JP2009263268A - Composition for reforming tooth interprismatic space - Google Patents
Composition for reforming tooth interprismatic space Download PDFInfo
- Publication number
- JP2009263268A JP2009263268A JP2008113465A JP2008113465A JP2009263268A JP 2009263268 A JP2009263268 A JP 2009263268A JP 2008113465 A JP2008113465 A JP 2008113465A JP 2008113465 A JP2008113465 A JP 2008113465A JP 2009263268 A JP2009263268 A JP 2009263268A
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- JP
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- Prior art keywords
- composition
- mass
- enamel
- teeth
- tooth
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- Granted
Links
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Landscapes
- Cosmetics (AREA)
Abstract
Description
本発明は、歯の小柱間隙再形成用組成物に関する。 The present invention relates to a composition for remodeling the trabecular space of teeth.
人の歯の着色は、歯石や歯垢、喫煙、又はコーヒー若しくはお茶等の習慣的飲食等により歯面に着色物が付着する外因性着色と、加齢や外傷等によって着色した象牙質の色がエナメル質から透けて見える場合、又は、歯の形成期にテトラサイクリン等の薬剤の使用によりエナメル質も着色した場合等の内因性着色に依存する。従って、歯を根本的に白くするためには、外因性着色のみならず内因性着色にも対応する必要がある。 The coloring of human teeth can be exogenous coloring, such as calculus, plaque, smoking, or customary eating and drinking such as coffee or tea, and the color of dentin colored by aging or trauma. Depends on intrinsic coloring, such as when the enamel is visible through the enamel or when the enamel is colored by the use of a drug such as tetracycline during the tooth formation. Therefore, in order to fundamentally whiten teeth, it is necessary to deal with not only exogenous coloring but also intrinsic coloring.
従来、歯を白くするための手段としては、種々の物理的又は化学的方法が報告されている。物理的方法としては研磨除去による他に、n−ブチルエーテルやブチルブチレート等を用いて着色物を除去する方法(特許文献1、特許文献2)、或いは、セラミックベニヤ等を用いて歯を被覆し色調を改善する方法がある。化学的方法としては、ヒドロキシアパタイトを配合した口腔用組成物により再石灰化を促進する方法(特許文献3、特許文献4)、過酸化物を用いて酸化漂白する方法(特許文献5)、過酸化物に自己硬化性リン酸カルシウム化合物及びフッ素化合物等を配合した歯美白組成物を用いる方法(特許文献6)、液状化リン酸カルシウム系化合物を含有する口腔用組成物によりエナメル質の再石灰化を促進する方法(特許文献7)等が知られている。 Conventionally, various physical or chemical methods have been reported as means for whitening teeth. As a physical method, in addition to polishing removal, n-butyl ether, butyl butyrate, or the like is used to remove the colored material (Patent Document 1, Patent Document 2), or a ceramic veneer is used to coat the teeth. There are ways to improve color tone. As chemical methods, a method for promoting remineralization with an oral composition containing hydroxyapatite (Patent Document 3, Patent Document 4), an oxidative bleaching method using a peroxide (Patent Document 5), A method using a tooth whitening composition in which a self-curing calcium phosphate compound and a fluorine compound are mixed with an oxide (Patent Document 6), and an oral composition containing a liquefied calcium phosphate compound promotes remineralization of enamel. A method (Patent Document 7) and the like are known.
しかし、セラミックベニヤ等を用いる方法は歯質を削除する必要があり、この方法の使用には歯科医による指導や処置が必要である。また、過酸化物を用いて酸化漂白する方法は、歯の酸化漂白が可能な高濃度の過酸化物を用いる必要があるため、専門家の指導に従って慎重に行う必要がある。しかし、専門家の指導の下でも、過酸化物により歯と歯茎へのダメージや知覚過敏を発生する場合がある。 However, the method using ceramic veneer or the like needs to delete the tooth substance, and the use of this method requires guidance and treatment by a dentist. In addition, the method of oxidative bleaching using a peroxide requires the use of a high-concentration peroxide capable of oxidative bleaching of the teeth, and therefore needs to be performed carefully in accordance with the guidance of an expert. However, even under the guidance of specialists, damage to teeth and gums and hypersensitivity may occur due to peroxides.
一方、ヒドロキシアパタイト等のリン酸カルシウム系化合物を用いて歯の再石灰化を促進する方法は、主に、エナメル質表面をアパタイトにより補修することにより歯を健常化するものであり、美白効果については充分といえない。
本発明の目的は、歯に優れた美白効果を与える組成物を提供することを目的とする。 An object of the present invention is to provide a composition that gives an excellent whitening effect to teeth.
歯のエナメル質は、エナメル小柱と呼ばれるヒドロキシアパタイトの多結晶で構成された柱状物が集まって構成されている。一般的には若年期において、このエナメル質のエナメル小柱とエナメル小柱の間に空間(隙間)、すなわち、小柱間隙が存在し、水や唾液成分等で満たされている。この様な歯においては、エナメル質への入射光はエナメル小柱と小柱間隙の空間との大きな屈折率の差により散乱し、歯は白く見える。
しかし、例えば加齢等により歯のエナメル質表層の小柱間隙に唾液中に溶けた物質が沈積し続けると、この小柱間隙は埋まり、その結果、エナメル小柱と小柱間隙の屈折率の差が小さくなるため、エナメル質は透明性があがり入射光がエナメル質の深部に位置する黄色ないし褐色である象牙質まで達しやすくなり、歯は黄色く見えるようになる。
そこで、本発明者等は、歯のエナメル質表層の小柱間隙に存在する物質(以下「小柱間隙物質」という)を小柱間隙から選択的に取り除くことによって、エナメル質を形成しているエナメル小柱そのものへのダメージを抑えつつ小柱間隙を再形成し、小柱間隙の空間による光散乱によってエナメル質の内部からの反射光を増加させると、自然な白い歯を得ることができると考えた。
そして、さらに、種々検討を行った結果、フィチン酸に、失われた小柱間隙を再形成させる作用があることを見出し、本発明を完成するに至った。
The enamel of a tooth is made up of a collection of columnar bodies made of hydroxyapatite polycrystals called enamel trabeculae. In general, in the youth, a space (gap), that is, a trabecular space exists between the enamel trabeculae and the enamel trabeculae, and is filled with water, saliva components, and the like. In such a tooth, the incident light to the enamel is scattered due to a large difference in refractive index between the enamel trabeculae and the space between the trabeculae, and the teeth appear white.
However, if the substance dissolved in saliva continues to accumulate in the trabecular space of the tooth enamel surface, for example due to aging, the trabecular space is filled, and as a result, the refractive index of the enamel trabecular space is smaller than that of the trabecular space. As the difference becomes smaller, the enamel becomes more transparent and incident light tends to reach the dentin, which is yellow or brown, located deep in the enamel, and the teeth appear yellow.
Therefore, the present inventors have formed enamel by selectively removing from the trabecular space a material (hereinafter referred to as “trabecular space material”) present in the trabecular space of the tooth enamel surface layer. By re-forming the trabecular gap while suppressing damage to the enamel trabecula itself, and increasing the reflected light from the inside of the enamel by light scattering by the space of the trabecular gap, natural white teeth can be obtained Thought.
Further, as a result of various studies, it was found that phytic acid has an action of re-forming the lost trabecular space, and the present invention has been completed.
すなわち、本発明は、フィチン酸又はその塩を0.05〜18質量%含有し、水で30質量%に希釈したときのpHが5.5〜6.5である歯の小柱間隙再形成用組成物を提供するものである。
また、本発明は、フィチン酸又はその塩を0.05〜18質量%含有し、水で30質量%に希釈したときにpHが5.5〜6.5である口腔用組成物を歯に適用することを特徴とする、歯の小柱間隙物質の除去方法を提供する。
That is, the present invention contains 0.05 to 18% by mass of phytic acid or a salt thereof, and re-forms the trabecular space of a tooth having a pH of 5.5 to 6.5 when diluted to 30% by mass with water. The composition for use is provided.
Moreover, this invention contains 0.05-18 mass% of phytic acid or its salt, and when diluted to 30 mass% with water, the composition for oral cavity whose pH is 5.5-6.5 is used for a tooth | gear. A method for removing a trabecular bone material of a tooth is provided.
本発明の組成物を歯に適用すれば、加齢等によって生じた小柱間隙物質を選択的に除去し、失われた小柱間隙が再形成されるため、歯の内部から歯の着色を防止し、又は歯の内部から歯を白くすることができる。また、歯のエナメル質へのダメージを抑えつつ歯の内因性着色に対して高い美白効果を得ることが可能である。これにより、日常の口腔の手入れ又はチューインガムの愛用等、繰り返しの使用を通じて、手軽に歯を美白することができる。 When the composition of the present invention is applied to teeth, the trabecular space material generated by aging and the like is selectively removed, and the lost trabecular space is re-formed. Preventing or whitening teeth from inside the teeth. In addition, it is possible to obtain a high whitening effect on the intrinsic coloring of the tooth while suppressing damage to the enamel of the tooth. Thereby, it is possible to easily whiten teeth through repeated use such as daily oral care or regular use of chewing gum.
本発明の小柱間隙再形成用組成物の有効成分はフィチン酸又はその塩である。フィチン酸は、別名myo−イノシトール6リン酸ともいい、リン酸化合物である。種々のリン酸化合物の中で、小柱間隙の再形成作用とエナメル質へのダメージの両者を考慮した場合、フィチン酸又はその塩が特に優れている。
その塩としては、ナトリウムやカリウム等のアルカリ金属塩やアンモニウム塩等が挙げられる。
The active ingredient of the composition for remodeling the trabecular cavity of the present invention is phytic acid or a salt thereof. Phytic acid is also called myo-inositol hexaphosphate and is a phosphate compound. Among various phosphoric acid compounds, phytic acid or a salt thereof is particularly excellent when considering both the remodeling action of trabecular space and damage to enamel.
Examples of the salt include alkali metal salts such as sodium and potassium, ammonium salts, and the like.
本発明の小柱間隙再形成用組成物は、フィチン酸又はその塩を当該組成物中に0.05質量%〜18質量%含有するものである。
本発明の小柱間隙再形成効果を十分に発揮する観点から、フィチン酸又はその塩を当該組成物中に0.05質量%以上、好ましくは0.1質量%以上含むものであり、歯の脱灰を抑制する観点、味やきしみの観点から18質量%以下、好ましくは10質量%以下含むものである。尚、本発明の小柱間隙再形成用組成物におけるフィチン酸又はその塩の含有量は、水酸化カリウム又は水酸化ナトリウムで中和して測定し、全量を酸に換算したものを採用する。
The trabecular cavity re-forming composition of the present invention contains phytic acid or a salt thereof in an amount of 0.05% by mass to 18% by mass.
From the viewpoint of sufficiently exerting the trabecular space re-forming effect of the present invention, phytic acid or a salt thereof is contained in the composition in an amount of 0.05% by mass or more, preferably 0.1% by mass or more. From the viewpoint of suppressing decalcification and from the viewpoint of taste and squeakiness, the content is 18% by mass or less, preferably 10% by mass or less. In addition, the content of phytic acid or a salt thereof in the composition for re-forming the trabecular space of the present invention is measured by neutralizing with potassium hydroxide or sodium hydroxide, and the total amount is converted to an acid.
本発明の小柱間隙再形成用組成物は、水で30質量%に希釈したときのpHが5.5〜6.5である。
すなわち、当該組成物を口腔内に適用した際に小柱間隙物質を除去し、かつ歯の表面の脱灰を抑制し、歯の表面の凸凹形成を抑制する観点、つまり小柱間隙物質を選択的に除去する観点から、当該組成物を水で30質量%に希釈したときのpHを5.5以上、さらに5.8以上とすることが好ましく、小柱間隙の形成による光散乱効果を十分に奏する観点から当該pHを6.5以下、さらに6.2以下とすることが好ましい。
当該pHは、例えば練り歯磨きのように粘度の高い口腔用組成物の場合に正確にpHを測定できないことから、当該組成物を水で30質量%に希釈したものを当該組成物のpHとしている。水で30質量%に希釈したものを採用したのは、当該組成物の口腔内に適用した状態と想定したものである。
組成物のpHを上記範囲に調整するには、pH調整剤を用いるのが好ましく、当該pH調整剤としては、フィチン酸による小柱間隙再形成効果を阻害せず、歯の脱灰を抑制できる範囲で、酢酸、フマル酸、リンゴ酸、乳酸、グルコン酸、酒石酸等の有機酸塩、フィチン酸以外のリン酸(例えば、オルトリン酸)、塩酸、硫酸等の無機酸塩、水酸化ナトリウム等の水酸化物、アンモニア又はアンモニア水、低級アルカノールアミン類、アルギニン、リジン等の塩基性アミノ酸等が挙げられ、これらを単独で又は2種以上組み合わせて用いてもよい。
The trabecular cavity re-forming composition of the present invention has a pH of 5.5 to 6.5 when diluted to 30% by mass with water.
That is, when the composition is applied to the oral cavity, the trabecular crevice material is removed, the decalcification of the tooth surface is suppressed, and the formation of irregularities on the tooth surface is suppressed, that is, the trabecular crevice material is selected. From the viewpoint of removal, the pH when the composition is diluted to 30% by mass with water is preferably 5.5 or more, more preferably 5.8 or more, and the light scattering effect due to the formation of the trabecular space is sufficient. From the viewpoint of achieving the above, it is preferable that the pH is 6.5 or less, more preferably 6.2 or less.
Since the pH cannot be accurately measured in the case of a highly viscous oral composition such as toothpaste, the pH of the composition is determined by diluting the composition to 30% by mass with water. . What was diluted to 30% by mass with water was assumed to be applied to the oral cavity of the composition.
In order to adjust the pH of the composition to the above range, it is preferable to use a pH adjusting agent, and the pH adjusting agent can suppress decalcification of teeth without inhibiting the trabecular space re-forming effect by phytic acid. In range, organic acid salts such as acetic acid, fumaric acid, malic acid, lactic acid, gluconic acid, tartaric acid, phosphoric acid other than phytic acid (for example, orthophosphoric acid), inorganic acid salts such as hydrochloric acid, sulfuric acid, sodium hydroxide, etc. Examples include hydroxides, ammonia or aqueous ammonia, lower alkanolamines, basic amino acids such as arginine and lysine, and these may be used alone or in combination of two or more.
本発明の小柱間隙再形成用組成物は、多価カチオンの含有量を低く抑えることが好ましい。多価カチオンは、フィチン酸を不溶性にしたり小柱間隙物質の除去効果を低下させるため、当該効果の低下を防止するためである。その含有量はICP発光分析法(ICP発光分析装置:Perkin Elmer社 Optima 5300DV)で測定して100ppm以下であることが好ましい。すなわち、アルミニウム、カルシウム、マグネシウム、鉄、亜鉛等の多価カチオンを主に供給する剤は配合しないことが望ましく、多価カチオンを実質的にほとんど含まないものが好ましい。 In the trabecular cavity re-forming composition of the present invention, the content of polyvalent cations is preferably kept low. This is because the polyvalent cation makes phytic acid insoluble or reduces the effect of removing the trabecular crevice substance, thereby preventing the reduction of the effect. The content is preferably 100 ppm or less as measured by ICP emission analysis (ICP emission analyzer: Optima 5300DV, manufactured by Perkin Elmer). That is, it is desirable not to add an agent that mainly supplies polyvalent cations such as aluminum, calcium, magnesium, iron, and zinc, and those that substantially do not contain polyvalent cations are preferable.
また、本発明の小柱間隙再形成用組成物には、フィチン酸又はその塩による小柱間隙の再形成効果を阻害しない範囲(含有量、剤形等)でフッ化ナトリウム、フッ化カリウム、フッ化アンモニウム、モノフルオロリン酸ナトリウム等のフッ化物を配合してもよい。フッ化物は、当該組成物中に0.01〜0.5質量%、さらに0.02〜0.2質量%含有するのが好ましい。 Further, the composition for remodeling the trabecular space of the present invention includes sodium fluoride, potassium fluoride, and the like within a range (content, dosage form, etc.) that does not inhibit the remodeling effect of the trabecular space by phytic acid or a salt thereof. Fluoride such as ammonium fluoride and sodium monofluorophosphate may be blended. The fluoride is preferably contained in the composition in an amount of 0.01 to 0.5% by mass, and more preferably 0.02 to 0.2% by mass.
本発明の小柱間隙再形成用組成物には、前記成分の他、例えば発泡剤、発泡助剤、研磨剤、湿潤剤、粘稠剤、ゲル化剤、粘結剤、増量剤、甘味剤、保存料、殺菌剤、薬効成分、粘着剤、顔料、色素、香料等を適宜含有させ、種々の剤形に応じた常法により当該組成物を製造することができる。また、従来用いられた美白成分であるポリエチレングリコールなどの併用も制限されない。 In addition to the above components, the composition for re-forming the trabecular space of the present invention includes, for example, a foaming agent, a foaming aid, an abrasive, a wetting agent, a thickening agent, a gelling agent, a binder, a bulking agent, and a sweetening agent. In addition, preservatives, bactericides, medicinal ingredients, pressure-sensitive adhesives, pigments, dyes, fragrances and the like can be appropriately contained, and the composition can be produced by conventional methods according to various dosage forms. Moreover, combined use, such as polyethylene glycol which is a conventionally used whitening component, is not limited.
本発明の小柱間隙再形成用組成物は、例えば溶液状、ゲル状、ペースト状といった剤形に調製され、粉歯磨剤、潤性歯磨剤、練り歯磨剤、液状歯磨剤、洗口剤等の口腔用組成物、或いは、チューインガム、トローチ、キャンディ等の食品として用いたり、シート材や、布、繊維等に含浸させたものをデンタルフロス等の口腔衛生器具として用いることができる。
それらどの剤形においてもポリエチレングリコール、プロピレングリコール、グリセリン、ソルビトール、マルチトール、キシリトール、ラクチトール、エリスリトール等を湿潤剤あるいは粘稠剤等の目的で含有させることができる。
The trabecular cavity re-forming composition of the present invention is prepared in a dosage form such as a solution, gel, or paste, for example, powder dentifrice, moisturizing dentifrice, toothpaste, liquid dentifrice, mouthwash, etc. Can be used as a food composition such as chewing gum, troche, candy, etc., or can be used as an oral hygiene device such as dental floss.
In any of these dosage forms, polyethylene glycol, propylene glycol, glycerin, sorbitol, maltitol, xylitol, lactitol, erythritol and the like can be contained for the purpose of a wetting agent or a thickening agent.
また、溶液状組成物の粘稠剤あるいはゲル状組成物のゲル化剤としてさらにはペースト状組成物とする場合の粘結剤としてカルボキシメチルセルロースナトリウム、ヒドロキシエチルセルロース、カルボキシビニルポリマー、キサンタンガム、カラギーナン、アルギン酸ナトリウム、ヒドロキシプロピルセルロース、グアガム、コンドロイチン硫酸ナトリウム等を1種又は2種以上含有させることができる。このうち、フィチン酸又はその塩の美白効果を十分に発揮させる観点からアルギン酸ナトリウム以外の粘着剤を選択することが好ましい。
また、特に緩衝液系の為に高塩濃度となる場合は、非イオン性のポリマー、即ちヒドロキシエチルセルロース、グアガム、ヒドロキシプロピルセルロース等を1種又は2種以上含有させることもできる。
Further, as a thickening agent for a solution-like composition or a gelling agent for a gel-like composition, and as a binder for a paste-like composition, sodium carboxymethylcellulose, hydroxyethylcellulose, carboxyvinyl polymer, xanthan gum, carrageenan, alginic acid Sodium, hydroxypropyl cellulose, guar gum, sodium chondroitin sulfate and the like can be contained alone or in combination. Among these, it is preferable to select an adhesive other than sodium alginate from the viewpoint of sufficiently exerting the whitening effect of phytic acid or a salt thereof.
In particular, in the case of a high salt concentration due to the buffer system, one or more kinds of nonionic polymers, that is, hydroxyethyl cellulose, guar gum, hydroxypropyl cellulose and the like can be contained.
斯様な小柱間隙再形成用組成物を人の歯に、10秒から10時間(洗口剤であれば10秒以上、歯磨剤であれば1分以上、塗布具であれば5分以上)、例えば1日に1〜5回、好ましくは1週間から16週間適用すると、小柱間隙物質を小柱間隙から選択的に取り除くことによって、エナメル質を形成しているエナメル小柱そのものへのダメージを抑えつつ小柱間隙を再形成し、小柱間隙の空間によりエナメル質からの反射光を増やすことによって、自然な白い歯を得ることができる。即ち、長時間の使用、又は繰り返しの使用によっても、歯のエナメル小柱そのものへのダメージは抑えつつ、自然な白い歯を得ることができる。
本発明の口腔用組成物を歯に適用するには、そのまま適用してもよいし、水又は唾液等で30質量%程度まで希釈した状態で適用する場合の両者が含まれる。すなわち、洗口剤のような場合には希釈することなく歯に適用される。一方、練歯磨剤等の場合には唾液により30質量%程度まで希釈された状態で歯に適用されることになる。
Such a trabecular cavity re-forming composition is applied to human teeth for 10 seconds to 10 hours (10 seconds or more for mouthwashes, 1 minute or more for dentifrices, 5 minutes or more for applicators) ), For example, once to 5 times a day, preferably 1 to 16 weeks, by selectively removing trabecular interstitial material from the trabecular space to the enamel trabecules themselves forming the enamel Natural white teeth can be obtained by re-forming the trabecular space while suppressing damage and increasing the reflected light from the enamel through the space of the trabecular space. That is, even when used for a long time or repeatedly, natural white teeth can be obtained while suppressing damage to the enamel trabecules themselves.
In order to apply the composition for oral cavity of the present invention to teeth, it may be applied as it is, or includes both cases in which the composition is diluted to about 30% by mass with water or saliva. That is, in the case of a mouthwash, it is applied to teeth without dilution. On the other hand, in the case of a toothpaste, etc., it is applied to the teeth in a state diluted to about 30% by mass with saliva.
試験例1:リン酸化合物の選択
表1にフィチン酸1%含有の練歯磨剤の各成分及びその含有量(実施例1)を示した。これら成分を混合した練歯磨剤を試験溶液として調製した。試験溶液中のマグネシウム、アルミニウムはICP発光分析法(ICP発光分析装置:Perkin Elmer社 Optima 5300DV)で測定して100ppm以下であった。
表1中の実施例2における練歯磨剤中のフィチン酸をそれぞれ、オルトリン酸、ピロリン酸、ポリリン酸、メタリン酸に代えた以外は実施例2と同様の各成分及び配合割合で、各試験溶液を調製した。
試験に用いるヒト歯は、エナメル表面の一部を鏡面に研磨し処理面とし、それ以外の部分を蝋で被覆したサンプルである。
各試験溶液にヒト歯を室温48時間浸漬した。この場合の浸漬前後b*値の変化Δb*を測定した。当該変化Δb*は、(浸漬後のb*―浸漬前のb*)から求めた。
このb*値は、デジタルカメラD1x(ニコン製)と白色フラッシュ光源(コニカミノルタ製)を用いて撮影された画像をAdobe Photoshop(アドビシステムズ製)を用いてL*a*b*表色系で表し、求めた。b*の値は0に近いほど、黄色味が少なく白さが増すことを意味し、−Δb*(Δb*絶対値)が大きいほど白さが増すことを意味する。
歯のエナメル小柱へのダメージは、歯の表面状態の凸凹をルーペ(倍率10倍)により肉眼で観察をして評価した。
試験例1の結果を表2に示す。
Test Example 1: Selection of Phosphate Compound Table 1 shows each component of a toothpaste containing 1% phytic acid and its content (Example 1). A toothpaste mixed with these components was prepared as a test solution. Magnesium and aluminum in the test solution were 100 ppm or less as measured by ICP emission analysis (ICP emission analyzer: Optima 5300DV manufactured by Perkin Elmer).
Each test solution with the same components and mixing ratios as in Example 2 except that phytic acid in the toothpaste in Example 2 in Table 1 was replaced with orthophosphoric acid, pyrophosphoric acid, polyphosphoric acid, and metaphosphoric acid, respectively. Was prepared.
The human tooth used for the test is a sample in which a part of the enamel surface is polished into a mirror surface to be a treated surface, and the other part is coated with wax.
Human teeth were immersed in each test solution for 48 hours at room temperature. In this case, a change Δb * in b * value before and after immersion was measured. The change [Delta] b * is - was determined from (after immersion b * before immersion b *).
This b * value is calculated using the L * a * b * color system for images taken using a digital camera D1x (Nikon) and a white flash light source (Konica Minolta) using Adobe Photoshop (Adobe Systems). Represented and sought. The closer the value of b * is to 0, the less yellowish the whiteness increases, and the larger -Δb * (Δb * absolute value) means the whiteness increases.
The damage to the enamel trabeculae of the teeth was evaluated by visually observing the irregularities of the tooth surface state with a magnifying glass (magnification 10 times).
The results of Test Example 1 are shown in Table 2.
ピロリン酸、ポリリン酸、メタリン酸は、b*値の変化(Δb*)がある程度観察され、美白効果があると認められるものの、表面観察によるとエナメル小柱に深い凸凹が観察され、ダメージが認められた。オルトリン酸はエナメル小柱のへのダメージは殆ど観察されなかったが、Δb*が小さく、十分な美白効果は認められなかった。一方、フィチン酸はΔb*の値が大きく、高い小柱間隙物質除去効果が認められ、しかも試験溶液処理前後でエナメル小柱の表面はなめらかなままで変化が観察されず、エナメル小柱へのダメージは認められなかった。なお、トリポリリン酸、テトラポリリン酸、ヘキサポリリン酸又はペンタポリリン酸についても同様にして行ったが、小柱間隙物質の除去効果はフィチン酸が際立って優れていた。
従って、フィチン酸がこれらリン酸化合物の中で美白効果とエナメル小柱へのダメージの評価において最も優れていた。さらにフィチン酸を含有する試験溶液を対象に以下の試験を行った。
Although pyrophosphoric acid, polyphosphoric acid, and metaphosphoric acid are observed to have some b * value change (Δb *) and have a whitening effect, surface observation reveals deep irregularities in the enamel trabecula and damage is observed. It was. For orthophosphoric acid, almost no damage to the enamel trabeculae was observed, but Δb * was small and a sufficient whitening effect was not recognized. On the other hand, phytic acid has a large Δb * value, and a high trabecular space substance removal effect is recognized. Moreover, the surface of the enamel trabecular remains smooth before and after the test solution treatment, and no change is observed. No damage was found. Tripolyphosphoric acid, tetrapolyphosphoric acid, hexapolyphosphoric acid, and pentapolyphosphoric acid were also performed in the same manner, but phytic acid was remarkably superior in removing the trabecular space material.
Accordingly, phytic acid was most excellent in the whitening effect and the evaluation of damage to the enamel trabeculae among these phosphate compounds. Furthermore, the following tests were conducted on test solutions containing phytic acid.
試験例2:組成物のpH及び組成物中のフィチン酸の含有量
(1)組成物及び試験対象物の調製
表1及び3に実施例1〜7及び比較例1〜8の練歯磨剤の各成分及びその含有量を示す。これらの練歯磨剤(試験溶液)のpHは、水で30質量%に希釈したときのpHである。
練歯磨剤中のフィチン酸の含有量を1質量%とし、このpHは水で30質量%に希釈したときに、3.0、4.0、5.0、5.5、6.0、6.5、7.0、8.0に調整した練歯磨剤の試験溶液(実施例1〜3及び比較例1〜5)を調製した。これらの各試験溶液中のマグネシウム、アルミニウムの含有量は100ppm以下であった。
また、練歯磨剤中のフィチン酸の含有量を0、0.05、0.1、10、18、19、20質量%とし、このpHを6.0に調整した練歯磨剤の各試験溶液(実施例4〜7及び比較例6〜8)を調製した。フィチン酸の含有量1質量%は実施例2を対象とした。これらの各試験溶液中のマグネシウム、アルミニウムの含有量も100ppm以下であった。
試験に用いるヒト歯、それぞれの試験溶液による浸漬前後b*値の変化Δb*の測定、歯の表面状態の凸凹の測定、及びSEMによる小柱間隙の状態の観察は、上記試験例1と同様にして行った。
Test Example 2: Composition pH and Phytic Acid Content in Composition (1) Preparation of Composition and Test Object Tables 1 and 3 show the toothpastes of Examples 1-7 and Comparative Examples 1-8. Each component and its content are shown. The pH of these toothpastes (test solutions) is the pH when diluted to 30% by mass with water.
When the content of phytic acid in the toothpaste is 1% by mass and the pH is diluted to 30% by mass with water, 3.0, 4.0, 5.0, 5.5, 6.0, Toothpaste test solutions (Examples 1 to 3 and Comparative Examples 1 to 5) adjusted to 6.5, 7.0, and 8.0 were prepared. The content of magnesium and aluminum in each of these test solutions was 100 ppm or less.
In addition, each test solution of toothpaste with a phytic acid content in the toothpaste adjusted to 0, 0.05, 0.1, 10, 18, 19, 20% by mass and the pH adjusted to 6.0 (Examples 4 to 7 and Comparative Examples 6 to 8) were prepared. A phytic acid content of 1% by mass was intended for Example 2. The contents of magnesium and aluminum in each test solution were also 100 ppm or less.
The measurement of b * value change Δb * before and after immersion with each test solution, the measurement of unevenness of the tooth surface state, and the observation of the trabecular space state by SEM are the same as in Test Example 1 above. I went there.
(2)SEMによる歯の小柱間隙の観察方法
実施例2の練歯磨剤(試験溶液)をヒト歯に適用(浸漬)させた前後のヒト歯を電子顕微鏡(SEM:日立S−4800)により観察した写真を図2(a)(b) に示す。
(2) Method for observing tooth trabecular gap of SEM by electron microscope (SEM: Hitachi S-4800) before and after applying toothpaste (test solution) of Example 2 to human teeth. The observed photographs are shown in FIGS. 2 (a) and 2 (b).
(3)パネラーによる試験方法
また、各組成物の練歯磨剤をパネラー(健常男女20人)で1日の朝晩5分間歯磨きを2週間行った。このときの健常男女の年齢構成は、40〜70代20人である。
(3) Test method by paneler Further, the toothpaste of each composition was brushed with a paneler (20 healthy men and women) for 5 minutes in the morning and evening for 2 weeks. The age structure of healthy men and women at this time is 20 people in their 40s to 70s.
(4)結果
(SEMによる歯の小柱間隙の観察)
電子顕微鏡(SEM:日立S−4800)により歯の小柱間隙を観察した写真を図1、図2に示す。図1(a)には白い歯A(10代のヒト歯)、図1(b)には着色のある歯B(50代のヒト歯)の電子顕微鏡(SEM)により観察した写真を示す。 図1(a)、(b)の写真が示すように、白い歯Aでは小柱間隙を観察できるが、着色のある歯Bでは小柱間隙をほとんど観察することができなくなっている。
図2(b)には本発明のフィチン酸を含む組成物に浸漬する前の歯B、図2(a)には、本発明のフィチン酸を含む組成物(実施例2)に浸漬した後の歯Bの電子顕微鏡により観察した写真を示す。図2(a)(b)の写真が示すように、歯Bの浸漬前の図2(b)の写真では小柱間隙を殆ど観察できないが、浸漬後の図2(a)の写真では小柱間隙が観察され、小柱間隙が形成されたことを確認できた。
(4) Results (observation of trabecular space of teeth by SEM)
The photographs of the trabecular space of the teeth observed with an electron microscope (SEM: Hitachi S-4800) are shown in FIGS. FIG. 1 (a) shows a photograph of white teeth A (10th generation human teeth) observed with an electron microscope (SEM), and FIG. 1 (b) shows colored teeth B (50th generation human teeth). As shown in the photographs of FIGS. 1A and 1B, the trabecular space can be observed with the white teeth A, but the trabecular space can hardly be observed with the colored teeth B.
FIG. 2 (b) shows the tooth B before dipping in the composition containing phytic acid of the present invention, and FIG. 2 (a) shows that after dipping in the composition containing phytic acid of the present invention (Example 2). The photograph observed with the electron microscope of the tooth | gear B of is shown. As shown in the photographs of FIGS. 2 (a) and 2 (b), the trabecular space can hardly be observed in the photograph of FIG. 2 (b) before the immersion of the tooth B, but small in the photograph of FIG. 2 (a) after the immersion. The column gap was observed, and it was confirmed that a small column gap was formed.
(組成物のpHにおける試験結果)
それぞれのpHにおける浸漬による表面状態の変化を表1に、Δb*の変化を図3及び表4に示す。
(Test result at pH of composition)
Table 1 shows changes in the surface state due to immersion at each pH, and Tables 3 and 4 show changes in Δb * .
図3及び表4(表1、3)に示すように、pHが5.5より低い領域では歯の白さの変化を示すb*の変化(Δb*)は大きいが、歯の表面状態に凸凹が観察され、かつ、電子顕微鏡(SEM)による観察では、本来のエナメル小柱の小柱間隙(0.1〜0.5μm)よりも広い隙間が観察された。従って、pH5.5よりも低い領域では、歯の白さは得られるが、エナメル小柱に溶解を生じ、脱灰状態にあると判断できる。一方、pHが7.0以上では、浸漬後の歯の白さの変化Δb*は非常に小さいが、表面状態はなめらかで変化は観察されなかった。これに対して本発明の小柱間隙再形成用組成物はpHが5.5以上6.5以下であり、この条件ではでは、Δb*は充分に大きく高い美白性能を示し、SEMによる観察でもエナメル小柱間に適度な隙間が観察され、表面状態はなめらかで変化は観察されず、脱灰を殆ど発生させていないと判断できた。
このように、本発明に示すpHが5.5〜6.5の領域のフィチン酸(イノシトール6リン酸)及びその塩は、エナメル質を構成しているエナメル小柱にダメージを殆ど与えず、小柱間隙物質を選択的に除去できる。
As shown in FIG. 3 and Table 4 (Tables 1 and 3), in the region where the pH is lower than 5.5, the change in b * (Δb * ) indicating the change in tooth whiteness is large, but the surface condition of the tooth Unevenness was observed, and in observation with an electron microscope (SEM), a gap wider than the trabecular gap (0.1 to 0.5 μm) of the original enamel trabecula was observed. Therefore, in the region lower than pH 5.5, whiteness of the teeth can be obtained, but it can be determined that the enamel trabeculae are dissolved and decalcified. On the other hand, when the pH was 7.0 or more, the change Δb * in tooth white after immersion was very small, but the surface condition was smooth and no change was observed. On the other hand, the trabecular cavity re-forming composition of the present invention has a pH of 5.5 or more and 6.5 or less. Under these conditions, Δb * is sufficiently large and exhibits high whitening performance. Appropriate gaps were observed between the enamel trabeculae, the surface state was smooth and no change was observed, and it was judged that almost no demineralization occurred.
Thus, the phytic acid (inositol 6-phosphate) and its salt in the region of pH 5.5 to 6.5 shown in the present invention hardly damage the enamel trabeculae constituting the enamel, The trabecular space material can be selectively removed.
(組成物中のフィチン酸の含有量における試験結果)
図4及び表5(表1、3)にフィチン酸濃度別のΔb*を示す。図4(b)は、フィチン酸濃度が1.5質量%以下の領域のΔb*を拡大して示したものである。図4(b)及び表1、3に示すようにフィチン酸濃度0.05質量%においてもb*値の変化Δb*が−4.5と美白性能を示し、0.1%以上ではΔb*が最大となり高い美白性能を示した。
しかし、図4(a)に示すように、フィチン酸濃度18質量%までは表面状態の変化は殆ど観察されていないが、19質量%以上の濃度では凸凹が発生している。また、味の観点からも、18質量%以下の濃度、さらに10質量%以下の濃度が好ましい。
(Test results for the content of phytic acid in the composition)
FIG. 4 and Table 5 (Tables 1 and 3) show Δb * by phytic acid concentration. FIG. 4B is an enlarged view of Δb * in a region where the phytic acid concentration is 1.5% by mass or less. As shown in FIG. 4 (b) and Tables 1 and 3, even when the phytic acid concentration was 0.05% by mass, the b * value change Δb * was −4.5, indicating whitening performance, and at 0.1% or more, Δb * Showed the highest whitening performance.
However, as shown in FIG. 4A, almost no change in the surface state is observed up to a phytic acid concentration of 18% by mass, but unevenness occurs at a concentration of 19% by mass or more. Moreover, also from a viewpoint of taste, the density | concentration of 18 mass% or less and also the density | concentration of 10 mass% or less are preferable.
よって、5.5〜6.5の領域のpHで、0.05〜18質量%濃度のフィチン酸を用いた小柱間隙再形成用組成物は、使用感がよく歯や歯茎にダメージを殆ど与えずに高い美白性能を有する。 Therefore, the trabecular space re-forming composition using phytic acid at a concentration of 0.05 to 18% by mass at a pH in the range of 5.5 to 6.5 has a good feeling and hardly damages teeth or gums. High whitening performance without giving.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2010058522A1 (en) * | 2008-11-19 | 2010-05-27 | 花王株式会社 | Method for removing solid product formed on surfaces of teeth |
JP2010120880A (en) * | 2008-11-19 | 2010-06-03 | Kao Corp | Oral composition |
JP2010150225A (en) * | 2008-11-19 | 2010-07-08 | Kao Corp | Composition for removing solid product formed on surface of tooth |
WO2011062151A1 (en) | 2009-11-18 | 2011-05-26 | 新日本製鐵株式会社 | High strength hot-rolled steel plate exhibiting excellent acid pickling property, chemical conversion processability, fatigue property, stretch flangeability, and resistance to surface deterioration during molding, and having isotropic strength and ductility, and method for producing said high strength hot-rolled steel plate |
US8580234B2 (en) | 2008-11-19 | 2013-11-12 | Kao Corporation | Method for removing solid product formed on surfaces of teeth |
JP2020063205A (en) * | 2018-10-17 | 2020-04-23 | 花王株式会社 | Composition for oral cavity |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN109862874A (en) * | 2016-10-18 | 2019-06-07 | 花王株式会社 | Composition for oral cavity |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5618913A (en) * | 1979-07-25 | 1981-02-23 | Lion Corp | Detergent for tooth or artificial denture |
JPS5618911A (en) * | 1979-07-25 | 1981-02-23 | Lion Corp | Dentifrice composition |
JPH1017447A (en) * | 1996-06-28 | 1998-01-20 | Lion Corp | Antiodontolithic agent and composition for oral cavity |
JP2003335646A (en) * | 2002-05-20 | 2003-11-25 | Lion Corp | Dentifrice composition |
JP2004224779A (en) * | 2003-01-27 | 2004-08-12 | Kao Corp | Composition for oral cavity |
JP2005170867A (en) * | 2003-12-12 | 2005-06-30 | Lion Corp | Oral composition |
-
2008
- 2008-04-24 JP JP2008113465A patent/JP5303180B2/en active Active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5618913A (en) * | 1979-07-25 | 1981-02-23 | Lion Corp | Detergent for tooth or artificial denture |
JPS5618911A (en) * | 1979-07-25 | 1981-02-23 | Lion Corp | Dentifrice composition |
JPH1017447A (en) * | 1996-06-28 | 1998-01-20 | Lion Corp | Antiodontolithic agent and composition for oral cavity |
JP2003335646A (en) * | 2002-05-20 | 2003-11-25 | Lion Corp | Dentifrice composition |
JP2004224779A (en) * | 2003-01-27 | 2004-08-12 | Kao Corp | Composition for oral cavity |
JP2005170867A (en) * | 2003-12-12 | 2005-06-30 | Lion Corp | Oral composition |
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2010058522A1 (en) * | 2008-11-19 | 2010-05-27 | 花王株式会社 | Method for removing solid product formed on surfaces of teeth |
JP2010120880A (en) * | 2008-11-19 | 2010-06-03 | Kao Corp | Oral composition |
JP2010150225A (en) * | 2008-11-19 | 2010-07-08 | Kao Corp | Composition for removing solid product formed on surface of tooth |
US8580234B2 (en) | 2008-11-19 | 2013-11-12 | Kao Corporation | Method for removing solid product formed on surfaces of teeth |
WO2011062151A1 (en) | 2009-11-18 | 2011-05-26 | 新日本製鐵株式会社 | High strength hot-rolled steel plate exhibiting excellent acid pickling property, chemical conversion processability, fatigue property, stretch flangeability, and resistance to surface deterioration during molding, and having isotropic strength and ductility, and method for producing said high strength hot-rolled steel plate |
KR101412343B1 (en) | 2009-11-18 | 2014-06-25 | 신닛테츠스미킨 카부시키카이샤 | High strength hot-rolled steel plate exhibiting excellent acid pickling property, chemical conversion processability, fatigue property, stretch flangeability, and resistance to surface deterioration during molding, and having isotropic strength and ductility, and method for producing said high strength hot-rolled steel plate |
US8852360B2 (en) | 2009-11-18 | 2014-10-07 | Nippon Steel & Sumitomo Metal Corporation | High strength hot-rolled steel plate exhibiting excellent acid pickling property, chemical conversion processability, fatigue property, stretch flangeability, and resistance to surface deterioration during molding, and having isotropic strength and ductility |
US9523134B2 (en) | 2009-11-18 | 2016-12-20 | Nippon Steel & Sumitomo Metal Corporation | Method for producing a high strength hot-rolled steel plate exhibiting excellent acid pickling property, chemical conversion processability, fatigue property, stretch flangeability, and resistance to surface deterioration during molding, and having isotropic strength and ductility |
JP2020063205A (en) * | 2018-10-17 | 2020-04-23 | 花王株式会社 | Composition for oral cavity |
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