JP4873155B2 - Tooth whitening composition and tooth whitening set - Google Patents
Tooth whitening composition and tooth whitening set Download PDFInfo
- Publication number
- JP4873155B2 JP4873155B2 JP2006548869A JP2006548869A JP4873155B2 JP 4873155 B2 JP4873155 B2 JP 4873155B2 JP 2006548869 A JP2006548869 A JP 2006548869A JP 2006548869 A JP2006548869 A JP 2006548869A JP 4873155 B2 JP4873155 B2 JP 4873155B2
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- JP
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- Prior art keywords
- tooth
- composition
- tooth whitening
- sodium
- teeth
- Prior art date
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- FYGDTMLNYKFZSV-BYLHFPJWSA-N β-1,4-galactotrioside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@H](CO)O[C@@H](O[C@@H]2[C@@H](O[C@@H](O)[C@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O FYGDTMLNYKFZSV-BYLHFPJWSA-N 0.000 description 1
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/731—Cellulose; Quaternized cellulose derivatives
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/26—Aluminium; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/27—Zinc; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
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- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/28—Zirconium; Compounds thereof
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/29—Titanium; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
- A61K8/66—Enzymes
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/88—Polyamides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/54—Polymers characterized by specific structures/properties
- A61K2800/542—Polymers characterized by specific structures/properties characterized by the charge
- A61K2800/5426—Polymers characterized by specific structures/properties characterized by the charge cationic
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Description
本発明は、歯を元の色よりも白くみせるための歯牙美白用組成物及び歯牙美白用セットに関し、更に詳述すると、歯牙に貼付又は塗布して、二酸化チタンなどの粉体を一定時間歯の表面に固定し、乱反射によって歯を白く見せるものであって、高い白色化効果を長時間持続的に発揮させる歯牙美白用組成物及び歯牙美白用セットに関する。 The present invention relates to a tooth whitening composition and a tooth whitening set for making a tooth whiter than the original color. More specifically, the present invention relates to a tooth whitening composition which is applied or applied to a tooth and a powder such as titanium dioxide is applied to the tooth for a certain period of time. The present invention relates to a tooth whitening composition and a tooth whitening set, which are fixed to the surface of the tooth and make teeth appear white by irregular reflection and exhibit a high whitening effect for a long time.
従来より、歯を白くするための技術は、(1)歯に付着した着色物質を取り除き、元の歯の白さを取り戻す技術と、(2)歯を元の色より更に白くする技術に大別される。(1)の方法としては、歯磨剤、歯ブラシを用い、歯磨剤に含まれる研磨成分でブラッシングすることによる物理的な除去方法や、ポリエチレングリコール、ポリビニルピロリドン等の可溶化剤、酵素、キレート剤等により着色物を分解する等の化学的な方法が用いられ、(2)の方法としては、欧米で多用される過酸化物を使った漂白や、歯のマニキュア剤などに代表される隠蔽剤の塗布、あるいはラミネートベニア等の歯科材料が使われてきた。 Conventional techniques for whitening teeth include (1) a technique for removing colored substances attached to the teeth and restoring the whiteness of the original teeth, and (2) a technique for making the teeth whiter than the original color. Separated. As the method of (1), using a dentifrice or toothbrush, a physical removal method by brushing with a polishing component contained in the dentifrice, a solubilizer such as polyethylene glycol or polyvinylpyrrolidone, an enzyme, a chelating agent, etc. Chemical methods such as decomposing colored materials are used, and (2) methods include bleaching using peroxides frequently used in Europe and the United States, and concealing agents typified by dental nail polish. Dental materials such as coated or laminated veneers have been used.
近年、口腔衛生意識と審美願望の向上を受けて、歯の美白に対するニーズは、(1)の「清掃」から(2)の「白色化」に移行しつつある。しかしながら、過酸化物での漂白は、歯肉の炎症、退縮のおそれがあり、専門知識のない消費者が勝手に使用することは非常に危険である。一方、マニキュア等の塗布剤は、飲食等により剥離するため持続性に欠ける。また、ラミネートベニアによる方法は、歯科医しか行うことができず、しかも健全な歯の表面を削る必要があり、患者が結果に対して不満足であっても、術後元の歯に戻すことができない。 In recent years, with the improvement of oral hygiene awareness and desire for aesthetics, the need for whitening teeth is shifting from “cleaning” in (1) to “whitening” in (2). However, bleaching with peroxides may cause gingival irritation and regression, and it is extremely dangerous for consumers without expert knowledge to use it without permission. On the other hand, since coating agents such as nail polish are peeled off by eating and drinking, etc., they lack sustainability. In addition, the laminate veneer method can only be performed by a dentist, and it is necessary to cut the surface of a healthy tooth. Even if the patient is not satisfied with the result, it cannot be restored to the original tooth after the operation. .
以上のことから、「白色化」の分野において、審美性が良く、且つ簡便で安全性が高い、歯牙白色化技術の開発が望まれてきた。 In view of the above, in the field of “whitening”, it has been desired to develop a tooth whitening technique that has good aesthetics, is simple and has high safety.
このような白色化技術として、シェラック、酢酸ビニル樹脂やアクリル系樹脂の被膜形成能を活用したマニキュア等の塗布剤が提案されているが(特開平04−82821号公報、特開平05−58844号公報、特開平09−100215号公報、特開平09−202718号公報、特開平09−151123号公報)、歯にコーティングされた被膜剤のザラザラした使用感に課題があった。また、被膜剤と併用して用いられる酸化チタンの粒径は100nm以下が好ましいことが開示されているが(特開平09−151123号公報)、被膜剤を併用しない場合の酸化チタンの歯牙への吸着性は必ずしも十分とは言えなかった。 As such whitening technology, coating agents such as nail polish utilizing the film forming ability of shellac, vinyl acetate resin and acrylic resin have been proposed (Japanese Patent Laid-Open Nos. 04-82821 and 05-58844). There is a problem in the rough feeling of use of the coating agent coated on the teeth, Japanese Patent Laid-Open No. 09-1000021, Japanese Patent Laid-Open No. 09-202718, and Japanese Patent Laid-Open No. 09-151123. Moreover, although it is disclosed that the particle size of titanium oxide used in combination with a coating agent is preferably 100 nm or less (Japanese Patent Application Laid-Open No. 09-151123), the titanium oxide to the teeth when not using the coating agent is disclosed. The adsorptivity was not always sufficient.
従来より歯磨剤等で一般的に顔料として用いられる酸化チタンの比表面積は10〜20m2/gであるが、この範囲の比表面積を有する金属酸化物を被膜剤のような支持体なしで歯牙に適用しても、歯牙への吸着性が低く、十分な白色化効果を発揮することができなかった。The specific surface area of titanium oxide generally used as a pigment in dentifrices and the like is 10 to 20 m 2 / g, and a metal oxide having a specific surface area in this range can be used without a support such as a coating agent. Even when applied to the tooth, the adsorptivity to the teeth was low, and a sufficient whitening effect could not be exhibited.
一方、特開2003−183142号公報には、金属酸化物の表面水酸基数を増加させる活性化処理を施すことで、エナメル質への吸着性を高めて歯を白く見せる方法及びその組成物が開示されている。しかしながら、前処理として金属酸化物を高アルカリ条件で処理する必要があるため、操作性、安全性に課題があった。 On the other hand, Japanese Patent Application Laid-Open No. 2003-183142 discloses a method and composition for enhancing the adsorptivity to enamel and making teeth appear white by performing an activation treatment to increase the number of surface hydroxyl groups of the metal oxide. Has been. However, since it is necessary to treat the metal oxide under high alkali conditions as a pretreatment, there are problems in operability and safety.
従って、本発明の目的は、歯を元の色よりも白くみせるための歯牙美白用組成物であって、歯牙に貼付又は塗布して、二酸化チタンなどの粉体を一定時間歯の表面に固定し、乱反射によって歯を白く見せ、且つ、長時間安定して粉体を歯面に保持することで色ムラや剥がれを大幅に低減して、高い白色化効果を持続的に発揮させる歯牙美白用組成物及び歯牙美白用セットを提供することである。 Accordingly, an object of the present invention is a tooth whitening composition for making a tooth whiter than the original color, which is applied or applied to the tooth, and a powder such as titanium dioxide is fixed to the tooth surface for a certain period of time. Tooth whitening that makes teeth appear white due to diffuse reflection and holds the powder on the tooth surface stably for a long time, greatly reducing color unevenness and peeling and providing a high whitening effect continuously. It is to provide a composition and a set for tooth whitening.
本発明者らは上記課題を解決するために鋭意検討を重ねた結果、二酸化チタン、二酸化ケイ素、酸化亜鉛、酸化アルミニウム、酸化マグネシウム、酸化ジルコニウムから選ばれる白色化粉体と、ゲル化剤としてのプルランと、リゾチーム、カチオン化セルロース、ポリリジンから選ばれるカチオン性高分子を組み合わせることで、白色化粉体を歯面に長時間安定して固定し、色ムラや剥がれを大幅に低減して、高い白色化効果の持続性を与えることを見出し、本発明をなすに至った。 As a result of intensive studies in order to solve the above problems, the present inventors have found that whitening powder selected from titanium dioxide, silicon dioxide, zinc oxide, aluminum oxide, magnesium oxide, zirconium oxide, and a gelling agent By combining pullulan with a cationic polymer selected from lysozyme, cationized cellulose, and polylysine, whitening powder is stably fixed on the tooth surface for a long time, and color unevenness and peeling are greatly reduced. The inventors have found that the whitening effect is sustained, and have made the present invention.
従って、本発明は、
(A)二酸化チタン、二酸化ケイ素、酸化亜鉛、酸化アルミニウム、酸化マグネシウム、酸化ジルコニウムから選ばれる1種又は2種以上、
(B)プルラン、
(C)リゾチーム、カチオン化セルロース、ポリリジンから選ばれる1種又は2種以上
を含有することを特徴とする歯牙美白用組成物を提供する。Therefore, the present invention
(A) One or more selected from titanium dioxide, silicon dioxide, zinc oxide, aluminum oxide, magnesium oxide, zirconium oxide,
(B) Pullulan,
(C) A tooth whitening composition characterized by containing one or more selected from lysozyme, cationized cellulose, and polylysine.
また、本発明は上記歯牙美白用組成物を保持した状態で、歯に着脱可能に装着される適用用具とを備えたことを特徴とする歯牙美白用セットを提供する。この場合、適用用具としては、テープ、シート、フィルム、マウストレー、マウスピース、スポンジ、印象材、パック材、又は歯列に成型した歯のカバーが挙げられる。 The present invention also provides a tooth whitening set comprising an application tool that is detachably attached to a tooth while holding the tooth whitening composition. In this case, examples of the application tool include a tape, a sheet, a film, a mouth tray, a mouthpiece, a sponge, an impression material, a pack material, or a tooth cover molded into a dentition.
本発明によれば、歯牙への吸着性に優れた金属酸化物粉体が歯の表面で光を乱反射して本来の色よりも白く見せることができ、この場合、特に長時間安定して該粉体を歯面に保持し、高い白色化効果を持続的に発揮させることができる。 According to the present invention, the metal oxide powder having excellent adsorptivity to teeth can diffusely reflect light on the tooth surface and appear whiter than the original color. The powder can be held on the tooth surface and a high whitening effect can be exhibited continuously.
本発明の歯牙美白用組成物に用いられる(A)成分は、二酸化チタン、二酸化ケイ素、酸化亜鉛、酸化アルミニウム、酸化マグネシウム、酸化ジルコニウムから選ばれる金属酸化物であり、好ましくは二酸化チタン、酸化亜鉛、酸化アルミニウム、酸化ジルコニウムであり、これらの1種又は2種以上が用いられ、これら金属酸化物の複合物であってもよい。 Component (A) used in the tooth whitening composition of the present invention is a metal oxide selected from titanium dioxide, silicon dioxide, zinc oxide, aluminum oxide, magnesium oxide, and zirconium oxide, preferably titanium dioxide and zinc oxide. , Aluminum oxide and zirconium oxide, one or more of these being used, and a composite of these metal oxides.
本発明に用いられる金属酸化物は、表面処理の有無は特に制限されないが、金属酸化物の触媒活性を抑制する目的で二酸化ケイ素、アルミナ、酸化ジルコニウムで被覆したものも好適に用いられる。 The presence or absence of the surface treatment is not particularly limited for the metal oxide used in the present invention, but those coated with silicon dioxide, alumina and zirconium oxide are also preferably used for the purpose of suppressing the catalytic activity of the metal oxide.
本発明に用いられる(A)成分の金属酸化物の配合量は、歯牙美白用組成物から歯の表面に十分な量放出することができれば特に制限されないが、好ましくは組成物全体の0.1〜50質量%、更に好ましくは0.5〜20質量%である。配合量が0.1質量%未満の場合には、十分な白色化効果を得ることができず、50質量%を超える場合には、歯牙への適用形態によっては使用性の悪い組成物になってしまう場合がある。 The blending amount of the metal oxide of the component (A) used in the present invention is not particularly limited as long as a sufficient amount can be released from the tooth whitening composition to the tooth surface, but preferably 0.1% of the entire composition. -50 mass%, More preferably, it is 0.5-20 mass%. When the blending amount is less than 0.1% by mass, a sufficient whitening effect cannot be obtained, and when it exceeds 50% by mass, it becomes a composition having poor usability depending on the application form to the tooth. May end up.
本発明の(A)成分として用いられる金属酸化物の平均粒子径は、0.005〜5μmが好ましい。特に好ましくは0.01〜1μmである。平均粒子径が0.005μm未満の場合には十分に光を散乱することができず、白色化効果が得られない場合がある。平均粒子径が5μmを超える場合には、歯牙への固定性が十分でなく、白色化効果が持続しないことがある。なお、本発明において、平均粒子径はマイクロトラック粒度分析計(日機装(株))による50%粒径の測定値である。 As for the average particle diameter of the metal oxide used as (A) component of this invention, 0.005-5 micrometers is preferable. Most preferably, it is 0.01-1 micrometer. When the average particle diameter is less than 0.005 μm, the light cannot be sufficiently scattered, and the whitening effect may not be obtained. When the average particle diameter exceeds 5 μm, the fixation to the teeth is not sufficient, and the whitening effect may not be sustained. In addition, in this invention, an average particle diameter is a measured value of 50% particle diameter by a micro track particle size analyzer (Nikkiso Co., Ltd.).
本発明に用いられる(B)成分のプルランは、マルトトリオースがα1−6結合した高分子であり、重量平均分子量約4〜80万のものが挙げられる。なかでも特に10〜50万のものが好適に使用される。なお、プルランの重量平均分子量は既知分子量のポリエチレンオキサイドを標準物質とし、LiBrを添加したジメチルホルムアミドを溶媒とした、ゲルパーミエーションクロマトグラフ(GPC)法により求められる。プルランは、ポリアクリル酸又はその塩、カルボキシビニルポリマー、酢酸ビニル・ビニルピロリドン共重合体、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、ヒドロキシプロピルセルロース等のセルロース誘導体、ポリビニルピロリドン、ポリビニルアルコール、キサンタンガム、カラギーナン、アルギン酸塩などの他の水溶性高分子と組み合わせて使用できる。プルランの組成物中の配合量は、組成物全体の0.1〜20質量%の範囲、特に0.3〜15質量%の範囲が好ましい。この場合、プルランの分子量に応じて配合量を選定することが好ましく、特に、重量平均分子量約79万の場合0.1〜5質量%が好ましく、更に好ましくは0.3〜3質量%である。重量平均分子量約40万の場合0.1〜7質量%が好ましく、更に好ましくは0.5〜5質量%である。重量平均分子量約20万の場合0.3〜15質量%が好ましく、更に好ましくは0.5〜10質量%である。重量平均分子量約4.7万の場合0.5〜20質量%が好ましく、更に好ましくは1〜15質量%である。プルランの配合量が、各重量平均分子量における好ましい配合量に満たない場合には、他の水溶性高分子と組み合わせても、組成物の歯牙への吸着性と持続性が低く、金属酸化物が歯に長時間安定して吸着できない場合がある。また各重量平均分子量における好ましい配合量を超える場合には、組成物の粘度が高くなり、十分な量の金属酸化物が歯に吸着できない場合がある。 The pullulan as the component (B) used in the present invention is a polymer in which maltotriose is α1-6 bonded, and examples thereof include those having a weight average molecular weight of about 4 to 800,000. Of these, those having 100,000 to 500,000 are particularly preferred. The weight average molecular weight of pullulan is determined by a gel permeation chromatograph (GPC) method using polyethylene oxide having a known molecular weight as a standard substance and dimethylformamide added with LiBr as a solvent. Pullulan is polyacrylic acid or a salt thereof, carboxyvinyl polymer, vinyl acetate / vinyl pyrrolidone copolymer, cellulose derivatives such as sodium carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, polyvinyl pyrrolidone, polyvinyl alcohol, xanthan gum, carrageenan, alginate It can be used in combination with other water-soluble polymers. The blending amount of the pullulan in the composition is preferably in the range of 0.1 to 20% by mass, particularly in the range of 0.3 to 15% by mass of the whole composition. In this case, it is preferable to select the blending amount according to the molecular weight of pullulan. In particular, when the weight average molecular weight is about 790,000, 0.1 to 5% by mass is preferable, and more preferably 0.3 to 3% by mass. . When the weight average molecular weight is about 400,000, it is preferably 0.1 to 7% by mass, and more preferably 0.5 to 5% by mass. When the weight average molecular weight is about 200,000, it is preferably 0.3 to 15% by mass, and more preferably 0.5 to 10% by mass. When the weight average molecular weight is about 47,000, the content is preferably 0.5 to 20% by mass, and more preferably 1 to 15% by mass. When the blending amount of pullulan is less than the preferred blending amount in each weight average molecular weight, even when combined with other water-soluble polymers, the adsorptivity and sustainability of the composition to the teeth are low, and the metal oxide is There are cases where it cannot be stably adsorbed to teeth for a long time. Moreover, when the preferable compounding quantity in each weight average molecular weight is exceeded, the viscosity of a composition becomes high and sufficient metal oxide may not adsorb | suck to a tooth | gear.
本発明に用いられる(C)成分は、リゾチーム、カチオン化セルロース、ポリリジンから選ばれる1種又は2種以上である。 The component (C) used in the present invention is one or more selected from lysozyme, cationized cellulose, and polylysine.
リゾチームは塩化リゾチームが好適に用いられる。リゾチームの配合量は、組成物全体の0.1〜10質量%が好ましく、0.5〜5質量%が更に好ましい。リゾチームの配合量が、0.1質量%未満の場合には、組成物の歯牙への吸着性と持続性が低く、金属酸化物が歯に長時間安定して吸着できない場合がある。また10質量%を超える場合には、リゾチーム独特の苦味が強くなり、組成物の味が悪くなる場合がある。 The lysozyme is preferably lysozyme chloride. The blending amount of lysozyme is preferably from 0.1 to 10% by weight, more preferably from 0.5 to 5% by weight, based on the entire composition. When the blending amount of lysozyme is less than 0.1% by mass, the adsorptivity and persistence of the composition on the teeth are low, and the metal oxide may not be stably adsorbed on the teeth for a long time. On the other hand, if it exceeds 10% by mass, the bitterness peculiar to lysozyme becomes strong, and the taste of the composition may deteriorate.
カチオン化セルロースはヒドロキシジメチルアリルアンモニウムクロライドや塩化O−{2−ヒドロキシ−3−(トリメチルアンモニオ)}プロピルヒドロキシエチルセルロースが好適に用いられる。重量平均分子量は約30万〜約200万のものが好適に用いられる。重量平均分子量が30万より小さい場合、歯牙への固定性が十分でなく、白色化効果が持続しないことがあり、重量平均分子量が200万より大きい場合は製剤の粘度が高くなり、操作性が損なわれる場合がある。カチオン基の置換度は、窒素分として0.5〜3質量%が好適に用いられる。窒素分が0.5質量%未満の場合、歯牙への固定性が十分でなく、白色化効果が持続しないことがあり、窒素分が3質量%を超える場合は味が悪くなり、使用感が低下する場合がある。なお、重量平均分子量はポリエチレングリコールを標準物質としたゲルパーミエーションクロマトグラフ(GPC)法により求めた値である。また、窒素分はCHN有機元素分析によって求めた値である。カチオン化セルロースの配合量は、組成物全体の0.1〜5質量%が好ましく、0.5〜3質量%が更に好ましい。カチオン化セルロースの配合量が、0.1質量%未満の場合には、組成物の歯牙への吸着性と持続性が低く、金属酸化物が歯に長時間安定して吸着できない場合がある。また5質量%を超える場合には、組成物の粘度が高くなり、十分な量の金属酸化物が歯に吸着できない場合がある。 As the cationized cellulose, hydroxydimethylallylammonium chloride or O- {2-hydroxy-3- (trimethylammonio)} propylhydroxyethylcellulose chloride is preferably used. A weight average molecular weight of about 300,000 to about 2 million is preferably used. When the weight average molecular weight is less than 300,000, the fixity to the teeth is not sufficient, and the whitening effect may not be sustained. When the weight average molecular weight is more than 2 million, the viscosity of the preparation is increased and the operability is improved. It may be damaged. The substitution degree of the cationic group is preferably 0.5 to 3% by mass as the nitrogen content. When the nitrogen content is less than 0.5% by mass, the fixity to the teeth is not sufficient, and the whitening effect may not be sustained. When the nitrogen content exceeds 3% by mass, the taste is poor and the feeling of use is poor. May decrease. The weight average molecular weight is a value determined by a gel permeation chromatograph (GPC) method using polyethylene glycol as a standard substance. The nitrogen content is a value obtained by CHN organic element analysis. 0.1-5 mass% of the whole composition is preferable, and, as for the compounding quantity of a cationized cellulose, 0.5-3 mass% is still more preferable. When the blending amount of cationized cellulose is less than 0.1% by mass, the adsorptivity and persistence of the composition on the teeth are low, and the metal oxide may not be stably adsorbed on the teeth for a long time. On the other hand, when it exceeds 5% by mass, the viscosity of the composition increases, and a sufficient amount of metal oxide may not be adsorbed on the teeth.
ポリリジンは、ポリリジン単独やポリリジン塩酸塩、ポリリジンハイドロブロマイドなどの塩を使用することができる。ポリリジンの数平均分子量は、1000〜100万のものを用いることができ、特に3000〜30万のものが好適に使用される。数平均分子量が1000より小さい場合、歯牙への固定性が十分でなく、白色化効果が持続しないことがあり、数平均分子量が100万より大きい場合は製剤の粘度が高くなり、操作性が損なわれる場合がある。なお、数平均分子量の測定法は特に限定されるものではないが、例えばポリスチレンを標準物質としたゲルパーミエーションクロマトグラフの低角度光散乱法(GPC−LALLS法)により以下の条件で求めることができる。
カラム :Tosoh Biosep G5000 PWXL、7.8mm×30cm
移動層 :0.1mol/L リン酸ナトリウムバッファー(pH7.0)
流 量 :0.5mL/min
カラム温度:40℃As polylysine, salts such as polylysine alone, polylysine hydrochloride and polylysine hydrobromide can be used. The number average molecular weight of polylysine can be 1,000 to 1,000,000, with 3000 to 300,000 being particularly preferred. When the number average molecular weight is less than 1000, the fixity to the teeth is not sufficient, and the whitening effect may not be sustained. When the number average molecular weight is more than 1 million, the viscosity of the preparation increases and the operability is impaired. May be. The method for measuring the number average molecular weight is not particularly limited. For example, the number average molecular weight can be determined by the gel permeation chromatograph low angle light scattering method (GPC-LALLS method) using polystyrene as a standard substance under the following conditions. it can.
Column: Tosoh Biosep G5000 PW XL , 7.8 mm × 30 cm
Moving layer: 0.1 mol / L sodium phosphate buffer (pH 7.0)
Flow rate: 0.5 mL / min
Column temperature: 40 ° C
また、ポリリジンの配合量は組成物全体の0.01〜20質量%が好ましく、0.5〜10質量%が更に好ましい。ポリリジンの配合量が、0.01質量%未満の場合には、組成物の歯牙への吸着性と持続性が低く、金属酸化物が歯に長時間安定して吸着できない場合がある。また20質量%を超える場合には、組成物の粘度が高くなり、十分な量の金属酸化物が歯に吸着できない場合がある。 Moreover, 0.01-20 mass% of the whole composition is preferable, and, as for the compounding quantity of polylysine, 0.5-10 mass% is still more preferable. When the blending amount of polylysine is less than 0.01% by mass, the adsorptivity and persistence of the composition on the teeth are low, and the metal oxide may not be stably adsorbed on the teeth for a long time. On the other hand, when it exceeds 20% by mass, the viscosity of the composition increases, and a sufficient amount of metal oxide may not be adsorbed on the teeth.
本発明の歯牙美白用組成物は、上記成分に加え、更に歯牙に長時間適用でき、且つ歯牙美白用組成物の口腔全体への溶け出しを防ぐゲル化剤をその形態に応じて配合することができる。 In addition to the above components, the composition for tooth whitening of the present invention is further formulated with a gelling agent that can be applied to teeth for a long time and prevents the tooth whitening composition from dissolving into the entire oral cavity according to its form. Can do.
本発明に用いられるゲル化剤は特に制限されないが、ポリアクリル酸又はその塩、カルボキシビニルポリマー、酢酸ビニル・ビニルピロリドン共重合体、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、ヒドロキシプロピルセルロース等のセルロース誘導体、ポリビニルピロリドン、ポリビニルアルコール、キサンタンガム、カラギーナン、アルギン酸塩が好適に用いられ、これらの中から選ばれる1種又は2種以上を配合し得る。 The gelling agent used in the present invention is not particularly limited, but polyacrylic acid or a salt thereof, carboxyvinyl polymer, vinyl acetate / vinyl pyrrolidone copolymer, cellulose derivatives such as sodium carboxymethylcellulose, hydroxyethylcellulose, hydroxypropylcellulose, polyvinyl Pyrrolidone, polyvinyl alcohol, xanthan gum, carrageenan, and alginate are preferably used, and one or more selected from these can be blended.
上記ゲル化剤の配合量は、組成物全体の0.1〜10質量%が好適であり、特に0.5〜5質量%が望ましい。配合量が10質量%を超えるとゲル化剤が十分に溶けきらず、製剤が不均一になるだけでなく、製剤の歯面への吸着を阻害する場合がある。配合量が0.1質量%未満の場合は、ゲルの溶け出しによる口中の粘つき等の違和感が生じる場合がある。 0.1-10 mass% of the whole composition is suitable for the compounding quantity of the said gelatinizer, and 0.5-5 mass% is especially desirable. If the blending amount exceeds 10% by mass, the gelling agent may not be sufficiently dissolved, resulting in not only a non-uniform preparation but also inhibition of the preparation on the tooth surface. When the blending amount is less than 0.1% by mass, an uncomfortable feeling such as stickiness in the mouth due to gel dissolution may occur.
本発明の歯牙美白用組成物には、更に必要に応じて適宜、他の成分を配合することができる。
例えば、乳化、分散などの目的で、界面活性剤として、アニオン性界面活性剤、ノニオン性界面活性剤や両性イオン界面活性剤の1種又は2種以上を併用することができる。
この場合、アニオン性界面活性剤としては、ラウリル硫酸ナトリウム、ミリスチル硫酸ナトリウム、セチル硫酸ナトリウムなどのアルキル硫酸ナトリウム、N−ラウロイルグルタミン酸ナトリウム、N−パルミトイルグルタミン酸ナトリウムなどのN−アシルグルタミン酸ナトリウム、N−ラウロイルサルコシンナトリウム、N−ミリストイルサルコシンナトリウムなどのN−アシルサルコシンナトリウム、N−ラウロイルメチルタウリンナトリウム、N−ミリストイルメチルタウリンナトリウムなどのN−メチル−N−アシルタウリンナトリウム、N−メチル−N−アシルアラニンナトリウム、ラウリルベンゼンスルホン酸ナトリウム、水素添加ココナツ脂肪酸モノグリセリドモノ硫酸ナトリウム、ラウリルスルホ酢酸ナトリウム、α−オレフィンスルホン酸ナトリウム、ラウリルPOE硫酸ナトリウム、ラウリルPOE酢酸ナトリウム、ラウリルPOEリン酸ナトリウム、ステアリルPOEリン酸ナトリウム等が用いられる。In the tooth whitening composition of the present invention, other components can be appropriately blended as necessary.
For example, for the purpose of emulsification and dispersion, one or more of an anionic surfactant, a nonionic surfactant and a zwitterionic surfactant can be used in combination as the surfactant.
In this case, anionic surfactants include sodium alkyl sulfates such as sodium lauryl sulfate, sodium myristyl sulfate and sodium cetyl sulfate, sodium N-acyl glutamate such as sodium N-lauroyl glutamate, sodium N-palmitoyl glutamate, and N-lauroyl. N-acyl sarcosine sodium, such as sarcosine sodium, N-myristoyl sarcosine sodium, N-methyl-N-acyl taurine sodium, N-methyl-N-acylalanine sodium, such as N-lauroylmethyl taurine sodium, N-myristoyl methyl taurine sodium Sodium laurylbenzene sulfonate, hydrogenated coconut fatty acid monoglyceride sodium monosulfate, sodium lauryl sulfoacetate, α-o Sodium fins sulfonate, lauryl POE sodium sulfate, sodium lauryl POE acetate, sodium lauryl POE phosphate, stearyl POE sodium phosphate and the like are used.
ノニオン性界面活性剤としては、ステアリン酸モノグリセリル、ラウリン酸デカグリセリルなどのグリセリン脂肪酸エステル、ショ糖脂肪酸エステル、マルトース脂肪酸エステル、ラクトース脂肪酸エステルなどの糖脂肪酸エステル、マルチトール脂肪酸エステル、ラクチトール脂肪酸エステルなどの糖アルコール脂肪酸エステル、ポリオキシエチレンソルビタンモノラウレート、ポリオキシエチレンソルビタンモノステアレートなどのポリオキシエチレンソルビタン脂肪酸エステル、ポリオキシエチレン硬化ヒマシ油等のポリオキシエチレン脂肪酸エステル、ミリスチン酸モノ又はジエタノールアミドなどの脂肪酸エタノールアミド、ソルビタン脂肪酸エステル、ポリオキシエチレン高級アルコールエーテル、ポリオキシエチレンポリオキシプロピレン共重合体、ポリオキシエチレンポリオキシプロピレン脂肪酸エステル等が用いられる。 Nonionic surfactants include glycerin fatty acid esters such as monoglyceryl stearate and decaglyceryl laurate, sugar fatty acid esters such as sucrose fatty acid ester, maltose fatty acid ester and lactose fatty acid ester, maltitol fatty acid ester, and lactitol fatty acid ester. Sugar alcohol fatty acid esters, polyoxyethylene sorbitan monolaurate, polyoxyethylene sorbitan fatty acid esters such as polyoxyethylene sorbitan monostearate, polyoxyethylene fatty acid esters such as polyoxyethylene hydrogenated castor oil, myristic acid mono- or diethanolamide Fatty acid ethanolamide, sorbitan fatty acid ester, polyoxyethylene higher alcohol ether, polyoxyethylene polyoxy Propylene copolymer, polyoxyethylene polyoxypropylene fatty acid ester or the like is used.
両性イオン界面活性剤としては、ラウリルジメチルアミノ酢酸ベタインなどのアルキルジメチルアミノ酢酸ベタイン、N−ラウリルジアミノエチルグリシン、N−ミリスチルジアミノエチルグリシンなどのN−アルキルジアミノエチルグリシン、N−アルキル−N−カルボキシメチルアンモニウムベタイン、2−アルキル−1−ヒドロキシエチルイミダゾリンベタインナトリウム等が用いられる。 Zwitterionic surfactants include alkyldimethylaminoacetic acid betaines such as lauryldimethylaminoacetic acid betaine, N-alkyldiaminoethylglycine such as N-lauryldiaminoethylglycine, N-myristyldiaminoethylglycine, and N-alkyl-N-carboxyl. Methyl ammonium betaine, 2-alkyl-1-hydroxyethyl imidazoline betaine sodium and the like are used.
更に、本発明においては、有効成分として、デキストラナーゼ、ムタナーゼ、アミラーゼ、プロテアーゼ、スーパーオキサイドディスムターゼなどの酵素、ピロリン酸カリウム、トリポリリン酸ナトリウム、メタリン酸ナトリウムなどの水溶性ポリリン酸塩、アラントイン、ジヒドロコレスタノール、グリチルリチン酸類、グリチルレチン酸、ε−アミノカプロン酸、トラネキサム酸、ビサボロール、イソプロピルメチルフェノール、塩化ナトリウム、トリクロサン、クロルヘキシジン塩類、塩化セチルピリジニウム、塩化ベンゼトニウム、塩化ベンザルコニウム、アスコルビン酸及びその塩類、トコフェロール、オウゴン、オオバク、ローズマリー、チョウジ、タイムなどの生薬抽出物等の有効成分の1種又は2種以上を配合し得る。 Further, in the present invention, active ingredients include enzymes such as dextranase, mutanase, amylase, protease, superoxide dismutase, water-soluble polyphosphates such as potassium pyrophosphate, sodium tripolyphosphate, sodium metaphosphate, allantoin, dihydro Cholestanol, glycyrrhizic acid, glycyrrhetinic acid, ε-aminocaproic acid, tranexamic acid, bisabolol, isopropylmethylphenol, sodium chloride, triclosan, chlorhexidine salts, cetylpyridinium chloride, benzethonium chloride, benzalkonium chloride, ascorbic acid and its salts, tocopherol One or two or more active ingredients such as herbal extracts such as green grass, green grass, rosemary, clove, and thyme can be blended.
本発明の歯牙美白用組成物には、更に、アネトール、カルボン、ペパーミント油、スペアミント油などの香料、安息香酸及びそのナトリウム塩、パラベン類などの防腐剤、赤色3号、赤色104号、黄色4号、青色1号、緑色3号、雲母チタン、弁柄などの色素又は着色剤、サッカリン及びそのナトリウム塩、ステビオサイド、グリチルリチン、アスパルテームなどの甘味剤等を配合し得る。 The composition for tooth whitening of the present invention further includes perfumes such as anethole, carvone, peppermint oil, spearmint oil, preservatives such as benzoic acid and its sodium salt, parabens, red No. 3, red No. 104, yellow 4 No. 1, Blue No. 1, Green No. 3, mica titanium, a pigment or coloring agent such as petite, sweeteners such as saccharin and its sodium salt, stevioside, glycyrrhizin, aspartame and the like.
歯牙美白用組成物のpHは、口腔内及び人体に安全性上問題ない範囲であれば、特に限定されるものではないが、望ましくは歯牙美白用組成物を精製水で10倍希釈した時のpHが4〜10であり、更に望ましくはpHが5.5〜9である。pH4未満の場合には適用時間によっては脱灰の懸念があり、pH10を超える場合には、歯肉に触れた場合、粘膜剥離等の懸念がある。pH調整剤として、酢酸、塩酸、硫酸、硝酸、クエン酸、リン酸、水酸化ナトリウム、水酸化カリウム、酢酸ナトリウム、炭酸ナトリウム、クエン酸ナトリウム、クエン酸水素ナトリウム、リン酸ナトリウム、リン酸水素ナトリウム等を配合し得る。 The pH of the tooth whitening composition is not particularly limited as long as it is within the range of safety in the oral cavity and human body. Desirably, the tooth whitening composition is diluted 10 times with purified water. The pH is 4-10, more preferably the pH is 5.5-9. When the pH is less than 4, there is a concern of decalcification depending on the application time, and when the pH exceeds 10, when the gingiva is touched, there is a concern such as mucosal detachment. As pH adjusters, acetic acid, hydrochloric acid, sulfuric acid, nitric acid, citric acid, phosphoric acid, sodium hydroxide, potassium hydroxide, sodium acetate, sodium carbonate, sodium citrate, sodium hydrogen citrate, sodium phosphate, sodium hydrogen phosphate Etc. may be blended.
上記歯牙美白用組成物は、ペースト状、ゲル状、液状等の形態に調製されるが、その形態に応じて、歯牙への保持・固定専用の適用用具と併せて適用することが好ましいが、本発明の歯牙美白用組成物と併用して使用される歯牙への保持・固定専用の適用用具は、歯牙美白用組成物の歯牙への確実な適用、固定を補助すると共に、使用中の歯牙美白用組成物の歯肉、舌及び口腔粘膜への溶出を抑え、不快な使用感や唾液の誘発を防ぎ、更に唾液の侵入や咬合、咀嚼、その他物理的な刺激による歯牙美白用組成物の希釈や歯牙からの離脱を防ぐ目的で使用される。用具の素材及び形状については、上記目的を達成できるものであれば特に限定されないが、水不溶性の素材で作られたテープ、シート、フィルム、マウストレー、マウスピース、スポンジ、印象材、パック材、又は歯列に成型した歯のカバーが好適に用いられる。 The tooth whitening composition is prepared in the form of a paste, gel, liquid, etc., but depending on the form, it is preferably applied together with an application tool dedicated to holding and fixing to the tooth, The application tool dedicated to holding and fixing the tooth used in combination with the tooth whitening composition of the present invention assists the reliable application and fixing of the tooth whitening composition to the tooth, and the tooth in use Suppresses elution of the whitening composition into the gingiva, tongue and oral mucosa, prevents unpleasant feeling of use and induction of saliva, and further dilutes the tooth whitening composition by saliva intrusion, occlusion, chewing and other physical stimuli Used to prevent detachment from teeth. The material and shape of the tool are not particularly limited as long as the above object can be achieved, but tapes, sheets, films, mouth trays, mouthpieces, sponges, impression materials, pack materials made of water-insoluble materials, Alternatively, a tooth cover molded into a dentition is preferably used.
上記適用用具の厚みは、口腔着用時に違和感のない0.01〜5mmが好ましく、特にテープ、シート、フィルムについては、0.01〜2mmが望ましい。 The thickness of the application tool is preferably 0.01 to 5 mm, which does not give a sense of incongruity when worn on the oral cavity, and is particularly preferably 0.01 to 2 mm for tapes, sheets and films.
上記用具の素材については、口腔適用時のフィット感に優れ、唾液の発生を抑えることで製剤の長時間適用を可能にするポリエチレン、発泡ポリエチレン、ポリプロピレン、発泡ポリプロピレン、ポリエステル、ポリウレタン、レーヨン、パルプ、綿、絹、紙、多糖フィルム、金属箔等の1種又は2種以上を用いるのが好ましく、特にポリエチレン、発泡ポリエチレン、ポリプロピレン、発泡ポリプロピレン、ポリエステル、ポリウレタン、レーヨン、水難溶性プルランフィルムが良い。水難溶性プルランフィルムはプルランをフィルム化したもので、上記(B)成分のプルランには含まれない。更に、口腔粘膜及び舌と接する側の材質を親水性、吸水性の高い素材、例えばレーヨン、パルプ、綿、絹、紙等を使った織布又は不織布で構成することにより、口中で発生した唾液を吸収し保持するため、使用感に優れており好ましい。この場合、歯牙美白用組成物を保持する側には、ポリエチレン、ポリプロピレン、ポリエステル、ポリウレタン等の水不透過性フィルムを組み合わせることで、歯牙美白用組成物の適用用具への吸着、浸透を防ぐこともできる。 About the material of the above-mentioned tool, polyethylene, foamed polyethylene, polypropylene, foamed polypropylene, polyester, polyurethane, rayon, pulp, which has excellent fit when applied to the oral cavity and enables long-term application of the preparation by suppressing the generation of saliva One or more of cotton, silk, paper, polysaccharide film, metal foil and the like are preferably used, and polyethylene, foamed polyethylene, polypropylene, foamed polypropylene, polyester, polyurethane, rayon, poorly water-soluble pullulan film are particularly preferable. The poorly water-soluble pullulan film is a film of pullulan and is not included in the pullulan component (B). In addition, saliva generated in the mouth by making the material on the side in contact with the oral mucosa and tongue with a hydrophilic or highly water-absorbing material such as woven or non-woven fabric using rayon, pulp, cotton, silk, paper, etc. It is preferable because it absorbs and retains and is excellent in use feeling. In this case, by adhering the water-impermeable film such as polyethylene, polypropylene, polyester, polyurethane, etc. on the side holding the tooth whitening composition, it prevents adsorption and penetration of the tooth whitening composition to the application tool. You can also.
一方、シリコーンゴム、天然ゴム等の可塑性樹脂及び酢酸ビニル樹脂、アクリル樹脂、エチレン−酢酸ビニル共重合体等の熱可塑性樹脂からなるトレー又はマウスピースは、変形の自由度が高く、使用者の歯列、歯型にフィットさせやすいため、密着性、固定性に優れており、より長時間の歯牙美白用組成物の歯牙への適用を目的とする場合に適している。 On the other hand, trays or mouthpieces made of plastic resins such as silicone rubber and natural rubber, and thermoplastic resins such as vinyl acetate resin, acrylic resin, and ethylene-vinyl acetate copolymer have a high degree of freedom of deformation, and the user's teeth Since it is easy to fit to a row and a tooth shape, it has excellent adhesion and fixability, and is suitable for the purpose of applying a tooth whitening composition to a tooth for a longer time.
更に、粘度が低く歯牙への粘着性の弱いゲル組成物を併用する場合には、製剤を含浸させたスポンジや、レーヨン、綿、パルプ等の吸水性樹脂を歯のカバー、トレー等の内側に敷き詰め、これを咬み続けることで、適量のゲル組成物を歯牙に適用することもできる。 Furthermore, when using a gel composition with low viscosity and low adhesiveness to teeth, a sponge impregnated with the preparation, or a water-absorbing resin such as rayon, cotton, pulp, etc. on the inside of the tooth cover, tray, etc. An appropriate amount of the gel composition can be applied to the teeth by spreading and continuing to bite.
なお、適用回数、時間等は適宜選定されるが、通常、1日1〜6回、特に1〜3回で、1回1〜10分、特に1〜3分である。 In addition, although the application frequency, time, etc. are selected suitably, it is 1-6 times a day normally, especially 1-3 times, 1-10 minutes once, especially 1-3 minutes.
以下、実施例及び比較例を示し、本発明を具体的に説明するが、本発明は下記実施例に制限されるものではない。なお、各例中の%はいずれも質量%である。また、下記例で平均粒子径、重量平均分子量、数平均分子量、窒素分の測定は上述した通りである。また、下記実施例及び比較例において、チッソ(株)製ポリリジン粉末を用いた例があるが、これは50%粉末であるので、その配合量は、純分換算したものを示した。
製剤の調製
全原料を秤量し、ニーダーに投入後、4kPaまで減圧し、組成物が均一になるまで混合して歯牙美白用組成物を調製した。なお、pHは精製水で10倍希釈した時の25℃における1分後のpHをpHメーター(東亜ディーケーケー(株)製、HM−26S)で測定し、pH5.5〜9.0になるように必要に応じて水酸化ナトリウム又は塩酸を用いて調整した。EXAMPLES Hereinafter, although an Example and a comparative example are shown and this invention is demonstrated concretely, this invention is not restrict | limited to the following Example. In addition, all% in each example is the mass%. Moreover, the measurement of an average particle diameter, a weight average molecular weight, a number average molecular weight, and a nitrogen content is as above-mentioned in the following example. Moreover, in the following Examples and Comparative Examples, there is an example using a polylysine powder manufactured by Chisso Corporation. Since this is a 50% powder, the blending amount is shown as a pure component.
Preparation of Formulation All raw materials were weighed, put into a kneader, decompressed to 4 kPa, and mixed until the composition became uniform to prepare a tooth whitening composition. In addition, pH is measured with a pH meter (HM-26S, manufactured by Toa DKK Co., Ltd.) after 1 minute at 25 ° C. when diluted 10-fold with purified water, and becomes pH 5.5 to 9.0. If necessary, it was adjusted using sodium hydroxide or hydrochloric acid.
シートの作製
加熱したポリエチレンフィルム(低密度ポリエチレン、厚さ10μm、東ソー(株)製、商品グレード;212)を、ポリプロピレン不織布(ポリプロピレン100%、スパンボンド、目付40g/m2、表面エンボス加工、出光石油化学(株)製、商品グレード;出光RN2040)とレーヨン/ポリプロピレン不織布(レーヨン/ポリプロピレン=70/30、スパンレース、目付40g/m2、シンワ(株)製、商品グレード;7140−6)で挟んで熱融着させて厚さ0.5mmの3層不織布シートを作製した。この3層不織布シートのレーヨン/ポリプロピレン不織布面側と、フェイシングフィルム(ポリエチレンテレフタレート100%、片面シリコンコート、厚さ50μm、東レフィルム加工(株)製、商品グレード;セラピールBK(S)#50)のシリコンコート面の間に、トータルの厚みが1mmになるように展延機(花栄機械工業製、ロールサンドコーター)を用いて歯牙美白用組成物を塗膏した。その後、上下顎の左右1〜3番の歯の唇面、舌面を覆える大きさ(60mm×25mm)になるように歯牙美白用組成物を塗膏したシートを型抜きし、上下顎の歯列に貼付可能なシートを作製した。 Preparation of sheet Heated polyethylene film (low density polyethylene, thickness 10 μm, manufactured by Tosoh Corporation, product grade; 212), polypropylene nonwoven fabric (100% polypropylene, spunbond, basis weight 40 g / m 2 , surface embossing, Idemitsu Petrochemical Co., Ltd., product grade; Idemitsu RN2040) and rayon / polypropylene nonwoven fabric (rayon / polypropylene = 70/30, spun lace, basis weight 40 g / m 2 , Shinwa Co., Ltd., product grade: 7140-6) A three-layer nonwoven fabric sheet having a thickness of 0.5 mm was produced by sandwiching and heat-sealing. Rayon / polypropylene nonwoven side of this three-layer nonwoven sheet and facing film (polyethylene terephthalate 100%, single-sided silicon coat, thickness 50 μm, manufactured by Toray Film Processing Co., Ltd., product grade; Therapy BK (S) # 50) The tooth whitening composition was coated between the silicon coated surfaces using a spreader (manufactured by Hanae Machinery Co., Ltd., roll sand coater) so that the total thickness was 1 mm. After that, the sheet coated with the tooth whitening composition was cut out so that the lip surface and the tongue surface of the left and right third to third teeth of the upper and lower jaws could be covered (60 mm × 25 mm). A sheet that can be attached to the dentition was prepared.
[実施例1〜10、比較例1〜4]
予め色差L*a*b*を測定したヒト抜去歯の上に、表1に示した組成物を上記の方法により塗膏したシートをのせ、37℃,3分間恒温槽中に静置後、シートを剥がし、ゲルをティッシュで軽く拭き取って水洗した後、人工唾液中に移した。人工唾液中に3時間浸漬後、色差L*a*b*を測定してΔEを求めた。色差は分光測色計(ミノルタ(株)製、CM−2022)を用いて測定した。なお、人工唾液の組成は以下の通りである。
塩化カルシウム・二水塩 0.2205g
リン酸二水素カリウム 0.6805g
塩化ナトリウム 5.8440g
酢酸 6.0g
NaOH(pH調整剤) 適量
水 残
計 1,000mL
・白色化効果
ΔE*(1)=((L*1−L*0)2+(a*1−a*0)2+(b*1−b*0)2)1/2
・白色化効果の持続性
ΔE*(2)=((L*2−L*0)2+(a*2−a*0)2+(b*2−b*0)2)1/2
なお、L*0、a*0、b*0は初期L*a*b*値を表し、同様にL*1、a*1、b*1、L*2、a*2、b*2はそれぞれ白色化操作後のL*a*b*値、人工唾液浸漬後のL*a*b*値である。
評価基準
白色化効果 ◎:ΔE*(1)が7.0以上
○:ΔE*(1)が5.0以上〜7.0未満
△:ΔE*(1)が3.0以上〜5.0未満
×:ΔE*(1)が3.0未満
白色化効果の持続性 ◎:ΔE*(2)が6.0以上
○:ΔE*(2)が4.0以上〜6.0未満
△:ΔE*(2)が3.0以上〜4.0未満
×:ΔE*(2)が3.0未満
結果を表1に示す。[Examples 1 to 10, Comparative Examples 1 to 4]
On the human extracted tooth whose color difference L * a * b * was measured in advance, a sheet coated with the composition shown in Table 1 by the above method was placed, and left in a constant temperature bath at 37 ° C. for 3 minutes. The sheet was peeled off, the gel was lightly wiped with a tissue, washed with water, and then transferred into artificial saliva. After immersion in artificial saliva for 3 hours, the color difference L * a * b * was measured to determine ΔE. The color difference was measured using a spectrocolorimeter (Minolta, CM-2022). The composition of artificial saliva is as follows.
Calcium chloride dihydrate 0.2205g
Potassium dihydrogen phosphate 0.6805g
Sodium chloride 5.8440g
Acetic acid 6.0g
NaOH (pH adjuster) appropriate amount
Water remaining
1,000 mL in total
Whitening effect ΔE * (1) = ((L * 1-L * 0) 2 + (a * 1-a * 0) 2 + (b * 1-b * 0) 2 ) 1/2
Persistence of whitening effect ΔE * (2) = ((L * 2-L * 0) 2 + (a * 2-a * 0) 2 + (b * 2-b * 0) 2 ) 1/2
Note that L * 0, a * 0, and b * 0 represent initial L * a * b * values. Similarly, L * 1, a * 1, b * 1, L * 2, a * 2, b * 2 the L * a * b * value after whitening operation respectively, the L * a * b * value after artificial saliva immersion.
Evaluation standard whitening effect A: ΔE * (1) is 7.0 or more
○: ΔE * (1) is 5.0 or more and less than 7.0
Δ: ΔE * (1) is 3.0 or more and less than 5.0
X: ΔE * (1) is less than 3.0 Persistence of whitening effect A: ΔE * (2) is 6.0 or more
○: ΔE * (2) is 4.0 or more and less than 6.0
Δ: ΔE * (2) is 3.0 or more and less than 4.0
X: ΔE * (2) is less than 3.0 The results are shown in Table 1.
[実施例11]
予め下記歯牙美白用組成物1が2.0g塗布された、前歯左3番から右3番の唇面を覆える発泡ポリエチレン製シート(積水化学工業(株)製ボラーラXL−IF08008、15mm×60mm×厚さ800μm)を歯牙の唇面に貼付した。前述の実施例1〜10、比較例1〜4と同様の方法により評価したところ白色化効果は◎、白色化効果の持続性は◎であった。
歯牙美白用組成物1(ペースト状)
二酸化チタン 3.0%
(石原産業(株)タイペークCR−50、平均粒子径0.25μm)
プルラン((株)林原商事、PF−2、重量平均分子量20万) 10.0
ポリリジン(チッソ(株)、ポリリジン粉末、数平均分子量4400) 2.5
カルボキシメチルセルロースナトリウム 0.5
(ダイセル化学工業(株)製、商品名CMCダイセル−1150)
70%ソルビトール 30.0
プロピレングリコール 3.0
サッカリンナトリウム 0.2
メチルパラベン 0.1
香料 1.0
精製水 バランス
計 100.0%[Example 11]
A foamed polyethylene sheet (Borara XL-IF08008 manufactured by Sekisui Chemical Co., Ltd., 15 mm x 60 mm) that covers the lip of the front teeth left 3 to right 3 with 2.0 g of the following tooth whitening composition 1 applied in advance. X thickness 800 μm) was applied to the labial surface of the tooth. When evaluated in the same manner as in Examples 1 to 10 and Comparative Examples 1 to 4, the whitening effect was ◎, and the sustainability of the whitening effect was ◎.
Tooth whitening composition 1 (paste)
Titanium dioxide 3.0%
(Ishihara Sangyo Co., Ltd. Taipei CR-50, average particle size 0.25 μm)
Pullulan (Hayashibara Corporation, PF-2, weight average molecular weight 200,000) 10.0
Polylysine (Chisso Corporation, polylysine powder, number average molecular weight 4400) 2.5
Sodium carboxymethylcellulose 0.5
(Daicel Chemical Industries, trade name CMC Daicel-1150)
70% sorbitol 30.0
Propylene glycol 3.0
Saccharin sodium 0.2
Methylparaben 0.1
Fragrance 1.0
Purified water balance
Total 100.0%
[実施例12]
予め下記歯牙美白用組成物2が2.0g塗布された、前歯左3番から右3番の唇面を覆えるポリウレタンフィルム(シーダム(株)製、DUS2124−CDB、15mm×60mm×厚さ50μm)を歯牙の唇面に貼付した。前述の実施例1〜10、比較例1〜4と同様の方法により評価したところ白色化効果は◎、白色化効果の持続性は○であった。
歯牙美白用組成物2(ゲル状)
二酸化チタン 4.0%
(石原テクノ(株)TTO−51(A)、平均粒子径0.02μm)
プルラン(昭光通商(株)、P−800、重量平均分子量79万) 3.0
カチオン化セルロース 0.3
(日本NSC(株)、窒素分2%、重量平均分子量30万)
キサンタンガム 0.2
(三栄源エフ・エフ・アイ(株)製、商品名サンエースNXG−S)
ポリアクリル酸ナトリウム 0.6
(日本純薬(株)製、商品名アロンビスSS)
ブチルパラベン 0.1
70%ソルビトール 23.0
プロピレングリコール 5.0
安息香酸ナトリウム 0.2
香料 1.0
精製水 バランス
計 100.0%[Example 12]
Polyurethane film (made by Sea Dam Co., Ltd., DUS2124-CDB, 15 mm × 60 mm × thickness 50 μm), which is coated with 2.0 g of the following tooth whitening composition 2 in advance and covers the lip surfaces of the front teeth left 3 to right 3 ) Was affixed to the lips of the teeth. When evaluated in the same manner as in Examples 1 to 10 and Comparative Examples 1 to 4, the whitening effect was ◎ and the whitening effect persistence was ○.
Tooth whitening composition 2 (gel)
Titanium dioxide 4.0%
(Ishihara Techno Co., Ltd. TTO-51 (A), average particle size 0.02 μm)
Pullulan (Shoko Tsusho Co., Ltd., P-800, weight average molecular weight 790,000) 3.0
Cationized cellulose 0.3
(Japan NSC Co., Ltd., nitrogen content 2%, weight average molecular weight 300,000)
Xanthan gum 0.2
(Product name: Sanace NXG-S, manufactured by San-Ei Gen FFI Co., Ltd.)
Sodium polyacrylate 0.6
(Nippon Pure Chemicals, trade name Aronbis SS)
Butylparaben 0.1
70% sorbitol 23.0
Propylene glycol 5.0
Sodium benzoate 0.2
Fragrance 1.0
Purified water balance
Total 100.0%
[実施例13]
予め下記歯牙美白用組成物3が0.2g塗布された、歯1本ずつの形をしたポリエチレン製フィルム(東レ(株)製軟質PE、10mm×15mm×厚さ25μm)を色の気になる歯だけに貼付した。前述の実施例1〜10、比較例1〜4と同様の方法により評価したところ白色化効果は◎、白色化効果の持続性は◎であった。
歯牙美白用組成物3(ゲル状)
酸化ジルコニウム(日本電工、N−PC、平均粒子径0.02μm) 0.5%
二酸化チタン 3.0
(石原テクノ(株)TTO−51(A)、平均粒子径0.02μm)
プルラン(昭光通商(株)、P−400、重量平均分子量40万) 5.0
リゾチーム(和光純薬工業(株)、リゾチーム、分子量14400) 0.1
ポリリジン(チッソ(株)、ポリリジン粉末、数平均分子量4400) 1.5
グリセリン 15.0
ポリオキシエチレン(60モル)硬化ヒマシ油 1.0
キサンタンガム 0.2
(三栄源エフ・エフ・アイ(株)製、商品名サンエースNXG−S)
フッ化ナトリウム 0.2
香料 1.0
サッカリンナトリウム 0.1
精製水 バランス
計 100.0%[Example 13]
A polyethylene film (soft PE manufactured by Toray Industries, Inc., 10 mm × 15 mm × 25 μm thick) in which 0.2 g of the following tooth whitening composition 3 is applied in advance and each tooth is shaped Affixed only to the teeth. When evaluated in the same manner as in Examples 1 to 10 and Comparative Examples 1 to 4, the whitening effect was ◎, and the sustainability of the whitening effect was ◎.
Teeth whitening composition 3 (gel)
Zirconium oxide (Nippon Denko, N-PC, average particle size 0.02 μm) 0.5%
Titanium dioxide 3.0
(Ishihara Techno Co., Ltd. TTO-51 (A), average particle size 0.02 μm)
Pullulan (Shoko Tsusho Co., Ltd., P-400, weight average molecular weight 400,000) 5.0
Lysozyme (Wako Pure Chemical Industries, Ltd., lysozyme, molecular weight 14400) 0.1
Polylysine (Chisso Corporation, polylysine powder, number average molecular weight 4400) 1.5
Glycerin 15.0
Polyoxyethylene (60 mol) hydrogenated castor oil 1.0
Xanthan gum 0.2
(Product name: Sanace NXG-S, manufactured by San-Ei Gen FFI Co., Ltd.)
Sodium fluoride 0.2
Fragrance 1.0
Saccharin sodium 0.1
Purified water balance
Total 100.0%
[実施例14]
下記歯牙美白用組成物4を1.0g筆で前歯左3番から右3番の歯の唇面に塗布後、上からポリプロピレン製フィルム(東レ(株)製軟質PP、15mm×60mm×厚さ100μm)を貼付した。前述の実施例1〜10、比較例1〜4と同様の方法により評価したところ白色化効果は◎、白色化効果の持続性は◎であった。
歯牙美白用組成物4(液状)
酸化アルミニウム 2.0%
(メラー社製、商品名:純アルミナ末、平均粒子径0.06μm)
プルラン((株)林原商事、PF−2、重量平均分子量20万) 3.0
カチオン化セルロース 1.5
(日本NSC(株)、窒素分2%、重量平均分子量30万)
カラギーナン 0.1
(三栄源エフ・エフ・アイ(株)製、商品名ゲルリッチNo.3)
ポリオキシエチレン(60モル)硬化ヒマシ油 1.0
安息香酸ナトリウム 0.3
メチルパラベン 0.1
クエン酸 0.1
クエン酸ナトリウム 0.3
香料 0.5
サッカリン 0.02
精製水 バランス
計 100.0%[Example 14]
After applying the following tooth whitening composition 4 with a 1.0 g brush to the lip of the left third tooth to the right third tooth, a polypropylene film (soft PP made by Toray Industries, 15 mm x 60 mm x thickness) 100 μm) was affixed. When evaluated in the same manner as in Examples 1 to 10 and Comparative Examples 1 to 4, the whitening effect was ◎, and the sustainability of the whitening effect was ◎.
Teeth whitening composition 4 (liquid)
Aluminum oxide 2.0%
(Meller's product name: pure alumina powder, average particle size 0.06 μm)
Pullulan (Hayashibara Corporation, PF-2, weight average molecular weight 200,000) 3.0
Cationized cellulose 1.5
(Japan NSC Co., Ltd., nitrogen content 2%, weight average molecular weight 300,000)
Carrageenan 0.1
(Product name: GELRICH No. 3 manufactured by San-Ei Gen FFI Co., Ltd.)
Polyoxyethylene (60 mol) hydrogenated castor oil 1.0
Sodium benzoate 0.3
Methylparaben 0.1
Citric acid 0.1
Sodium citrate 0.3
Fragrance 0.5
Saccharin 0.02
Purified water balance
Total 100.0%
[実施例15]
エチレンビニルアセテート樹脂製のマウスピースをお湯で温めて軟化させ、噛んで各自の歯型にフィットしたマウスピースを作製した。下記歯牙美白用組成物5をマウスピースに1.0g充填し、装着した。前述の実施例1〜10、比較例1〜4と同様の方法により評価したところ白色化効果は◎、白色化効果の持続性は○であった。
歯牙美白用組成物5(ゲル状)
二酸化ケイ素 1.0%
(Huber社製、商品名Zeodent113、平均粒子径5.0μm)
プルラン(昭光通商(株)、P−50、重量平均分子量4.7万) 5.0
ポリリジン 1.2
(和光純薬工業(株)、ポリLリジン臭化水素酸塩、数平均分子量30万以上)
カルボキシメチルセルロースナトリウム 0.3
(ダイセル化学工業(株)製、商品名CMCダイセル−1150)
カラゲナン 0.2
(三栄源エフ・エフ・アイ(株)製、商品名ゲルリッチNo.3)
ソルビット 20.0
キシリット 10.0
プロピレングリコール 3.0
メチルパラベン 0.05
香料 1.0
サッカリンナトリウム 0.15
精製水 バランス
計 100.0%
[Example 15]
Mouthpieces made of ethylene vinyl acetate resin were warmed and softened with hot water and chewed to produce mouthpieces fitted to their respective tooth shapes. A mouthpiece was filled with 1.0 g of the following tooth whitening composition 5 and attached. When evaluated in the same manner as in Examples 1 to 10 and Comparative Examples 1 to 4, the whitening effect was ◎ and the whitening effect persistence was ○.
Tooth whitening composition 5 (gel)
Silicon dioxide 1.0%
(Manufactured by Huber, trade name Zeodent 113, average particle size 5.0 μm)
Pullulan (Shoko Tsusho Co., Ltd., P-50, weight average molecular weight 47,000) 5.0
Polylysine 1.2
(Wako Pure Chemical Industries, Ltd., poly L lysine hydrobromide, number average molecular weight of 300,000 or more)
Sodium carboxymethylcellulose 0.3
(Daicel Chemical Industries, trade name CMC Daicel-1150)
Carrageenan 0.2
(Product name: GELRICH No. 3 manufactured by San-Ei Gen FFI Co., Ltd.)
Sorbit 20.0
Xylit 10.0
Propylene glycol 3.0
Methylparaben 0.05
Fragrance 1.0
Saccharin sodium 0.15
Purified water balance
Total 100.0%
Claims (3)
(B)プルラン、
(C)リゾチーム、カチオン化セルロース、ポリリジンから選ばれる1種又は2種以上
を含有することを特徴とする歯牙美白用組成物。(A) One or more selected from titanium dioxide, silicon dioxide, zinc oxide, aluminum oxide, magnesium oxide, zirconium oxide,
(B) Pullulan,
(C) A tooth whitening composition comprising one or more selected from lysozyme, cationized cellulose, and polylysine.
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Cited By (1)
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KR20150057718A (en) * | 2013-11-20 | 2015-05-28 | 주식회사 엘지생활건강 | Solid coating preparation for tooth whitening |
Families Citing this family (10)
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US7807141B2 (en) | 2003-09-08 | 2010-10-05 | E.I. Du Pont De Nemours And Company | Peptide-based oral care surface reagents for personal care |
KR100870232B1 (en) | 2006-12-07 | 2008-11-24 | 재단법인서울대학교산학협력재단 | Teeth Whitening Functional Materials Delivery System |
JP5057029B2 (en) * | 2006-12-28 | 2012-10-24 | ライオン株式会社 | Tooth cosmetic pressure transfer seal |
GB0706787D0 (en) * | 2007-04-05 | 2007-05-16 | Glaxo Group Ltd | Novel use |
US8481678B2 (en) | 2009-03-30 | 2013-07-09 | E I Du Pont De Nemours And Company | Peptide-based tooth whitening reagents |
JP5705513B2 (en) * | 2010-11-29 | 2015-04-22 | 花王株式会社 | Liquid oral composition |
CN103421329B (en) * | 2013-08-21 | 2015-07-01 | 华南理工大学 | Preparation method for antimicrobial edible film material |
CA3018963A1 (en) * | 2016-03-29 | 2017-10-05 | Safewhite, Inc. | Polyelectrolyte dental adhesives for whitening teeth and teeth components |
CN114286667A (en) | 2019-08-27 | 2022-04-05 | 狮王株式会社 | Oral composition |
CN116898741A (en) * | 2023-08-18 | 2023-10-20 | 广州品硬生物科技有限公司 | Gum repair toothpaste containing lysozyme and probiotics and preparation method thereof |
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JPH0217108A (en) * | 1988-07-05 | 1990-01-22 | Sunstar Inc | Dental coating composition |
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JPH09151123A (en) * | 1995-11-30 | 1997-06-10 | Mitsubishi Pencil Co Ltd | Tooth coating liquid |
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KR20150057718A (en) * | 2013-11-20 | 2015-05-28 | 주식회사 엘지생활건강 | Solid coating preparation for tooth whitening |
KR102012409B1 (en) * | 2013-11-20 | 2019-10-21 | 주식회사 엘지생활건강 | Solid coating preparation for tooth whitening |
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JPWO2006068011A1 (en) | 2008-06-12 |
WO2006068011A1 (en) | 2006-06-29 |
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