420 to 750 nm is preferable. In the case of irradiating infrared rays, the wavelength is 750 to 2000 nm, preferably 800 to 1500 nm, more preferably 800 to 1300 nm, and particularly preferably 850 to 1050 nm. Long-wavelength laser light having a wavelength of about 800 to 1000 nm can also be used for irradiation. The irradiation of light may be performed by irradiating either visible light or infrared light alone, or by irradiating these lights simultaneously or continuously (irradiating infrared light after irradiating visible light, Alternatively, visible light may be irradiated after irradiation with infrared light). Irradiation with infrared light warms the surface of the tooth to which the composition is applied, so that the bleaching effect can be enhanced.

The intensity of the irradiated light is, for example, 1 to 50 W, 3 to 20 W, or 5 to 10 W. The light irradiation time is 1 to 30 minutes, preferably 3 to 20 minutes, more preferably 5 to 15 minutes. In particular, when a tooth bleaching composition containing platinum nanocolloid is used, irradiation with light having a wavelength of 420 to 750 nm facilitates excitation of the platinum nanocolloid and functions more effectively as a catalyst. As a result, the tooth surface is more effectively bleached, and the time required for bleaching can be shortened.

In the tooth bleaching method (2), the liquid mixture obtained by mixing all of the constituent preparations is transferred to a container capable of spraying the liquid as it is, and then sprayed toward the tooth to obtain a certain amount. The mixture is placed in the mouth and bleached. Alternatively, use a container such as a mouthpiece or a dental tray, put the liquid mixture in such a container, bring the mixture into contact with the tooth surface, and avoid contact of the mixture with anything other than the tooth surface. I do. When such a container is used, the tooth surface can be bleached while avoiding irritation to the gum by the peroxide. A certain amount is the amount that can be contained in the oral cavity or the amount that does not spill out of the container. Thereafter, the mixture is discharged after a certain period of time, or the mouth is rinsed with gargle or the like. The certain period of time is, for example, 30 seconds to 20 minutes, preferably 1 to 10 minutes, and more preferably 1 to 2 minutes. is there.

In the denture bleaching method (3), the denture is immersed in a liquid mixture obtained by mixing all the constituent preparations, and the denture is taken out from the mixture after a predetermined time. The fixed time is, for example, the time from bedtime to wake-up, preferably 0.5 to 15 hours, more preferably 1 to 10 hours, still more preferably 1 to 5 hours, and particularly preferably 1 to 3 hours. .

Hereinafter, the present invention will be described with reference to examples, but it is needless to say that the present invention is not limited to the following examples.

(Example 1) Preparation of test tea astringent liquid Material Purified water: 110mL
Instant coffee: 5g
Black tea bags: 2 Green tea bags: 2

2. Preparation method 5 g of instant coffee, 2 tea tea bags and 2 green tea bags were put into 110 mL of purified water, and the resulting mixture was heated in a microwave for 2 minutes. Thereafter, the heated mixture was shaken at room temperature for 3 hours to overnight to dissipate heat. Thereafter, the mixture cooled to room temperature was filtered through a 200-mesh filter paper to obtain a tea astringent liquid.

(Example 2) Production of dry tea astringent apatite (1) Materials Protein solution (1% Ikuos SCP5000; manufactured by Nitta Gelatin Co.): 20 mL
Artificial saliva [20 mM HEPES, KOH (amount to be pH = 7.0), 1.5 mM CaCl ₂ , 0.9 mL KH ₂ PO ₄ ]: 20 mL
Tea astringent liquid prepared in Example 1: 20 mL
(Protein solution and artificial saliva were prepared in advance.)

(2) Manufacturing method This process was performed at room temperature unless otherwise specified.
2.5 g of hydroxyapatite (Biogel-HTP, manufactured by Biorad) was placed in a 50 mL tube, and 20 mL of protein solution was added. The resulting mixture was allowed to stand for 15 minutes, and then centrifuged (2,500 × g, 2 minutes) to remove the supernatant. Next, 20 mL of tea astringent liquid was added to the precipitated apatite after centrifugation. The obtained mixture was allowed to stand for 15 minutes, and then centrifuged again (2,500 × g, 2 minutes) to remove the supernatant. Subsequently, 20 mL of artificial saliva was added to the precipitated apatite after centrifugation. The obtained mixture was allowed to stand for 15 minutes, and further centrifuged (2,500 × g, 2 minutes). A series of operations of immersion and centrifugation in the protein solution, tea astringent fluid and artificial saliva was performed three times in total. The colored apatite thus obtained was suspended in purified water. The resulting suspension was suction filtered and collected on filter paper and dried at 40 ° C. In this way, dry tea astringent apatite was obtained. Hydroxyapatite is the main component of teeth.

(Example 3) Verification of bleaching effect by combination of carbonic acid source substance and hydrogen peroxide solution (1) Bleaching method This step was also performed at room temperature unless otherwise specified.
300 mg of the dried tea astringent apatite prepared in Example 2 was weighed, and 0.5 mL of any of the various test solutions shown in Table 1 was added thereto. The dry tea astringent apatite and various test solutions were mixed well and then allowed to stand at room temperature for 3 minutes or 10 minutes. Thereafter, apatite was precipitated by centrifugation (3,000 × g, 15 seconds). After removing the supernatant, 1 mL of purified water was added and mixed to wash the apatite. This washing with purified water was repeated a total of 3 times. The washed apatite was suspended in 200 μL of purified water, and the suspension was transferred to one well of a 96-well microtiter plate.

Note: In Table 1, “CO ₂ converted value” is the converted value to the mass of the —C (═O) —O— moiety, and “O ₂ converted value” is the mass of the —O—O— moiety. Is the conversion value. The same applies to the following tables.

(2) Evaluation Method for Stain Residual Rate A 96-well microtiter plate was scanned from the bottom with a scanner (Epson GT8300). The obtained image was inverted in gradation, and lightness (color density) was measured with Image J (image-J) (free software). The stain residual ratio was calculated from the measured brightness. The stain residual ratio was expressed as a relative color intensity, with the intensity of the color of the apatite not subjected to the bleaching treatment being 100% and the intensity of the color of the apatite not being subjected to the coloring treatment being 0%. Is.

Table 2 shows the stain residual ratio of the apatite powder from which the stain was removed using each test solution shown in Table 1.

As shown in Table 2, Test Solution 1 (a combination of ammonium carbonate carbamate and hydrogen peroxide as the carbon source material) had the highest color removal effect. On the other hand, test solutions 2 and 3 (a test solution in which the aqueous solution of hydrogen peroxide was the same concentration as test solution 1 and ammonia water or sodium hydroxide aqueous solution was added to adjust the pH value to approximately the same as test solution 1. Liquid) showed a higher stain residual ratio than when test liquid 1 was used.

(Example 4) Verification of bleaching effect by combination of carbonic acid source substance, hydrogen peroxide solution, and sodium polyphosphate Test solutions 4 to 9 shown in Table 3 were prepared. 30 mg of dried tea astringent apatite prepared by the same method as in Example 2 was weighed, and 0.5 mL of any of the prepared test solutions 4 to 9 was added to the apatite. The resulting mixture was mixed well and allowed to stand at room temperature for 3 minutes. The stain residual ratio was calculated in the same manner as in Example 3. Verification using this test solution was performed three times independently, and the results are shown in Table 4. Table 4 also shows the average value and standard deviation in addition to the results of each test.

As shown in Table 4, test solution 7 (a combination of ammonium carbamate, hydrogen peroxide solution and sodium polyphosphate) had the highest color removal effect, and the stain remaining rate was 30.96% after 3 minutes of treatment. . In addition, test solutions 5 and 6 (a test solution having the same concentration of hydrogen peroxide as test solution 4 and adjusted to a pH value approximately equal to that of test solution 4 by adding aqueous ammonia or sodium hydroxide solution) When the test solutions 8 and 9 (test solution obtained by adding sodium polyphosphate to the test solutions 5 and 6) were compared, the test solutions 8 and 9 showed lower stain residual ratio than the test solutions 5 and 6. However, the color removal effect of the test solutions 8 and 9 did not reach the color removal effect of the test solution 7 which is a combination of ammonium carbamate, hydrogen peroxide solution and sodium polyphosphate.

(Example 5) Verification of optimum concentration of ammonium carbamate Test liquids 10 to 19 were prepared in which the amount of hydrogen peroxide solution was kept constant and the concentration of ammonium carbamate was arbitrarily changed. Table 5 shows the formulations of the test solutions 10 to 19. 25 mg of dried tea astringent apatite prepared by the same method as in Example 2 was weighed, and 0.5 mL of any of test solutions 10 to 19 was added to the apatite. The resulting mixture was mixed well and allowed to stand at room temperature for 3 minutes. Then, the stain residual ratio was calculated by the same method as in Example 3. The results are shown in Table 6.

As is clear from Table 6, the bleaching effect tended to increase as the concentration of ammonium carbamate was increased. In particular, when the test solution 18 (concentration of ammonium carbamate: 20% by mass; CO ₂ conversion value = 11.3% by mass), a stain remaining rate of 39.67% was obtained with a 3-minute treatment. It was. In the test solution 19, since the undissolved ammonium carbamate was generated, the pH and the stain residual ratio could not be measured.

The pH increased slightly as the concentration of ammonium carbamate was increased. However, when test solutions having the same pH value were compared, it was considered that the higher the ammonium carbamate concentration, the lower the stain residual rate, so that there was almost no influence of pH on the increase in the bleaching effect.

(Example 6) Verification of bleaching effect due to difference in concentration of short-chain sodium polyphosphate and sodium ultraphosphate The degree of phosphoric acid polymerization of 7 to 15 phosphate residues in ammonium carbamate, hydrogen peroxide water and purified water Test solutions 20 to 25 were prepared by adding short-chain sodium polyphosphate mainly containing molecules or sodium ultraphosphate mainly containing molecules of phosphoric acid residues having a phosphoric acid polymerization degree of 5 to 15. Table 7 shows the formulations of the test solutions 20 to 25. 25 mg of dried tea astringent apatite prepared by the same method as in Example 2 was weighed, and 0.5 mL of any of the prepared test solutions 20 to 25 was added to the apatite. The resulting mixture was mixed well and allowed to stand at room temperature for 3 minutes. Thereafter, the stain residual ratio was calculated in the same manner as in Example 3. The results are shown in Table 8.

From Table 8, in addition to ammonium carbamate and hydrogen peroxide, the addition of short-chain sodium polyphosphate or sodium ultraphosphate significantly improved the bleaching effect. When comparing short-chain sodium polyphosphate and sodium ultraphosphate, it was found that the bleaching effect was higher when sodium ultraphosphate was added. Regarding the treatment concentration, in the case of the short-chain sodium polyphosphate, the test solution 21 having the concentration of 4% by mass was most effective, and the effect was not increased at the concentration of 8% by mass (test solution 22). With respect to sodium ultraphosphate, the bleaching effect increased in a concentration-dependent manner, and in the case of the test solution 25 having a concentration of 8% by mass, the stain residual ratio was 2.80%, and the bleaching effect was the highest. Therefore, it was found that sodium ultraphosphate is more effective than short-chain sodium polyphosphate for enhancing the bleaching effect by mixing ammonium carbamate and hydrogen peroxide.

(Example 7) Verification of bleaching effect by addition of platinum nanocolloid Ammonium carbamate, hydrogen peroxide solution, short-chain sodium polyphosphate mainly containing phosphoric acid residue molecules having a phosphoric acid polymerization degree of 7 to 15 and purification Platinum nanocolloid (the stock solution contains 0.02% by mass of platinum) was added to water to prepare test solutions 27 to 29. As a control, a test solution 26 containing no platinum nanocolloid was also prepared. Table 9 shows the formulations of the test solutions 26 to 29. 25 mg of dried tea astringent apatite prepared by the same method as in Example 2 was weighed, and 0.5 mL of any of test solutions 26 to 29 was added to the apatite. The resulting mixture was mixed well and allowed to stand at room temperature for 3 minutes. Thereafter, the stain residual ratio was calculated in the same manner as in Example 3. The results are shown in Table 10.

Test solution 28 containing 2 × 10 ⁻⁵ mass% of platinum showed the most excellent bleaching effect. The test solution 29 with a platinum content of 2 × 10 ⁻⁴ mass% was inferior to the control (test solution 26) in the bleaching effect, so it was assumed that the platinum content had an appropriate value.

(Example 8) Verification of bleaching effect by combination of urea peroxide and carbonic acid source material Combination of urea peroxide (powder) and ammonium carbamate, and bleaching effect when short-chain sodium polyphosphate is further added thereto Verified. Test solutions 30 to 40 shown in Table 11 were prepared. 25 mg of dried tea astringent apatite produced by the same method as in Example 2 was weighed, and 0.5 mL of any of test solutions 30 to 40 was added to the apatite. The resulting mixture was mixed well and allowed to stand at room temperature for 3 minutes. Thereafter, the stain residual ratio was calculated in the same manner as in Example 3. The results are shown in Table 12.

Test solutions 30 and 31 are controls containing no bleaching component, and test solutions 32 to 34 are controls containing only the bleaching component. Even when the peroxide was changed to urea peroxide, the bleaching effect increased depending on the concentration of the peroxide due to the combination with the carbonate source material ammonium carbamate (test solutions 35 to 37). Further, the bleaching effect was further improved by adding short-chain polyphosphoric acid (test solutions 38 to 40).

(Example 9) Comparison of bleaching effect by various carbonic acid source materials In order to verify the level of bleaching effect by the type of carbonic acid source material, test solutions 41 to 46, 48 and 49 using various carbonic acid source materials were prepared. . As a comparative example, a test solution 47 containing ammonium sulfate was prepared as a control, and a test solution 50 containing no carbonic acid source material was prepared as a control. Table 13 shows the formulations of the test solutions 41 to 50. 25 mg of dried tea astringent apatite prepared by the same method as in Example 2 was weighed, and 0.5 mL of any of test solutions 41 to 50 was added to the apatite. The resulting mixture was mixed well and allowed to stand at room temperature for 3 minutes. Thereafter, the stain residual ratio was calculated in the same manner as in Example 3. The results are shown in Table 14.

As is clear from Table 14, when a potassium salt or an ammonium salt was used as the carbonic acid source material (test solutions 41, 43, 46 and 49), a high bleaching effect was obtained. When ammonium sulfate, which is not a carbonic acid source material, was used (test solution 47), almost no bleaching effect was observed. Therefore, the presence or absence of carbonate ions in the test solution is necessary to develop or promote the bleaching effect. So I thought.

(Example 10) Comparison of bleaching effect From the results obtained in Example 9, two kinds of potassium hydrogen carbonate and ammonium carbamate, which had a high bleaching effect, were selected as carbonic acid source materials. Test solutions 52 containing potassium hydrogen carbonate and hydrogen peroxide and test solutions 53 to 55 to which short-chain sodium polyphosphate or sodium ultraphosphate was further added were prepared. Test solutions 56 containing ammonium carbamate and hydrogen peroxide and test solutions 57 to 59 to which short-chain sodium polyphosphate or sodium ultraphosphate was further added were also prepared. A control test solution 51 containing only hydrogen peroxide was also prepared. Table 15 shows the formulations of the test solutions 51 to 59.

25 mg of dry tea astringent apatite prepared by the same method as in Example 2 was weighed, and 0.5 mL of any of test solutions 51 to 59 was added to the apatite. The resulting mixture was mixed well and allowed to stand at room temperature for 3 minutes. Thereafter, the stain residual ratio was calculated in the same manner as in Example 3. The results are shown in Table 16.

Hydrogen peroxide added with ammonium carbamate and sodium ultraphosphate (test solutions 58 and 59) showed a markedly high bleaching effect, and the stain residual ratio was 0.00% and 0.60%, respectively. It was. A high bleaching effect was also obtained when short-chain sodium polyphosphate was used instead of sodium ultraphosphate (test solution 57). Even when potassium hydrogen carbonate was used as the carbonic acid source material, a high bleaching effect was obtained by using short-chain sodium polyphosphate or sodium ultraphosphate together (test solutions 53 to 55).

(Example 11) Promotion test of decolorization reaction of methylene blue (1)
Using a combined system of urea peroxide and a carbon source material (potassium hydrogen carbonate), the bleaching effect was evaluated using the decolorization reaction of methylene blue as an index.
0.5% by mass aqueous solution of methylene blue (manufactured by Kanto Chemical Co., Ltd., special grade reagent), 32% by mass aqueous solution of potassium bicarbonate (made by Wako Pure Chemical Industries, Ltd., special grade reagent), and urea peroxide (manufactured by Sigma Aldrich Japan Co., Ltd. , Reagents) 30.8 mass% aqueous solution was prepared respectively.

Experiments were performed using test solutions 60 and 61 shown in Table 17. First, components other than the urea peroxide aqueous solution were mixed among the components of the test solution. Subsequently, urea peroxide aqueous solution was added, and the obtained test solution was immediately put into a 37 ° C. incubator to start the reaction. A part was taken from the test solution immediately after the start of the reaction and every certain time, and it was diluted 20-fold with purified water, and the absorbance was measured at a wavelength of 660 nm (see Table 18 and FIG. 1). FIG. 2 shows the methylene blue decomposition rate calculated from the measured absorbance values in Table 18. Methylene blue exhibits maximum absorption near a wavelength of 660 nm, but becomes colorless by undergoing oxidative decomposition due to a hydroxyl radical, and the absorbance at the wavelength disappears. Therefore, a decrease in absorbance at this wavelength can be regarded as decomposition of methylene blue.

As apparent from Table 18 and FIG. 1, the absorbance at a wavelength of 660 nm decreased with time in the test solution 60, which is a combination of urea peroxide and potassium bicarbonate, which is a carbonate source material. On the other hand, in the test solution 61 containing no potassium hydrogen carbonate, the absorbance did not change substantially. From this, it can be inferred that the generation of hydroxyl radicals from urea peroxide was promoted by potassium bicarbonate. In the test solution 60, the decomposition rate of methylene blue was about 40% 30 minutes after the start of the reaction, and the decomposition rate increased over time. About 180% of methylene blue was decomposed 180 minutes after the start of the reaction (see FIG. 2).

(Example 12) Acceleration test of decolorization reaction of methylene blue (2)
Using a combined system of urea peroxide and a carbonic acid source substance (ammonium carbamate), the bleaching effect was evaluated using the decolorization reaction of methylene blue as an index.
0.5% by mass aqueous solution of methylene blue (manufactured by Kanto Chemical Co., Ltd., special grade reagent), 32% by mass aqueous solution of ammonium carbamate aqueous solution (special grade reagent, manufactured by Wako Pure Chemical Industries, Ltd.), and urea peroxide (Sigma Aldrich Japan Co., Ltd.) 30.7% by mass aqueous solution (manufactured by Reagent).

Experiments were performed using test solutions 62 and 63 shown in Table 19. First, components other than the urea peroxide aqueous solution were mixed among the components of the test solution. Subsequently, urea peroxide aqueous solution was added, and the obtained test solution was immediately put into a 37 ° C. incubator to start the reaction. A part was taken from the test solution immediately after the start of the reaction and every certain time, and it was diluted 20-fold with purified water, and the absorbance was measured at a wavelength of 660 nm (see Table 20 and FIG. 3). FIG. 4 shows the methylene blue decomposition rate calculated from the measured absorbance values in Table 20.

As is clear from Table 20 and FIG. 3, the absorbance at a wavelength of 660 nm decreased with time in the test liquid 62 which was a combination of urea peroxide and ammonium carbamate, which is a carbon source material. On the other hand, in the test solution 63 containing no ammonium carbamate, the absorbance decreased in the first 30 minutes, but no change was observed thereafter. From this, it can be inferred that the generation of hydroxyl radicals from urea peroxide was promoted by ammonium carbamate. In the test solution 62, the decomposition rate of methylene blue was about 20% 30 minutes after the start of the reaction, and the decomposition rate increased with the passage of time thereafter. About 180% of methylene blue was decomposed 180 minutes after the start of the reaction (see FIG. 4).

(Example 13: Formulation example 1)
Table 21 below shows formulation examples of the tooth bleaching composition of the present invention using potassium hydrogen carbonate as a carbon source material. In this method, the agent I and the agent II are mixed at a ratio of 1: 1 (volume ratio).

(Example 14: Formulation example 2)
Table 22 below shows formulation examples of the tooth bleaching composition of the present invention using ammonium carbamate as the carbonic acid source material. In this method, the agent I and the agent II are mixed at a ratio of 1: 1 (volume ratio).

Claims

A composition for tooth bleaching, comprising a preparation I containing a carbonic acid source substance and a preparation II containing a peroxide, wherein all the preparations constituting the composition are mixed and used.
The tooth bleaching composition according to claim 1, wherein the tooth bleaching composition further comprises condensed phosphoric acid, a salt thereof, or a solvate thereof.
The tooth bleaching composition according to claim 1 or 2, wherein the peroxide is a peroxide other than hydrogen peroxide.
The composition for tooth bleaching according to claim 1 or 2, wherein the peroxide is an inorganic peroxide other than hydrogen peroxide.
In the tooth bleaching composition, the carbonic acid source material is converted to the mass of the —C (═O) —O— moiety in the chemical formula of the carbonic acid source material in an amount of 0.2 to 20.0% by mass. The composition for tooth bleaching as described in any one of Claims 1 thru | or 4 containing.
The tooth according to any one of claims 1 to 5, wherein the carbonic acid source material is at least one selected from the group consisting of ammonium carbonate, ammonium hydrogen carbonate, carbamate, and solvates thereof. Bleaching composition.
The tooth bleaching composition contains the peroxide in an amount of 0.5 to 30.0% by mass in terms of the mass of the —O—O— moiety in the chemical formula of the peroxide. Item 7. The tooth bleaching composition according to any one of Items 1 to 6.
The tooth bleaching composition contains the peroxide in an amount of 1.5 to 6.5% by mass in terms of the mass of the —O—O— moiety in the chemical formula of the peroxide. Item 7. The tooth bleaching composition according to any one of Items 1 to 6.
9. The tooth bleaching composition according to any one of claims 2 to 8, wherein the condensed phosphoric acid, a salt thereof, or a solvate thereof is contained in an amount of 0.1 to 30.0% by mass. Tooth bleaching composition.
The tooth bleaching composition according to any one of claims 1 to 9, wherein the tooth bleaching composition further comprises a platinum nanocolloid.
11. The tooth bleaching composition according to claim 10, wherein the tooth bleaching composition contains the platinum nanocolloid in an amount of 2 × 10 −7 to 2 × 10 −4 mass% in terms of the amount of platinum. .
Using the composition for tooth bleaching according to any one of claims 1 to 11, mixing all the preparations constituting the composition, applying the obtained mixture to teeth; and A method for bleaching a tooth, comprising a step of removing a mixture applied after a certain period of time from a tooth.
The tooth bleaching method according to claim 12, wherein after the mixture is applied to a tooth, a step of irradiating the application portion with light having a wavelength in a visible or infrared region or laser light having a long wavelength is performed.
A step of mixing all the preparations comprising the composition, comprising using the tooth bleaching composition according to any one of claims 1 to 11, and determining a certain amount of the obtained mixture from the oral cavity A method for bleaching a tooth, which comprises a step of containing the inside or contacting a tooth surface using a container, and vomit or rinse the oral cavity after a lapse of a predetermined time.
Using the composition for tooth bleaching according to any one of claims 1 to 11, a step of mixing all the preparations constituting the composition, and immersing the denture in the obtained mixture; A method for bleaching a denture, comprising a step of taking out the denture from the mixture after a predetermined time has elapsed.