JPWO2018194111A1 - Oral biofilm remover and oral composition - Google Patents
Oral biofilm remover and oral composition Download PDFInfo
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- JPWO2018194111A1 JPWO2018194111A1 JP2019513676A JP2019513676A JPWO2018194111A1 JP WO2018194111 A1 JPWO2018194111 A1 JP WO2018194111A1 JP 2019513676 A JP2019513676 A JP 2019513676A JP 2019513676 A JP2019513676 A JP 2019513676A JP WO2018194111 A1 JPWO2018194111 A1 JP WO2018194111A1
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- Prior art keywords
- oral
- biofilm
- composition
- oil
- acid
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Abstract
(a)重量平均分子量が1,000以上20,000以下であるポリアクリル酸塩と、(b)アニオン性界面活性剤及び両性界面活性剤から選ばれる1種以上とからなる口腔バイオフィルム除去剤、更に好ましくは(a)/(b)が質量比として0.005〜2である上記口腔バイオフィルム除去剤。上記(a)及び(b)成分を含有する口腔用組成物、更に好ましくは(a)/(b)が質量比として0.005〜2である上記口腔用組成物。本発明によれば、優れたバイオフィルム除去効果を与え、使用感も良い口腔バイオフィルム除去剤及びこれを含有する口腔用組成物を提供できる。An oral biofilm remover comprising (a) a polyacrylate having a weight average molecular weight of 1,000 or more and 20,000 or less, and (b) at least one selected from an anionic surfactant and an amphoteric surfactant. The above-mentioned oral biofilm remover wherein (a) / (b) is more preferably 0.005 to 2 as a mass ratio. The oral composition containing the components (a) and (b), more preferably the oral composition wherein (a) / (b) has a mass ratio of 0.005 to 2. ADVANTAGE OF THE INVENTION According to this invention, the biofilm removal agent which gives the outstanding biofilm removal effect and has a good feeling of use, and the composition for oral cavity containing this can be provided.
Description
本発明は、口腔バイオフィルム除去剤及びこれを含有する口腔用組成物に関する。 The present invention relates to an oral biofilm remover and an oral composition containing the same.
口腔疾患は病原菌が原因で発症するが、この病原菌は歯面にプラーク(歯垢)を形成して口腔内に定着し、病原性を発現するため、歯周病等の口腔疾患の予防にはプラークコントロールが非常に重要である。プラークコントロールの手段としては、プラークの形成抑制や殺菌などがあるが、中でも重要なのがプラークの除去である。プラークを化学的に除去するには、グルカンやタンパクといった細菌の菌体外代謝物だけではなく、細菌凝集体、更には細菌凝集体と菌体外代謝物とで複合的に構成されたバイオフィルム構造物を効果的に除去することが非常に重要である。 Oral diseases are caused by pathogenic bacteria. These pathogenic bacteria form plaque (plaque) on the tooth surface and colonize the oral cavity, expressing pathogenicity. Therefore, to prevent oral diseases such as periodontal disease, Plaque control is very important. Means of plaque control include plaque formation suppression and sterilization, and the most important is plaque removal. In order to remove plaque chemically, not only bacterial extracellular metabolites such as glucan and protein, but also bacterial aggregates, and biofilms composed of bacterial aggregates and extracellular metabolites It is very important to remove structures effectively.
これまでに、アニオン性界面活性剤のα−オレフィンスルホン酸塩又はアルキルスルホ酢酸塩と酵素との併用によるバイオフィルム除去効果が報告されている(特許文献1;特開2015−20970号公報)。 A biofilm removal effect by using an anionic surfactant α-olefin sulfonate or alkyl sulfoacetate in combination with an enzyme has been reported (Patent Document 1; Japanese Patent Application Laid-Open No. 2015-20970).
本発明は、上記事情に鑑みなされたもので、優れたバイオフィルム除去効果を与える新たな口腔バイオフィルム除去剤及びこれを含有する口腔用組成物を提供することを目的とする。 The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a new oral biofilm remover that provides an excellent biofilm removal effect and an oral composition containing the same.
本発明者らは、上記目的を達成するため鋭意検討を行った結果、重量平均分子量が特定値以下である比較的低分子量のポリアクリル酸塩と、アニオン性界面活性剤又は両性界面活性剤とを組み合わせると、優れた口腔バイオフィルム除去作用を奏することを見出した。即ち、本発明では、(a)重量平均分子量が1,000以上20,000以下であるポリアクリル酸塩と(b)アニオン性界面活性剤及び両性界面活性剤から選ばれる1種以上とを併用することによって、バイオフィルム除去効果が優れ、使用感も良い口腔バイオフィルム除去剤が得られることを知見した。更に、上記(a)及び(b)成分を口腔用組成物に配合すると、(a)成分量が比較的少なくても、優れたバイオフィルム除去効果を与え、また、良好な使用感(口腔刺激のなさ、臭いのなさ)を付与することもできることを知見し、本発明をなすに至った。 The present inventors have conducted intensive studies to achieve the above object, and as a result, a relatively low molecular weight polyacrylate having a weight average molecular weight of a specific value or less, an anionic surfactant or an amphoteric surfactant. It has been found that when combined with, an excellent oral biofilm removing action is achieved. That is, in the present invention, (a) a polyacrylate having a weight average molecular weight of 1,000 or more and 20,000 or less and (b) one or more selected from anionic surfactants and amphoteric surfactants are used in combination. By doing so, it has been found that an oral biofilm remover having an excellent biofilm removing effect and a good feeling in use can be obtained. Furthermore, when the components (a) and (b) are blended with the oral composition, an excellent biofilm removing effect is obtained even if the amount of the component (a) is relatively small, and a good feeling in use (oral irritation) And no odor) can be imparted, and the present invention has been accomplished.
口腔用組成物用の粘結剤としては、一般的に重量平均分子量10万以上、通常は30万程度のポリアクリル酸又はその塩が用いられている。また、これに比べて低分子量(分子量約4,000〜5,500)のポリアクリル酸重合体に抗歯石作用があり、口腔用組成物への配合量は約2.5%以上がよいことが特許文献2(特公平7−29907号公報)に提案され、ポリアクリル酸を用いた具体例が示されている。一方、界面活性剤には洗浄作用や浸透、分散作用があり、わずかではあるが歯垢除去作用があると認識されているがバイオフィルムに対する作用は十分でなく、増量すると界面活性剤種によって口腔刺激や味の低下を招くことがあった。これに対して、本発明では、(a)重量平均分子量1,000以上20,000以下のポリアクリル酸塩を、界面活性剤のうちの(b)アニオン性界面活性剤及び両性界面活性剤から選ばれる1種以上と組み合わせることによって、意外にも、両者が特異的に相互作用して(b)成分によるバイオフィルム除去作用が格段に向上し、優れたバイオフィルム除去効果を付与できた。また同時に、(a)成分によって(b)成分による口腔刺激や臭い等の悪化が抑えられ、使用感も良好に保持できた。なお、重量平均分子量20,000以下のポリアクリル酸塩である(a)成分を単に使用したのでは、バイオフィルム除去効果がほとんど認められなかった(後述の比較例参照)。
上述したようにバイオフィルムは、細菌凝集体や菌体外代謝物で複合的に構成されて強固に構築され、高い抵抗性を示す構造物であるが、本発明によれば、このような強固かつ高抵抗性の付着物であるバイオフィルムが歯表面から剥がれて口腔内に分散し、高率でバイオフィルムを除去することができた。本発明の作用効果は(a)及び(b)成分の併用系に特異なものであり、後述の比較例にも示すように、ポリアクリル酸や重量平均分子量が不適切なポリアクリル酸塩を(b)成分と併用した場合にはバイオフィルム除去効果が劣っていた。As a binder for oral compositions, polyacrylic acid or a salt thereof having a weight average molecular weight of 100,000 or more, usually about 300,000 is used. In addition, a polyacrylic acid polymer having a low molecular weight (molecular weight of about 4,000 to 5,500) has an anti-calculus effect, and the compounding amount in the oral composition is preferably about 2.5% or more. Is proposed in Patent Document 2 (Japanese Patent Publication No. 7-29907), and a specific example using polyacrylic acid is shown. On the other hand, surfactants have a cleaning, penetrating, and dispersing action, and although they are recognized as having a slight plaque removing action, their action on biofilms is not sufficient. May cause irritation and reduced taste. On the other hand, in the present invention, (a) a polyacrylate having a weight average molecular weight of 1,000 to 20,000 is converted from (b) an anionic surfactant and an amphoteric surfactant among the surfactants. By combining with one or more selected ones, surprisingly, both interact specifically, and the biofilm removing action by the component (b) is remarkably improved, and an excellent biofilm removing effect can be imparted. At the same time, the component (a) suppressed the deterioration of oral irritation and odor caused by the component (b), and the sensation during use was well maintained. When the component (a), which is a polyacrylate having a weight average molecular weight of 20,000 or less, was simply used, a biofilm removing effect was hardly observed (see Comparative Examples described later).
As described above, a biofilm is a structure that is composed of bacterial aggregates and extracellular metabolites and is firmly constructed and exhibits high resistance. In addition, the biofilm, which is a highly resistant deposit, was peeled off from the tooth surface and dispersed in the oral cavity, and the biofilm could be removed at a high rate. The effect of the present invention is unique to the combination system of the components (a) and (b). As shown in the comparative examples described later, polyacrylic acid and polyacrylate having an inappropriate weight average molecular weight are used. When used in combination with the component (b), the biofilm removal effect was poor.
なお、特許文献3(特開平10−287537号公報)は、無水グルコースを構成単位とする多糖類から誘導されるポリカルボン酸又はその塩によるハイドロキシアパタイトの結晶生成抑制、特許文献4(特開2002−47160号公報)は、ポリアクリル酸塩による、フェノキシエタノール等由来の刺激の抑制であって実験例では分子量約50,000のポリアクリル酸ナトリウムが用いられている。特許文献3、4には、バイオフィルム除去に関する言及もない。特許文献3、4から、本発明の(a)及び(b)成分を併用することによる、バイオフィルム除去効果の向上は予測できない。 Patent Document 3 (Japanese Patent Application Laid-Open No. 10-287537) discloses a method of suppressing hydroxyapatite crystal formation by a polycarboxylic acid or a salt thereof derived from a polysaccharide having anhydrous glucose as a constituent unit. Japanese Patent No. 47160/1992) is a method for suppressing irritation derived from phenoxyethanol and the like by a polyacrylate. In the experimental examples, sodium polyacrylate having a molecular weight of about 50,000 is used. Patent Documents 3 and 4 do not mention biofilm removal. From Patent Documents 3 and 4, improvement in the biofilm removal effect by using the components (a) and (b) of the present invention in combination cannot be predicted.
従って、本発明は、下記の口腔バイオフィルム除去剤及び口腔用組成物を提供する。
〔1〕
(a)重量平均分子量が1,000以上20,000以下であるポリアクリル酸塩と、
(b)アニオン性界面活性剤及び両性界面活性剤から選ばれる1種以上と
からなる口腔バイオフィルム除去剤。
〔2〕
(a)/(b)が質量比として0.005〜2である〔1〕に記載の口腔バイオフィルム除去剤。
〔3〕
(a)/(b)が質量比として0.02〜1である〔2〕に記載の口腔バイオフィルム除去剤。
〔4〕
アニオン性界面活性剤が、炭素数12〜14のアルキル基を有するアルキル硫酸塩、アシルアミノ酸塩及びアシルタウリン塩から選ばれ、両性界面活性剤が、炭素数12〜14のアシル基を有するアシルアミノ酢酸ベタイン及び脂肪酸アミドプロピルベタインから選ばれる〔1〕〜〔3〕のいずれかに記載の口腔バイオフィルム除去剤。
〔5〕
(a)重量平均分子量が1,000以上20,000以下であるポリアクリル酸塩と、
(b)アニオン性界面活性剤及び両性界面活性剤から選ばれる1種以上と
を含有する口腔用組成物。
〔6〕
(a)/(b)が質量比として0.005〜2である〔5〕に記載の口腔用組成物。
〔7〕
(a)成分の含有量が0.01〜2質量%、(b)成分の含有量が0.5〜3質量%である〔5〕又は〔6〕に記載の口腔用組成物。
〔8〕
25℃におけるpH5〜9である〔5〕〜〔7〕のいずれかに記載の口腔用組成物。
〔9〕
歯磨剤組成物である〔5〕〜〔8〕のいずれかに記載の口腔用組成物。Accordingly, the present invention provides the following oral biofilm remover and oral composition.
[1]
(A) a polyacrylate having a weight average molecular weight of 1,000 to 20,000,
(B) An oral biofilm remover comprising at least one selected from anionic surfactants and amphoteric surfactants.
[2]
The oral biofilm remover according to [1], wherein (a) / (b) has a mass ratio of 0.005 to 2.
[3]
The oral biofilm remover according to [2], wherein (a) / (b) is 0.02 to 1 in terms of mass ratio.
[4]
The anionic surfactant is selected from an alkyl sulfate having an alkyl group having 12 to 14 carbon atoms, an acyl amino acid salt and an acyl taurine salt, and the amphoteric surfactant is an acyl amino acetic acid having an acyl group having 12 to 14 carbon atoms. The oral biofilm remover according to any one of [1] to [3], which is selected from betaine and fatty acid amidopropyl betaine.
[5]
(A) a polyacrylate having a weight average molecular weight of 1,000 to 20,000,
(B) an oral composition comprising at least one selected from an anionic surfactant and an amphoteric surfactant;
[6]
The oral composition according to [5], wherein (a) / (b) has a mass ratio of 0.005 to 2.
[7]
The oral composition according to [5] or [6], wherein the content of the component (a) is 0.01 to 2% by mass and the content of the component (b) is 0.5 to 3% by mass.
[8]
The oral composition according to any one of [5] to [7], which has a pH of 5 to 9 at 25 ° C.
[9]
The oral composition according to any one of [5] to [8], which is a dentifrice composition.
本発明によれば、優れたバイオフィルム除去効果を与え、使用感も良い口腔バイオフィルム除去剤及びこれを含有する口腔用組成物を提供できる。本発明の口腔バイオフィルム除去剤及び口腔用組成物は、歯周疾患の予防又は抑制用として有効である。 ADVANTAGE OF THE INVENTION According to this invention, the excellent biofilm removal effect is given, and the oral biofilm remover with a good feeling of use and the composition for oral cavity containing this can be provided. The oral biofilm remover and the oral composition of the present invention are effective for preventing or suppressing periodontal disease.
本発明の口腔バイオフィルム除去剤は、(a)重量平均分子量が1,000以上20,000以下であるポリアクリル酸塩と、(b)アニオン性界面活性剤及び両性界面活性剤から選ばれる1種以上とが有効成分である。 The oral biofilm remover of the present invention comprises: (a) a polyacrylate having a weight average molecular weight of 1,000 to 20,000, and (b) an anionic surfactant or an amphoteric surfactant. More than one species is the active ingredient.
(a)成分のポリアクリル酸塩は、重量平均分子量(Mw)が1,000以上20,000以下である。この場合、バイオフィルム除去効果の点から、重量平均分子量は1,000以上であり、また、20,000以下、好ましくは10,000以下である。重量平均分子量が1,000未満であると、バイオフィルム除去効果が劣る。20,000を超えると、バイオフィルム除去効果が低下し、十分な効果が得られない。
なお、重量平均分子量の測定は、GPC(ゲルパーミェーションクロマトグラフィー法)により、特許第5740859号公報に記載された方法及び測定条件で行った。具体的には下記に示す。
重量平均分子量の測定方法;
重量平均分子量は、ゲル浸透クロマトグラフ/多角度レーザー光散乱検出器(GPC−MALLS)を用いて測定された値であり、条件は以下の通りである。
移動相:0.3M NaClO4
NaN3水溶液カラム:TSKgelα−M 2本
プレカラム:TSKguardcolumn α
標準物質:ポリエチレングリコールThe polyacrylate salt of the component (a) has a weight average molecular weight (Mw) of 1,000 or more and 20,000 or less. In this case, the weight average molecular weight is 1,000 or more, and 20,000 or less, preferably 10,000 or less, from the viewpoint of a biofilm removing effect. When the weight average molecular weight is less than 1,000, the effect of removing the biofilm is inferior. If it exceeds 20,000, the effect of removing the biofilm decreases, and a sufficient effect cannot be obtained.
The weight average molecular weight was measured by GPC (gel permeation chromatography) under the method and measurement conditions described in Japanese Patent No. 5,740,859. The details are shown below.
Method for measuring weight average molecular weight;
The weight average molecular weight is a value measured using a gel permeation chromatograph / multi-angle laser light scattering detector (GPC-MALLS), and the conditions are as follows.
Mobile phase: 0.3 M NaClO 4
NaN 3 aqueous solution column: TSKgelα-M 2 precolumn: TSKguardcolumn α
Standard substance: polyethylene glycol
ポリアクリル酸塩は、バイオフィルム除去効果の点から直鎖状のポリアクリル酸塩が好ましい。
塩としては、一価塩が好ましく、アルカリ金属塩又はアンモニウム塩がより好ましく、更に好ましくはアルカリ金属塩、中でもナトリウム塩がよい。
なお、(a)成分に代えて、(a)成分以外のポリアクリル酸塩あるいはポリアクリル酸を使用した場合は、(b)成分と併用してもバイオフィルム除去率が悪く、また、口腔刺激性が強くなったり、臭いや味が悪くなることがあり、本発明の目的は達成されない。
このようなポリアクリル酸塩としては、市販品を使用し得る。The polyacrylate is preferably a linear polyacrylate from the viewpoint of biofilm removal effect.
As the salt, a monovalent salt is preferable, an alkali metal salt or an ammonium salt is more preferable, and an alkali metal salt, particularly a sodium salt, is more preferable.
When a polyacrylic acid salt or polyacrylic acid other than the component (a) is used instead of the component (a), the biofilm removal rate is poor even when used in combination with the component (b). In some cases, the properties may become strong, or the odor or taste may worsen, and the object of the present invention is not achieved.
A commercially available product can be used as such a polyacrylate.
(b)成分は、アニオン性界面活性剤(b1)及び両性界面活性剤(b2)から選ばれる1種又は2種以上であり、(b1)又は(b2)成分を用いても(b1)及び(b2)成分を用いてもよいが、特に使用感の点から、少なくともアニオン性界面活性剤(b1)を含むことが好ましく、(b1)成分だけを用いるか、又は(b1)及び(b2)成分を併用することが好ましい。 The component (b) is one or more selected from an anionic surfactant (b1) and an amphoteric surfactant (b2). Even when the component (b1) or (b2) is used, the components (b1) and (b2) The component (b2) may be used, but from the viewpoint of feeling in use, it is preferable to include at least the anionic surfactant (b1). Only the component (b1) is used, or the components (b1) and (b2) are used. It is preferable to use components in combination.
アニオン性界面活性剤(b1)としては、炭素数が好ましくは12〜14、特に12のアルキル基を有するアルキル硫酸塩、アシルアミノ酸塩、アシルタウリン塩が挙げられる。アシルアミノ酸塩及びアシルタウリン塩のアシル基は、それぞれ炭素数12〜14が好ましく、より好ましくは12である。
具体的にアルキル硫酸塩としては、ラウリル硫酸塩、ミリスチル硫酸塩が挙げられる。アシルアミノ酸塩としては、ラウロイルグルタミン酸塩、ミリストイルグルタミン酸塩等のアシルグルタミン酸塩、ラウロイルサルコシン塩等のアシルサルコシン塩が挙げられる。アシルタウリン塩としては、ラウロイルメチルタウリン塩が挙げられる。塩は、ナトリウム塩、カリウム塩等のアルカリ金属塩が好ましい。これらは、1種を単独で又は2種以上を組み合わせて使用できるが、特にアルキル硫酸塩、アシルサルコシン塩、アシルタウリン塩が好ましい。中でも、炭素数12の炭化水素基(ラウリル基)を有するアニオン性界面活性剤が好ましく、特にアルキル硫酸塩(ナトリウム塩)が、他の界面活性剤よりも味の点で優れることから、より好ましい。Examples of the anionic surfactant (b1) include alkyl sulfates having preferably 12 to 14 carbon atoms, particularly 12 alkyl groups, acyl amino acid salts, and acyl taurine salts. The acyl group of the acyl amino acid salt and the acyl taurine salt preferably has 12 to 14 carbon atoms, and more preferably 12 carbon atoms.
Specifically, examples of the alkyl sulfate include lauryl sulfate and myristyl sulfate. Examples of the acyl amino acid salt include acyl glutamates such as lauroyl glutamate and myristoyl glutamate, and acyl sarcosine salts such as lauroyl sarcosine salt. Examples of the acyltaurine salt include lauroylmethyltaurine salt. The salt is preferably an alkali metal salt such as a sodium salt and a potassium salt. These can be used alone or in combination of two or more, but alkyl sulfate, acyl sarcosine salt and acyl taurine salt are particularly preferable. Among them, an anionic surfactant having a hydrocarbon group having 12 carbon atoms (lauryl group) is preferable, and an alkyl sulfate (sodium salt) is more preferable because it is more excellent in taste than other surfactants. .
両性界面活性剤(b2)としては、ベタイン型が好ましく、炭素数12〜14のアシル基を有するアシルアミノ酢酸ベタイン、脂肪酸アミドプロピルベタインが挙げられる。アシルアミノ酢酸ベタインとしては、アシル基の炭素数が12〜14のものが好ましく、ラウロイルジメチルアミノ酢酸ベタインが挙げられ、脂肪酸アミドプロピルベタインとしては、ヤシ油脂肪酸アミドプロピルベタインが挙げられる。これらは、1種を単独で又は2種以上を組み合わせて使用できるが、特にアシルアミノ酢酸ベタインが好ましい。中でも、炭素数12の炭化水素基(ラウリル基)を有するものが好ましく、ラウリルジメチルアミノ酢酸ベタインが、より好ましい。 As the amphoteric surfactant (b2), betaine type is preferable, and acylaminoacetic acid betaine having an acyl group having 12 to 14 carbon atoms and fatty acid amidopropyl betaine are exemplified. As the acylaminoacetic acid betaine, one having an acyl group of 12 to 14 carbon atoms is preferable, and lauroyldimethylaminoacetic acid betaine is exemplified. As the fatty acid amidopropyl betaine, coconut oil fatty acid amidopropyl betaine is exemplified. These can be used alone or in combination of two or more, and betaine acylaminoacetate is particularly preferred. Among them, those having a hydrocarbon group having 12 carbon atoms (lauryl group) are preferable, and betaine lauryldimethylaminoacetate is more preferable.
(a)成分と(b)成分との量比を示す(a)/(b)は、質量比として0.005〜2が好ましく、より好ましくは0.005〜1、更に好ましくは0.02〜1、とりわけ好ましくは0.03〜0.5である。上記範囲内であると、バイオフィルム除去効果がより優れ、また、臭い、更には味も良く使用感がより改善する。0.005以上であると、バイオフィルム除去効果がより向上し、2以下であると、臭いや味の良い使用感を十分に保つことができる。 (A) / (b) indicating the quantitative ratio of the component (a) to the component (b) is preferably 0.005 to 2, more preferably 0.005 to 1, more preferably 0.02 as a mass ratio. To 1, particularly preferably 0.03 to 0.5. When the content is within the above range, the biofilm removing effect is more excellent, and the odor and taste are better and the feeling of use is further improved. When it is 0.005 or more, the biofilm removing effect is further improved, and when it is 2 or less, a good smell and taste of use can be sufficiently maintained.
本発明の口腔バイオフィルム除去剤は、有効成分として(a)及び(b)成分を併用し、前記成分を配合することで得ることができる。また、上記有効成分のみからなる口腔バイオフィルム除去剤として使用できるが、必要に応じて、その他の口腔用として公知の任意成分を更に含んでいてもよく、この場合、任意成分は本発明の効果を妨げない範囲で配合し得る。 The oral biofilm remover of the present invention can be obtained by using the components (a) and (b) together as an active ingredient and blending the aforementioned ingredients. In addition, although it can be used as an oral biofilm remover consisting of only the above-mentioned active ingredient, if necessary, it may further contain other optional ingredients known for oral use. Can be blended in a range that does not hinder.
本発明の口腔用組成物は、(a)及び(b)成分を有効成分として含有する。口腔用組成物は、具体的にはペースト状、ジェル状又は液状の歯磨剤組成物(練歯磨、ジェル状歯磨、液状歯磨、液体歯磨等)、洗口剤、マウススプレー、塗布剤、貼付剤が挙げられ、これらに調製することができる。中でも練歯磨が好適である。 The oral composition of the present invention contains the components (a) and (b) as active ingredients. The oral composition is specifically a paste, gel or liquid dentifrice composition (toothpaste, gel-like dentifrice, liquid dentifrice, liquid dentifrice, etc.), mouthwash, mouth spray, coating, patch And these can be prepared. Among them, toothpaste is preferred.
この場合、本発明において、口腔バイオフィルム除去の有効成分である(a)及び(b)成分は、上記特定の比率で規定することができるが、特に口腔用組成物に応用する場合は、バイオフィルム除去効果及び使用感の点から、(a)及び(b)成分の配合量がそれぞれ後述の範囲が好ましく、これらを満たす濃度で両成分を使用することが好ましい。 In this case, in the present invention, the components (a) and (b), which are active ingredients for removing oral biofilms, can be defined by the above specific ratio. From the viewpoints of the film removing effect and the feeling upon use, the amounts of the components (a) and (b) are preferably in the ranges described below, and it is preferable to use both components at concentrations satisfying these.
(a)成分の配合量は、組成物全体の0.01〜2%(質量%、以下同様)が好ましく、より好ましくは0.01〜1%、更に好ましくは0.05〜0.5%である。0.01%以上であると、十分なバイオフィルム除去効果が得られる。2%以下であると、臭いや味を良好かつ十分に維持できる。多く配合し過ぎると、臭いや味が悪くなり使用感が劣ることがある。 The compounding amount of the component (a) is preferably from 0.01 to 2% (% by mass, the same applies hereinafter) of the whole composition, more preferably from 0.01 to 1%, and still more preferably from 0.05 to 0.5%. It is. When the content is 0.01% or more, a sufficient biofilm removing effect can be obtained. When it is at most 2%, the odor and taste can be maintained well and sufficiently. If the amount is too large, the smell and taste may deteriorate and the feeling of use may be inferior.
(b)成分の配合量は、組成物全体の0.5〜3%が好ましく、より好ましくは0.5〜2%、更に好ましくは1.0〜2.0%である。0.5%以上であると、十分なバイオフィルム除去効果が得られる。3%以下であると、十分に口腔刺激を抑え、臭いや味を良好かつ十分に維持できる。多く配合し過ぎると、口腔刺激が強くなったり、臭いや味が悪くなり使用感が劣ることがある。 The amount of component (b) is preferably 0.5 to 3%, more preferably 0.5 to 2%, even more preferably 1.0 to 2.0% of the whole composition. If it is 0.5% or more, a sufficient biofilm removing effect can be obtained. When the content is 3% or less, oral irritation can be sufficiently suppressed, and odor and taste can be maintained well and sufficiently. If the amount is too large, the oral stimulus may become strong, or the odor or taste may be deteriorated, resulting in inferior usability.
本発明の口腔用組成物には、任意成分として、剤型等に応じた公知成分を必要に応じて、更に配合できる。任意成分は、本発明の効果を妨げない範囲で添加することが好ましい。具体的に歯磨剤組成物には、研磨剤、粘結剤、粘稠剤、界面活性剤としてノニオン性界面活性剤やカチオン性界面活性剤、更には、甘味剤、防腐剤、有効成分、色素、香料を配合でき、これら成分と水とを混合し、製造できる。 The oral composition of the present invention may further contain, if necessary, known components according to the dosage form and the like as optional components. The optional components are preferably added within a range that does not impair the effects of the present invention. Specifically, dentifrice compositions include abrasives, binders, thickeners, nonionic surfactants and cationic surfactants as surfactants, as well as sweeteners, preservatives, active ingredients, and pigments. , A fragrance can be blended, and these components can be mixed with water to produce.
研磨剤としては、第2リン酸水素カルシウム・無水和物や2水和物、第3リン酸カルシウム、第1リン酸カルシウム、炭酸カルシウム、ピロリン酸カルシウム、水酸化アルミニウム、アルミナ、無水ケイ酸、ケイ酸アルミニウム、不溶性メタリン酸ナトリウム、第3リン酸マグネシウム、炭酸マグネシウム、硫酸マグネシウム、ベントナイト、ケイ酸ジルコニウム、ポリメタリン酸メチル、その他合成樹脂を配合できる(配合量は通常、5〜60%、練歯磨の場合には10〜55%)。 Examples of the abrasive include dibasic calcium hydrogen phosphate / anhydride and dihydrate, tertiary calcium phosphate, monobasic calcium phosphate, calcium carbonate, calcium pyrophosphate, aluminum hydroxide, alumina, silicic anhydride, aluminum silicate, insoluble Sodium metaphosphate, tribasic magnesium phosphate, magnesium carbonate, magnesium sulfate, bentonite, zirconium silicate, polymethyl metaphosphate, and other synthetic resins can be blended (the blending amount is usually 5 to 60%, and 10% for toothpaste. ~ 55%).
特に練歯磨等のペースト状の歯磨剤組成物には、粘結剤としてアルギン酸ナトリウム、アルギン酸プロピレングリコールエステル等のアルギン酸誘導体、キサンタンガム、トラガカントガム、ジェラガム、カラヤガム、アラビアガム等のガム類、カラギーナン、カルボキシメチルセルロースナトリウム、メチルセルロース、ヒドロキシエチルセルロース、カルボキシメチルヒドロキシエチルセルロースナトリウム等のセルロース誘導体、ポリビニルアルコール、カルボキシビニルポリマー、ポリビニルピロリドン等の有機粘結剤、シリカゲル、アルミニウムシリカゲル、ビーガム、ラポナイト等の無機粘結剤を配合できる(配合量は通常、0.3〜10%)。 In particular, paste-like dentifrice compositions such as toothpastes include sodium alginate as a binder, alginic acid derivatives such as propylene glycol alginate, xanthan gum, tragacanth gum, gela gum, gum karaya, gums such as gum arabic, carrageenan, carboxymethyl cellulose. Cellulose derivatives such as sodium, methylcellulose, hydroxyethylcellulose, sodium carboxymethylhydroxyethylcellulose, organic binders such as polyvinyl alcohol, carboxyvinyl polymer, and polyvinylpyrrolidone, and inorganic binders such as silica gel, aluminum silica gel, veegum, and laponite can be blended. (The compounding amount is usually 0.3 to 10%).
更に、特にペースト状や液状の歯磨剤組成物には、粘稠剤として、ソルビトール、マルチトール、ラクチトール、エリスリトール等の糖アルコール、プロピレングリコール等の多価アルコールを配合でき、これらのうちの1種又は2種以上を配合し得る(配合量は通常、5〜70%)。 Furthermore, especially in paste or liquid dentifrice compositions, sugar alcohols such as sorbitol, maltitol, lactitol, erythritol and polyhydric alcohols such as propylene glycol can be blended as a thickener. Alternatively, two or more kinds can be blended (the blending amount is usually 5 to 70%).
ノニオン性界面活性剤としては、ショ糖脂肪酸エステル等の糖脂肪酸エステル;マルチトール脂肪酸エステル等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ステアレート等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;ラウリン酸モノ又はジエタノールアミド等の脂肪酸ジエタノールアミド;ポリオキシエチレン高級アルコールエーテルを配合できる。中でも、ポリオキシエチレン脂肪酸エステル、特に酸化エチレンの付加モル数(E.O.、以下同様)が20〜100、とりわけ20〜80のポリオキシエチレン硬化ヒマシ油が、バイオフィルム除去効果の点で、より好適である。
カチオン性界面活性剤としては、塩化ジステアリルメチルアンモニウム等のアルキルアンモニウム塩、塩化ステアリルジメチルベンジルアンモニウム等のアルキルベンジルアンモニウム塩等が挙げられる。
ノニオン性界面活性剤及びカチオン性界面活性剤の配合量は、合計で0.01〜10%が好ましい。
なお、本発明では、界面活性剤として(b)成分と共にノニオン性界面活性剤を配合することが好ましい。(a)成分に、ノニオン性界面活性剤、特にポリオキシエチレン硬化ヒマシ油を併用するとその添加量によって臭いや味が悪くなることがあるが、(b)成分と共にノニオン性界面活性剤を添加すると、このように使用感が悪化することなくバイオフィルム除去効果がより向上する。Nonionic surfactants include sugar fatty acid esters such as sucrose fatty acid esters; sugar alcohol fatty acid esters such as maltitol fatty acid esters; polyoxyethylene sorbitan fatty acid esters such as polyoxyethylene sorbitan monostearate; polyoxyethylene cured castor Polyoxyethylene fatty acid esters such as oil; fatty acid diethanolamide such as lauric acid mono- or diethanolamide; and polyoxyethylene higher alcohol ethers can be blended. Among them, polyoxyethylene fatty acid esters, in particular, polyoxyethylene hydrogenated castor oil having an addition mole number (EO, the same applies hereinafter) of ethylene oxide of 20 to 100, particularly 20 to 80, is effective in removing biofilms. More preferred.
Examples of the cationic surfactant include an alkyl ammonium salt such as distearyl methyl ammonium chloride and an alkyl benzyl ammonium salt such as stearyl dimethyl benzyl ammonium chloride.
The total amount of the nonionic surfactant and the cationic surfactant is preferably 0.01 to 10%.
In the present invention, it is preferable to mix a nonionic surfactant with the component (b) as the surfactant. When a nonionic surfactant, particularly polyoxyethylene hydrogenated castor oil, is used in combination with the component (a), the odor and taste may be deteriorated depending on the amount of addition. However, when a nonionic surfactant is added together with the component (b), Thus, the biofilm removing effect is further improved without deteriorating the feeling of use.
甘味剤としては、サッカリンナトリウム、ステビオサイド、グリチルリチン酸ジカリウム、ペリラルチン、ソーマチン、ネオヘスペリジルジヒドロカルコン、アスパラチルフェニルアラニンメチルエステルが挙げられる。防腐剤としては、パラオキシ安息香酸エステル、安息香酸ナトリウムが挙げられる。 Sweetening agents include saccharin sodium, stevioside, dipotassium glycyrrhizinate, perillartin, thaumatin, neohesperidyl dihydrochalcone, and asparatyl phenylalanine methyl ester. Examples of preservatives include p-hydroxybenzoate and sodium benzoate.
有効成分としては、デキストラナーゼ、ムタナーゼ、リゾチーム、アミラーゼ、プロテアーゼ、溶菌酵素、SOD(スーパーオキシドディスムターゼ)等の酵素;モノフルオロリン酸ナトリウム、モノフルオロリン酸カリウム等のアルカリ金属モノフルオロフォスフェート;フッ化ナトリウム、フッ化第一錫等のフッ化物;トラネキサム酸、イプシロンアミノカプロン酸、アルミニウムクロルヒドロキシルアラントイン、ジヒドロコレスタノール、グリチルリチン酸、グリチルレチン酸、グリセロフォスフェート、クロロフィル、塩化ナトリウム、キシリトール、塩化亜鉛、水溶性無機リン酸化物や、ビタミンA、ビタミンB群、ビタミンC、ビタミンE等のビタミン類が挙げられる。これら有効成分は、1種又は2種以上で使用でき、また、本発明の効果を妨げない範囲で有効量配合することができる。 Active ingredients include enzymes such as dextranase, mutanase, lysozyme, amylase, protease, lytic enzyme, and SOD (superoxide dismutase); alkali metal monofluorophosphates such as sodium monofluorophosphate and potassium monofluorophosphate; Fluorides such as sodium fluoride and stannous fluoride; tranexamic acid, epsilon aminocaproic acid, aluminum chlorohydroxyl allantoin, dihydrocholestanol, glycyrrhizic acid, glycyrrhetinic acid, glycerophosphate, chlorophyll, sodium chloride, xylitol, zinc chloride, Examples include water-soluble inorganic phosphates and vitamins such as vitamin A, vitamin B group, vitamin C and vitamin E. These active ingredients can be used alone or in combination of two or more, and can be blended in an effective amount within a range not to impair the effects of the present invention.
香料は、ペパーミント油、スペアミント油、アニス油、ユーカリ油、ウィンターグリーン油、カシア油、クローブ油、タイム油、セージ油、レモン油、オレンジ油、ハッカ油、カルダモン油、コリアンダー油、マンダリン油、ライム油、ラベンダー油、ローズマリー油、ローレル油、カモミル油、キャラウェイ油、マジョラム油、ベイ油、レモングラス油、オリガナム油、パインニードル油、ネロリ油、ローズ油、ジャスミン油、イリスコンクリート、アブソリュートペパーミント、アブソリュートローズ、オレンジフラワー等の天然香料、及び、これら天然香料の加工処理(前溜部カット、後溜部カット、分留、液液抽出、エッセンス化、粉末香料化等)した香料、及び、メントール、カルボン、アネトール、サリチル酸メチル、シンナミックアルデヒド、3−l−メントキシプロパン−1,2−ジオール、リナロール、リナリールアセテート、リモネン、メントン、メンチルアセテート、N−置換−パラメンタン−3−カルボキサミド、ピネン、オクチルアルデヒド、シトラール、プレゴン、カルビールアセテート、アニスアルデヒド、エチルアセテート、エチルブチレート、アリルシクロヘキサンプロピオネート、メチルアンスラニレート、エチルメチルフェニルグリシデート、バニリン、ウンデカラクトン、ヘキサナール、イソアミルアルコール、ヘキセノール、ジメチルサルファイド、シクロテン、フルフラール、トリメチルピラジン、エチルラクテート、エチルチオアセテート等の単品香料、更に、ストロベリーフレーバー、アップルフレーバー、バナナフレーバー、パイナップルフレーバー、グレープフレーバー、マンゴーフレーバー、バターフレーバー、ミルクフレーバー、フルーツミックスフレーバー、トロピカルフルーツフレーバー等の調合香料が挙げられ、口腔用組成物に用いられる公知の香料素材を使用でき、実施例の香料に限定されない。
また、上記の香料素材は、組成物全体の0.000001〜1%使用するのが好ましい。上記香料素材を使用した賦香用香料としては、製剤組成中に0.001〜2.0%使用するのが好ましい。Flavors include peppermint oil, spearmint oil, anise oil, eucalyptus oil, wintergreen oil, cassia oil, clove oil, thyme oil, sage oil, lemon oil, orange oil, peppermint oil, cardamom oil, coriander oil, mandarin oil, lime Oil, lavender oil, rosemary oil, laurel oil, camomill oil, caraway oil, marjoram oil, bay oil, lemongrass oil, origanum oil, pine needle oil, neroli oil, rose oil, jasmine oil, iris concrete, absolute peppermint , Fragrances such as Absolute Rose, Orange Flower, etc., and fragrances that have been processed (cut into front reservoir, cut into rear reservoir, fractionation, liquid-liquid extraction, essence, powdered fragrance, etc.) Menthol, carvone, anethole, methyl salicylate, cinnami Qualdehyde, 3-l-menthoxypropane-1,2-diol, linalool, linalool acetate, limonene, menthone, menthyl acetate, N-substituted-paramentan-3-carboxamide, pinene, octylaldehyde, citral, pulegone, cal Beer acetate, anisaldehyde, ethyl acetate, ethyl butyrate, allyl cyclohexane propionate, methyl anthranilate, ethyl methyl phenyl glycidate, vanillin, undecalactone, hexanal, isoamyl alcohol, hexenol, dimethyl sulfide, cycloten, furfural, Single flavors such as trimethylpyrazine, ethyl lactate, and ethyl thioacetate, as well as strawberry flavor, apple flavor, banana flavor, Ingredients such as inapple flavor, grape flavor, mango flavor, butter flavor, milk flavor, fruit mix flavor, tropical fruit flavor, and the like can be used, and known flavor materials used in oral compositions can be used. It is not limited to.
In addition, the above-mentioned perfume material is preferably used in 0.000001 to 1% of the whole composition. It is preferable to use 0.001 to 2.0% as a fragrance for flavoring using the above fragrance material in a pharmaceutical composition.
口腔用組成物のpH(25℃)は、好ましくは5〜9、より好ましくは6〜8である。pHが低すぎると、口腔刺激性や、エナメル質及び象牙質の脱灰のおそれがある。pHが高すぎると、口腔刺激性や、製剤安定性の低下が発生する場合がある。 The pH (25 ° C.) of the oral composition is preferably 5 to 9, more preferably 6 to 8. If the pH is too low, there is a risk of oral irritation and demineralization of enamel and dentin. If the pH is too high, oral irritation and a decrease in formulation stability may occur.
なお、pH調整剤を添加してもよい。pH調整剤としては、無機酸、有機酸やこれらの塩を用いることできる。例えば、酢酸、塩酸、硫酸、硝酸、クエン酸、リン酸、リンゴ酸、グルコン酸、マレイン酸、コハク酸、グルタミン酸、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、リン酸二水素ナトリウムが挙げられる。 In addition, you may add a pH adjuster. As the pH adjuster, an inorganic acid, an organic acid or a salt thereof can be used. For example, acetic acid, hydrochloric acid, sulfuric acid, nitric acid, citric acid, phosphoric acid, malic acid, gluconic acid, maleic acid, succinic acid, glutamic acid, sodium hydroxide, potassium hydroxide, sodium acetate, sodium carbonate, sodium citrate, citric acid Sodium hydrogen, sodium phosphate and sodium dihydrogen phosphate.
本発明の口腔用組成物は、アルミニウムチューブ、アルミニウム箔の両面をプラスチック等でラミネートしたラミネートチューブ、プラスチックチューブ、あるいは、ボトル状容器、エアゾール容器等の所定の容器に入れて使用することができる。 The oral composition of the present invention can be used in an aluminum tube, a laminated tube in which both surfaces of an aluminum foil are laminated with plastic or the like, a plastic tube, or a predetermined container such as a bottle-shaped container or an aerosol container.
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、本発明は下記の実施例に制限されるものではない。なお、下記の例において%は特に断らない限りいずれも質量%を示す。
なお、重量平均分子量は、ゲル浸透クロマトグラフ/多角度レーザー光散乱検出器(GPC−MALLS)を用いて測定された値であり、条件は以下の通りである。
移動相:0.3M NaClO4
NaN3水溶液カラム:TSKgelα−M 2本
プレカラム:TSKguardcolumn α
標準物質:ポリエチレングリコール
また、組成物のpHは、25℃における値である。Hereinafter, the present invention will be described specifically with reference to Examples and Comparative Examples, but the present invention is not limited to the following Examples. In the following examples,% indicates mass% unless otherwise specified.
The weight average molecular weight is a value measured using a gel permeation chromatograph / multi-angle laser light scattering detector (GPC-MALLS), and the conditions are as follows.
Mobile phase: 0.3 M NaClO 4
NaN 3 aqueous solution column: TSKgelα-M 2 precolumn: TSKguardcolumn α
Standard substance: polyethylene glycol The pH of the composition is a value at 25 ° C.
[実施例、比較例]
表1〜3に示す組成の歯磨剤組成物(練歯磨)を以下の方法で調製して容器(アルミニウムラミネートチューブ)に充填し、下記方法で評価した。結果を表に併記した。[Examples and Comparative Examples]
A dentifrice composition (toothpaste) having the composition shown in Tables 1 to 3 was prepared by the following method, filled in a container (aluminum laminated tube), and evaluated by the following method. The results are shown in the table.
<調製方法>
(1)精製水中に(a)成分、その他の水溶性成分及び粘度調整剤を常温で混合溶解させた(混合物X)。
(2)プロピレングリコール中に粘結剤を常温で分散させ(混合物Y)、撹拌中の混合物X中に、混合物Yを添加混合して、混合物Zを調製した。
(3)混合物Z中に、香料、(b)成分及び研磨剤を、ニーダーを用いて常温で混合し、減圧(5.3kPa)による脱泡を行い、歯磨剤組成物を得た。
なお、比較例の歯磨剤組成物は、上記方法に準じて調製した。<Preparation method>
(1) The component (a), other water-soluble components, and a viscosity modifier were mixed and dissolved at room temperature in purified water (mixture X).
(2) The binder was dispersed in propylene glycol at room temperature (mixture Y), and the mixture Y was added and mixed with the mixture X being stirred to prepare a mixture Z.
(3) In the mixture Z, the fragrance, the component (b), and the abrasive were mixed at room temperature using a kneader, and defoaming was performed under reduced pressure (5.3 kPa) to obtain a dentifrice composition.
In addition, the dentifrice composition of the comparative example was prepared according to the said method.
<バイオフィルム除去効果の評価方法>
(1)モデルバイオフィルムの作製方法
モデルバイオフィルムを作製するために用いた細菌は、アメリカンタイプカルチャーコレクション(ATCC)より購入し、以下の方法によりプレカルチャーを行った。
アクチノマイセス ヴィスコサス(Actinomyces viscosus)ATCC43146、フゾバクテリウム ヌクレアタム(Fusobacterium nucleatum)ATCC10953、ポルフィロモナス ジンジバリス(Porphyromonas gingivalis)ATCC33277は、5mg/L ヘミン(Sigma社製)及び1mg/L ビタミンK(和光純薬工業社製)を含むトッドへヴィットブロス(Becton and Dickinson社製)培養液〔THBHM〕により培養し、ベイヨネラ パルビュラ(Veillonella parvula)ATCC17745は、1.26%乳酸ナトリウム(Sigma社製)を含むトッドへヴィットブロス(Becton and Dickinson社製)培養液〔THBL〕により培養した。なお、培養は、37℃で一晩嫌気培養(80vol%窒素、10vol%二酸化炭素、10vol%水素)した。
培養後、菌液は遠心分離(10,000rpm、10分)により集菌した。遠心集菌した各細菌は、ベイサルメディウムムチン培養液〔BMM〕*1に再懸濁した後、予め同培地1,000mLを入れた培養槽に、菌数がそれぞれ1×107個/mLになるように接種し、37℃において嫌気条件下(95vol%窒素、5vol%二酸化炭素)で一晩培養した。その後、BMMを100mL/時間の速度で供給するとともに、同速度で培養液を排出した。上記培養槽から排出された培養液は、液量が300mLに保たれる別の培養槽に連続的に供給した。この培養槽内の回転盤(約80rpmで回転)には、バイオフィルムの付着担体として直径7mmのハイドロキシアパタイト板(ペンタックス社製)を装着した。
上記方法による培養は、10日間連続して行い、ハイドロキシアパタイト板上にバイオフィルムを形成させた。培養後、取り出したバイオフィルム形成ハイドロキシアパタイト板をリン酸緩衝生理食塩水*2(Phosphate Buffered Saline、以下PBSとする)5mLで2回洗浄し、モデルバイオフィルムを得た。<Evaluation method of biofilm removal effect>
(1) Method for Producing Model Biofilm Bacteria used for producing a model biofilm were purchased from American Type Culture Collection (ATCC) and precultured by the following method.
Actinomyces viscosus ATCC43146, Fusobacterium nucleatum ATCC10953, Porphyromonas gingivalis (Porphymonas gingivalis) and 5mg / L MGK / L MGK / L MGK / GLK MGL MGMG27 / Cultivated in a culture medium [THBHM] (Becton and Dickinson) containing Todd hevit broth (manufactured by Becton and Dickinson), and Veylonella parvula ATCC 17745 contains 1.26% sodium lactate (Sigma). (Becton and Dickins They were cultured by n Co., Ltd.) culture [THBL]. The culture was performed at 37 ° C. overnight under anaerobic culture (80 vol% nitrogen, 10 vol% carbon dioxide, 10 vol% hydrogen).
After the culture, the bacterial solution was collected by centrifugation (10,000 rpm, 10 minutes). Each of the bacteria collected by centrifugation was resuspended in a basal medium mucin culture solution [BMM] * 1, and then the number of bacteria was reduced to 1 × 10 7 cells / mL in a culture tank containing 1,000 mL of the same medium in advance. The cells were inoculated so as to be cultured at 37 ° C. under anaerobic conditions (95 vol% nitrogen, 5 vol% carbon dioxide) overnight. Thereafter, BMM was supplied at a rate of 100 mL / hour, and the culture solution was discharged at the same rate. The culture solution discharged from the culture tank was continuously supplied to another culture tank in which the liquid volume was maintained at 300 mL. A 7 mm-diameter hydroxyapatite plate (manufactured by PENTAX) was attached as a carrier for attaching a biofilm to a rotating disk (rotated at about 80 rpm) in the culture tank.
Culture by the above method was performed continuously for 10 days, and a biofilm was formed on a hydroxyapatite plate. After the culturing, the biofilm-formed hydroxyapatite plate taken out was washed twice with 5 mL of phosphate buffered saline * 2 (Phosphate Buffered Saline, hereinafter referred to as PBS) to obtain a model biofilm.
*1;BMMの組成(1リットル中の質量で表す。)
プロテオースペプトン(Becton and Dickinson社
製): 4g/L
トリプトン(Becton and Dickinson社製):
2g/L
イーストエキス(Becton and Dickinson社製):
2g/L
ムチン(Sigma社製): 5g/L
ヘミン(Sigma社製): 2.5mg/L
ビタミンK(和光純薬工業社製): 0.5mg/L
KCl(和光純薬工業社製): 1g/L
システイン(和光純薬工業社製): 0.2g/L
蒸留水: 残
(全量が1Lになるようにメスアップし、121℃で20分間オートク
レーブした。)* 1: BMM composition (expressed in mass per liter)
Proteose peptone (Becton and Dickinson): 4 g / L
Tryptone (Becton and Dickinson):
2g / L
Yeast extract (Becton and Dickinson):
2g / L
Mucin (manufactured by Sigma): 5 g / L
Hemin (Sigma): 2.5 mg / L
Vitamin K (manufactured by Wako Pure Chemical Industries): 0.5 mg / L
KCl (manufactured by Wako Pure Chemical Industries, Ltd.): 1 g / L
Cysteine (manufactured by Wako Pure Chemical Industries, Ltd.): 0.2 g / L
Distilled water: residual
*2;PBSの組成(1リットル中の質量で表す。)
NaCl(和光純薬工業社製): 8.0g
KCl(和光純薬工業社製): 0.2g
Na2HPO4・12H2O(和光純薬工業社製): 3.63g
KH2PO4(和光純薬工業社製): 0.24g
蒸留水: 残
(1N HClによりpH7.4に調整し、全量が1Lになるようにメ
スアップした。)* 2: Composition of PBS (expressed in mass per liter)
NaCl (manufactured by Wako Pure Chemical Industries, Ltd.): 8.0 g
KCl (manufactured by Wako Pure Chemical Industries, Ltd.): 0.2 g
Na 2 HPO 4 .12H 2 O (manufactured by Wako Pure Chemical Industries, Ltd.): 3.63 g
KH 2 PO 4 (manufactured by Wako Pure Chemical Industries, Ltd.): 0.24 g
Distilled water: residue (adjusted to pH 7.4 with 1N HCl and made up to 1 L in total volume)
(2)モデルバイオフィルムの除去効果の評価方法
(1)で作製したモデルバイオフィルム形成ハイドロキシアパタイト板は、24穴マルチプレート(住友ベークライト社製)に移した。これに、試験組成物として上記方法で調製した歯磨剤組成物を、人工唾液(50mM KCl、1mM CaCl2、0.1mM MgCl2、1mM KH2PO4、pH7.0)で3倍希釈した歯磨剤溶液の遠心上清(10,000rpm、10分)を2mL加え、3分間浸漬した。その後、PBS(和光純薬工業社製)1mLで6回洗浄し、上記と同バッファー2mLを添加した試験管(直径13mm×100mm)内で超音波処理(200μA、10秒間)により、残ったバイオフィルムを強制的に分散させた。この分散液の波長550nmでの濁度(OD)を測定し、バイオフィルムの残存量を測定した。
試験組成物のバイオフィルム除去効果は、下式によりコントロールに対する除去率を求め、この除去率から、下記基準に則り口腔バイオフィルム除去効果を判定した。
なお、上記歯磨剤溶液の代わりにPBS2mlを用いて同様に処置したものをコントロールとした。
バイオフィルム除去率(%)=
{(コントロールの濁度−試験組成物処置品の濁度)/コントロールの濁
度}×100
バイオフィルム除去効果の判定基準
◎:バイオフィルム除去率が90%以上
○:バイオフィルム除去率が70%以上90%未満
△:バイオフィルム除去率が50%以上70%未満
×:バイオフィルム除去率が50%未満(2) Evaluation method of removal effect of model biofilm The model biofilm-formed hydroxyapatite plate prepared in (1) was transferred to a 24-well multiplate (manufactured by Sumitomo Bakelite). To this, the dentifrice composition prepared by the above method as a test composition was diluted 3-fold with artificial saliva (50 mM KCl, 1 mM CaCl 2 , 0.1 mM MgCl 2 , 1 mM KH 2 PO 4 , pH 7.0). 2 mL of the centrifugal supernatant (10,000 rpm, 10 minutes) of the agent solution was added and immersed for 3 minutes. Thereafter, the residue was washed six times with 1 mL of PBS (manufactured by Wako Pure Chemical Industries, Ltd.) and subjected to ultrasonic treatment (200 μA, 10 seconds) in a test tube (diameter 13 mm × 100 mm) to which 2 mL of the same buffer was added as described above. The film was forced to disperse. The turbidity (OD) of this dispersion at a wavelength of 550 nm was measured, and the remaining amount of the biofilm was measured.
The biofilm removal effect of the test composition was determined by calculating the removal rate relative to the control by the following formula, and from this removal rate, the oral biofilm removal effect was determined according to the following criteria.
A control similarly treated with 2 ml of PBS instead of the dentifrice solution was used as a control.
Biofilm removal rate (%) =
{(Turbidity of control−turbidity of test composition treated product) / turbidity of control} × 100
Criteria for biofilm removal effect :: Biofilm removal rate is 90% or more 以上: Biofilm removal rate is 70% or more and less than 90% △: Biofilm removal rate is 50% or more and less than 70% ×: Biofilm removal rate Less than 50%
<使用感の評価方法>
10名の被験者が、歯磨剤組成物1gを歯ブラシにのせ、3分間ブラッシングして口腔内を洗浄した際の使用感として口腔刺激性、臭い(口腔刺激のなさ、臭いのなさ)を下記の評価基準により評価した。10人の評価点の平均を算出し、下記の判定基準により判定した。<How to evaluate usability>
Ten test subjects evaluated the following stimuli of oral irritation and odor (no oral irritation, no odor) as a feeling of use when 1 g of the dentifrice composition was placed on a toothbrush and brushed for 3 minutes to wash the inside of the mouth. The evaluation was based on criteria. The average of the evaluation points of 10 persons was calculated and judged according to the following criteria.
口腔刺激性の評価基準
4点:口腔内で刺激を感じない
3点:口腔内でやや刺激を感じるが問題ないレベル
2点:口腔内で刺激を感じる
1点:口腔内で非常に刺激を感じる
口腔刺激性の判定基準
◎:平均点3.0点以上
○:平均点2.5点以上3.0点未満
△:平均点1.5点以上2.5点未満
×:平均点1.5点未満
臭いの評価基準
4点:口腔内で不快な臭いを感じない
3点:口腔内で不快な臭いをやや感じるが問題ないレベル
2点:口腔内で不快な臭いを感じる
1点:口腔内で不快な臭いを強く感じる
臭いの判定基準
◎:平均点3.5点以上
○:平均点3.0点以上3.5点未満
△:平均点2.0点以上3.0点未満
×:平均点2.0点未満Evaluation criteria for oral irritation 4 points: no irritation in the oral cavity 3 points: level slightly in the oral cavity but no problem 2 points: irritation in the oral cavity 1 point: very irritation in the oral cavity Oral irritation criterion ◎: Average score of 3.0 or more :: Average score of 2.5 or more and less than 3.0 Δ: Average score of 1.5 or more and less than 2.5 ×: Average score of 1.5 Less than the score Odor evaluation criteria 4 points: No unpleasant odor is felt in the oral cavity 3 points: A level of unpleasant odor is slightly felt in the oral cavity, but there is no problem 2 points: An unpleasant odor is felt in the oral cavity 1 point: In the oral cavity A strong smell is felt in the odor. Criteria for odor ◎: Average score of 3.5 or more ○: Average score of 3.0 or more and less than 3.5 △: Average score of 2.0 or more and less than 3.0 ×: Average point less than 2.0
なお、使用したポリアクリル酸ナトリウム、ポリアクリル酸の詳細を下記に示す。
(a)ポリアクリル酸ナトリウム(Mw1,000):ポリサイエンス
社製
(a)ポリアクリル酸ナトリウム(Mw6,000):東亞合成社製、
AC−10NP
(a)ポリアクリル酸ナトリウム(Mw8,000):ポリサイエンス
社製
(a)ポリアクリル酸ナトリウム(Mw20,000):東亞合成社製
、アロンA−20UN
ポリアクリル酸ナトリウム(Mw300,000、比較品):ポリサイ
エンス社製
ポリアクリル酸(Mw6,000、比較品):東亞合成社製、アロンA
−10SLThe details of the sodium polyacrylate and polyacrylic acid used are shown below.
(A) Sodium polyacrylate (Mw 1,000): manufactured by Polyscience Co., Ltd. (a) Sodium polyacrylate (Mw 6,000): manufactured by Toagosei Co., Ltd.
AC-10NP
(A) Sodium polyacrylate (Mw 8,000): manufactured by Polyscience (a) Sodium polyacrylate (Mw 20,000): manufactured by Toagosei Co., Ltd., Alon A-20UN
Sodium polyacrylate (Mw 300,000, comparative product): Polyacrylic acid (Mw 6,000, comparative product): Alon A, manufactured by Toagosei Co., Ltd.
-10SL
Claims (9)
(b)アニオン性界面活性剤及び両性界面活性剤から選ばれる1種以上と
からなる口腔バイオフィルム除去剤。(A) a polyacrylate having a weight average molecular weight of 1,000 to 20,000,
(B) An oral biofilm remover comprising at least one selected from anionic surfactants and amphoteric surfactants.
(b)アニオン性界面活性剤及び両性界面活性剤から選ばれる1種以上と
を含有する口腔用組成物。(A) a polyacrylate having a weight average molecular weight of 1,000 to 20,000,
(B) an oral composition comprising at least one selected from an anionic surfactant and an amphoteric surfactant;
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WO2019107332A1 (en) * | 2017-11-30 | 2019-06-06 | ライオン株式会社 | Oral stain removing agent, oral stain formation inhibiting agent, and oral composition |
JP2020100596A (en) * | 2018-12-25 | 2020-07-02 | ライオン株式会社 | Oral biofilm remover and oral composition |
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JP7120087B2 (en) * | 2019-03-08 | 2022-08-17 | ライオン株式会社 | oral composition |
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