JP2013112650A - Liquid composition for oral cavity - Google Patents
Liquid composition for oral cavity Download PDFInfo
- Publication number
- JP2013112650A JP2013112650A JP2011260985A JP2011260985A JP2013112650A JP 2013112650 A JP2013112650 A JP 2013112650A JP 2011260985 A JP2011260985 A JP 2011260985A JP 2011260985 A JP2011260985 A JP 2011260985A JP 2013112650 A JP2013112650 A JP 2013112650A
- Authority
- JP
- Japan
- Prior art keywords
- salt
- mass
- oral cavity
- composition
- liquid oral
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 239000000203 mixture Substances 0.000 title claims abstract description 64
- 239000007788 liquid Substances 0.000 title claims abstract description 54
- 210000000214 mouth Anatomy 0.000 title claims abstract description 34
- -1 acyl sarcosine Chemical compound 0.000 claims abstract description 62
- 150000003839 salts Chemical class 0.000 claims abstract description 51
- FSYKKLYZXJSNPZ-UHFFFAOYSA-N N-methylaminoacetic acid Natural products C[NH2+]CC([O-])=O FSYKKLYZXJSNPZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 108010077895 Sarcosine Proteins 0.000 claims abstract description 20
- 229940043230 sarcosine Drugs 0.000 claims abstract description 20
- 229920000137 polyphosphoric acid Polymers 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000003945 anionic surfactant Substances 0.000 claims abstract description 11
- 239000003205 fragrance Substances 0.000 claims description 11
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 8
- 235000011187 glycerol Nutrition 0.000 claims description 4
- 239000002736 nonionic surfactant Substances 0.000 claims description 4
- HDTRYLNUVZCQOY-UHFFFAOYSA-N α-D-glucopyranosyl-α-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OC1C(O)C(O)C(O)C(CO)O1 HDTRYLNUVZCQOY-UHFFFAOYSA-N 0.000 claims description 3
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- 230000000694 effects Effects 0.000 abstract description 24
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- 125000004432 carbon atom Chemical group C* 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000000551 dentifrice Substances 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
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- 235000006679 Mentha X verticillata Nutrition 0.000 description 2
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- BACYUWVYYTXETD-UHFFFAOYSA-N N-Lauroylsarcosine Chemical compound CCCCCCCCCCCC(=O)N(C)CC(O)=O BACYUWVYYTXETD-UHFFFAOYSA-N 0.000 description 2
- 125000002252 acyl group Chemical group 0.000 description 2
- 125000004442 acylamino group Chemical group 0.000 description 2
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- RRAFCDWBNXTKKO-UHFFFAOYSA-N eugenol Chemical compound COC1=CC(CC=C)=CC=C1O RRAFCDWBNXTKKO-UHFFFAOYSA-N 0.000 description 2
- 235000003599 food sweetener Nutrition 0.000 description 2
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- 229930007503 menthone Natural products 0.000 description 1
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- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
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Landscapes
- Cosmetics (AREA)
Abstract
Description
本発明は、液体口腔用組成物に関する。 The present invention relates to a liquid oral composition.
ヒトの歯の着色は、加齢や外傷等によって着色する内因性着色のほか、歯石や歯垢、又はお茶や油、タバコ等の習慣的飲食等により、歯面に茶渋やタバコのヤニ等の着色汚れが付着する外因性着色がある。こうした外因性着色を防止することを目的として、特許文献1には、ポリリン酸又はその塩とアシルタウリン塩を含有する液体口腔用組成物が開示され、特許文献2には、ポリリン酸又はその塩と、二糖類、りんご酸等を含有する液体口腔用組成物が開示されており、これらを適用することによって歯面に着色汚れが付着するのを未然に防いでいる。 In addition to intrinsic coloring that colors due to aging, trauma, etc., human teeth are colored by tartar, plaque, or customary food and drink such as tea, oil, tobacco, etc. There is extrinsic coloring to which coloring dirt adheres. For the purpose of preventing such exogenous coloring, Patent Document 1 discloses a liquid oral composition containing polyphosphoric acid or a salt thereof and an acyl taurine salt, and Patent Document 2 discloses polyphosphoric acid or a salt thereof. In addition, liquid oral compositions containing disaccharides, malic acid and the like are disclosed, and by applying these, coloring stains are prevented from adhering to the tooth surface.
一方、外因性着色を防止するにあたり、着色汚れの付着を防止するだけでなく、すでに付着した着色汚れを除去するのがさらに効果的であることから、その際に用いるものとして、特許文献3には、顆粒ゼオライトとポリリン酸、両性界面活性剤、及びアニオン界面活性剤を含有する歯磨剤組成物が開示されている。 On the other hand, in preventing exogenous coloring, it is more effective not only to prevent the adhesion of colored stains but also to remove the colored stains already attached. Discloses a dentifrice composition containing granular zeolite and polyphosphoric acid, an amphoteric surfactant, and an anionic surfactant.
しかしながら、特許文献3に記載の歯磨剤組成物であると、ブラッシング作用との相加効果により着色汚れを除去するため、ブラシが届かない部分の除去効果が不十分となるおそれがある。また、仮に該文献に開示された歯磨剤組成物の処方を元に、水分の割合を単に増加させてブラッシングが不要である液体口腔用組成物を製造した場合であっても、低温において析出物が形成されたり、析出物により白濁するおそれがある。これに対して、特許文献1〜2に記載の液体口腔用組成物であれば、良好な安定性を有しつつ、歯に着色汚れが付着するのを未然に防ぐ効果を発揮するものの、すでに付着した着色汚れの除去効果については、依然として改善の余地がある。 However, in the case of the dentifrice composition described in Patent Document 3, since colored stains are removed by an additive effect with the brushing action, there is a possibility that the effect of removing the portion where the brush does not reach may be insufficient. Moreover, even when a liquid oral composition that does not require brushing is produced by simply increasing the proportion of moisture based on the prescription of the dentifrice composition disclosed in the document, precipitates are produced at low temperatures. May form or may become cloudy due to precipitates. On the other hand, if it is a composition for liquid oral cavity described in Patent Documents 1 and 2, while exhibiting the effect of preventing coloring stains from adhering to the teeth while having good stability, it has already been achieved. There is still room for improvement with respect to the effect of removing the attached colored stains.
したがって、本発明の課題は、すでに付着した着色汚れを除去する効果(外因性着色除去効果)に優れるとともに、高い安定性をも有する液体口腔用組成物を提供することにある。 Therefore, the subject of this invention is providing the composition for liquid oral cavity which is excellent in the effect (exogenous coloring removal effect) which removes the already adhering colored stain | pollution | contamination, and also has high stability.
そこで本発明者は、ポリリン酸又はその塩、及びサルコシン又はその塩を特定の質量比で含有し、硫酸エステル又はその塩の含有量を調整することによって、歯の外因性着色の要因となる茶渋やタバコのヤニ等の種々の着色汚れを除去する効果を充分に発揮し、しかも安定性に優れる液体口腔用組成物が得られることを見出した。 Therefore, the present inventor contains polyphosphoric acid or a salt thereof, and sarcosine or a salt thereof in a specific mass ratio, and adjusts the content of sulfate ester or a salt thereof, thereby causing tea astringency that causes extrinsic coloring of teeth. It has been found that a liquid composition for oral cavity can be obtained which exhibits a sufficient effect of removing various colored stains such as varnish of tobacco and tobacco, and which is excellent in stability.
すなわち、本発明は、次の成分(A)、(B)及び(C):
(A)アシルサルコシン又はその塩 0.02〜0.5質量%、
(B)ポリリン酸又はその塩 0.5〜5質量%、及び
(C)水 75〜95質量%
を含有し、かつ(D)アニオン界面活性剤としての硫酸エステル又はその塩を含有しないか、或いは含有量が0.001質量%以下であり、
成分(B)と成分(A)の含有量の質量比(B/A)が2〜50である液体口腔用組成物を提供するものである。
That is, the present invention includes the following components (A), (B) and (C):
(A) acyl sarcosine or a salt thereof 0.02 to 0.5% by mass,
(B) polyphosphoric acid or its salt 0.5-5 mass%, and (C) water 75-95 mass%
And (D) does not contain a sulfate ester or a salt thereof as an anionic surfactant, or the content is 0.001% by mass or less,
The composition for liquid oral cavity whose mass ratio (B / A) of content of a component (B) and a component (A) is 2-50 is provided.
本発明の液体口腔用組成物によれば、歯に付着した茶渋等の着色汚れだけでなく、タバコのヤニ等の着色汚れ等、種々の着色汚れを充分に除去することができ、しかも低温における高い安定性を兼ね備えている。なかでも、茶渋等の色素成分と飲食物やタバコのヤニ等の油性成分とが混在して歯に付着したような着色汚れに対し、顕著な除去効果(外因性着色除去効果)を発揮することができる。したがって、本発明の液体口腔用組成物は、種々の着色汚れを充分に除去しながら優れた外観を呈し、良好な使用感をもたらすことができるものである。 According to the composition for liquid oral cavity of the present invention, it is possible to sufficiently remove not only colored stains such as tea astringents attached to teeth but also various colored stains such as tobacco stains, and at low temperatures. Combines high stability. In particular, it exhibits a remarkable removal effect (exogenous color removal effect) against colored stains that adhere to teeth due to a mixture of pigment components such as tea astringents and oily components such as food and tobacco or tobacco. Can do. Therefore, the composition for liquid oral cavity of the present invention exhibits an excellent appearance while sufficiently removing various colored stains, and can provide a good feeling of use.
以下、本発明について詳細に説明する。
本発明の液体口腔用組成物は、アシルサルコシン又はその塩(A)を0.02〜0.5質量%含有する。アシルサルコシン又はその塩(A)はアニオン界面活性剤の一種であり、この特定量のアシルサルコシン又はその塩(A)と、特定の質量比を有する特定量のポリリン酸又はその塩(B)とが相まって、歯における茶渋等の着色汚れ、なかでも茶渋等と飲食物やタバコのヤニ等のように、ポリフェノールとタール等の油汚れの複数の成分が混在して歯に付着した着色汚れに対しても、充分な除去効果を発揮することができる。
Hereinafter, the present invention will be described in detail.
The composition for liquid oral cavity of the present invention contains 0.02 to 0.5% by mass of acyl sarcosine or a salt thereof (A). Acyl sarcosine or a salt thereof (A) is a kind of anionic surfactant, and this specific amount of acyl sarcosine or a salt thereof (A) and a specific amount of polyphosphoric acid or a salt thereof (B) having a specific mass ratio Combined with colored stains such as tea astringents on teeth, especially those that are mixed with multiple components of oil stains such as polyphenols and tar, such as tea astringents and food and tobacco dust. However, a sufficient removal effect can be exhibited.
アシルサルコシン又はその塩(A)としては、飽和脂肪酸を由来とするアシル基を有するアシルサルコシン又はその塩が好ましく、飽和脂肪酸としては、炭素数12〜18の飽和脂肪酸が好ましく、茶渋等と飲食物やタバコのヤニ等とのように複数の成分が混在して歯に付着したような着色汚れの除去効果にも優れる点から、炭素数12〜14の飽和脂肪酸がより好ましい。アシルサルコシン又はその塩(A)としては、N-アシルサルコシン又はその塩が好ましく、より具体的には、例えば、N-ラウロイルサルコシン、N−ミリストイルサルコシン、N−パルミトイルサルコシン、N−ステアロイルサルコシン、N−イソステアロイルサルコシン、N−オレオイルサルコシン、及びこれらの塩から選ばれる1種類又は2種以上のN-アシルサルコシン又はその塩(A)が好ましく、N-ラウロイルサルコシン塩、N-ミリストイルサルコシン塩から選ばれる1種又は2種以上がより好ましい。また、N-アシルサルコシン塩の塩としては、ナトリウム塩、カリウム塩が好ましく、ナトリウム塩がより好ましい。 As the acyl sarcosine or a salt thereof (A), an acyl sarcosine having an acyl group derived from a saturated fatty acid or a salt thereof is preferable. As the saturated fatty acid, a saturated fatty acid having 12 to 18 carbon atoms is preferable. A saturated fatty acid having 12 to 14 carbon atoms is more preferable because it is excellent in the effect of removing colored stains such as adhering to a tooth in a mixture of a plurality of components such as cigarette or tobacco. As the acyl sarcosine or a salt thereof (A), N-acyl sarcosine or a salt thereof is preferable, and more specifically, for example, N-lauroyl sarcosine, N-myristoyl sarcosine, N-palmitoyl sarcosine, N-stearoyl sarcosine, N -One or more kinds of N-acyl sarcosine or a salt thereof (A) selected from isostearoyl sarcosine, N-oleoyl sarcosine, and salts thereof are preferable, and from N-lauroyl sarcosine salt and N-myristoyl sarcosine salt One or more selected are more preferable. Moreover, as a salt of N-acyl sarcosine salt, a sodium salt and a potassium salt are preferable, and a sodium salt is more preferable.
アシルサルコシン又はその塩(A)の含有量は、保存安定性を高め、外因性着色除去効果を向上させ、また収容容器への充填性及び爽快感を損なわない観点から、本発明の液体口腔用組成物中に0.03〜0.4質量%が好ましく、0.05〜0.3質量%がより好ましく、0.08〜0.3質量%がさらに好ましい。 The content of the acyl sarcosine or its salt (A) increases the storage stability, improves the exogenous coloring removal effect, and does not impair the filling property and refreshing feeling of the container, so that the liquid oral cavity of the present invention 0.03-0.4 mass% is preferable in a composition, 0.05-0.3 mass% is more preferable, 0.08-0.3 mass% is further more preferable.
本発明の液体口腔用組成物は、ポリリン酸又はその塩(B)を0.5〜5質量%含有する。ポリリン酸又はその塩(B)を単独で用いた場合、充分な外因性着色除去効果を発揮するに至らず、特に茶渋等と飲食物やタバコのヤニ等とのように複数の成分が混在して歯に付着したような頑固な着色汚れを除去するのは困難である。しかしながら、本発明では、特定量かつ特定の質量比を有するアシルサルコシン又はその塩(A)とポリリン酸又はその塩(B)とが相まって、優れた外因性着色除去効果を発揮することができ、頑固な着色汚れであっても充分に取り除くことが可能である。 The liquid composition for oral cavity of the present invention contains 0.5 to 5% by mass of polyphosphoric acid or a salt thereof (B). When polyphosphoric acid or a salt thereof (B) is used alone, it does not exhibit a sufficient exogenous coloring removal effect, and in particular, a plurality of components such as tea astringents, foods and drinks, tobacco crabs and the like are mixed. Therefore, it is difficult to remove stubborn colored stains attached to the teeth. However, in the present invention, acyl sarcosine having a specific amount and a specific mass ratio or a salt thereof (A) and polyphosphoric acid or a salt thereof (B) can be combined to exert an excellent exogenous color removal effect, Even stubborn colored stains can be removed sufficiently.
ポリリン酸としては、ピロリン酸、トリポリリン酸、テトラポリリン酸、メタリン酸から選ばれる1種又は2種以上が好ましく、その塩としては、ナトリウム、カリウムから選ばれる塩が好ましく、ピロリン酸ナトリウム、ピロリン酸カリウム、トリポリリン酸ナトリウム、及びトリポリリン酸カリウムから選ばれる1種又は2種以上がより好ましく、ピロリン酸ナトリウム及びトリポリリン酸ナトリウムから選ばれる1種又は2種がさらに好ましい。 The polyphosphoric acid is preferably one or more selected from pyrophosphoric acid, tripolyphosphoric acid, tetrapolyphosphoric acid, and metaphosphoric acid, and the salt thereof is preferably a salt selected from sodium and potassium, sodium pyrophosphate, pyrophosphoric acid One or more selected from potassium, sodium tripolyphosphate, and potassium tripolyphosphate are more preferable, and one or two selected from sodium pyrophosphate and sodium tripolyphosphate are more preferable.
ポリリン酸又はその塩(B)の含有量は、外因性着色除去効果及び味の点から、本発明の液体口腔用組成物中に0.6〜3質量%が好ましく、0.8〜2質量%がより好ましい。 The content of polyphosphoric acid or a salt thereof (B) is preferably 0.6 to 3% by mass, preferably 0.8 to 2% by mass, in the liquid oral composition of the present invention from the viewpoint of exogenous color removal effect and taste. % Is more preferable.
本発明の液体口腔用組成物は、ポリリン酸又はその塩(B)の含有量と、アシルサルコシン又はその塩(A)の含有量との質量比(B/A)が、味及び外因性着色汚れ除去効果を向上する点から、2〜50であって、2.5〜40であることがより好ましく、3〜30であることがさらに好ましい。このように、本発明の液体口腔用組成物は、アシルサルコシン又はその塩(A)とポリリン酸又はその塩(B)を特定量かつ特定の質量比で含有することにより、外因性着色の要因となる単一の着色汚れだけでなく、複数の着色汚れが付着した複合汚れ、即ち、現実の歯牙の表面に存在する外因性の着色汚れに類似する着色汚れに対しても、優れた外因性着色除去効果を奏する。 In the liquid oral cavity composition of the present invention, the mass ratio (B / A) between the content of polyphosphoric acid or a salt thereof (B) and the content of acyl sarcosine or a salt thereof (A) is a taste and exogenous coloring. From the point which improves a dirt removal effect, it is 2-50, it is more preferable that it is 2.5-40, and it is further more preferable that it is 3-30. As described above, the liquid oral composition of the present invention contains the acyl sarcosine or its salt (A) and the polyphosphoric acid or its salt (B) in a specific amount and a specific mass ratio, thereby causing extrinsic coloring. Excellent exogenous not only for single colored stains, but also for composite stains with multiple colored stains attached, that is, for colored stains similar to the exogenous colored stains present on the actual tooth surface There is a color removal effect.
本発明の液体口腔用組成物は、水(C)を75〜95質量%含有する。水(C)としては、精製水やイオン交換水として配合される水分のほか、ソルビトール水などに含まれる水分も含まれる。水(C)の含有量は、分散性及び使用感の点から、本発明の液体口腔用組成物中に80〜95質量%が好ましく、80〜90質量%がより好ましい。 The composition for liquid oral cavity of the present invention contains 75 to 95% by mass of water (C). The water (C) includes water contained in purified water and ion exchange water, as well as water contained in sorbitol water. The content of water (C) is preferably 80 to 95% by mass and more preferably 80 to 90% by mass in the liquid oral composition of the present invention from the viewpoint of dispersibility and usability.
本発明の液体口腔用組成物は、成分(A)以外のアニオン界面活性剤として、硫酸エステル又はその塩(D)を含有しないか、或いはこれを含有する場合、その含有量は0.001質量%以下である。アニオン界面活性剤としての硫酸エステル又はその塩(D)は、ポリリン酸又はその塩(B)と共に錯体を形成しやすいため、成分(D)の含有量によっては、保存中に析出物が生成したり白濁したりして外因性着色除去効果が損なわれるおそれがあり、こうした状況は特に低温下で顕著になる傾向にある。そのため、本発明の液体口腔用組成物は、かかる成分(D)を含有しないか、或いは含有量が0.001質量%以下であることにより、外因性着色除去効果を損なうことなく良好な保存安定性を発揮することができる。 The composition for liquid oral cavity of the present invention does not contain or contains a sulfate ester or a salt thereof (D) as an anionic surfactant other than the component (A). % Or less. Since the sulfate ester or its salt (D) as an anionic surfactant tends to form a complex with polyphosphoric acid or its salt (B), a precipitate may be formed during storage depending on the content of the component (D). There is a possibility that the exogenous coloring removal effect may be impaired due to turbidity or white turbidity, and such a situation tends to become remarkable particularly at low temperatures. Therefore, the liquid oral composition of the present invention does not contain such a component (D) or has a content of 0.001% by mass or less, so that good storage stability can be obtained without impairing the exogenous coloring removal effect. Can demonstrate its sexuality.
アニオン界面活性剤としての硫酸エステル(D)としては、アルキル硫酸エステル、ポリオキシアルキレン化アルキル硫酸エステルが挙げられ、アルキル硫酸エステル塩としては、ラウリル硫酸ナトリウム、ミリスチル硫酸ナトリウム等が挙げられる。前記硫酸エステル又はその塩(D)と、ポリリン酸又はその塩(B)とを含有する場合、より確実に析出物の形成や白濁を防止する点から、前記硫酸エステル又はその塩(D)の含有量は、本発明の液体口腔用組成物中に0.0001質量%以下であることが好ましい。 Examples of the sulfate ester (D) as the anionic surfactant include alkyl sulfate esters and polyoxyalkylenated alkyl sulfate esters. Examples of the alkyl sulfate ester salts include sodium lauryl sulfate and sodium myristyl sulfate. In the case of containing the sulfate ester or a salt thereof (D) and polyphosphoric acid or a salt thereof (B), the sulfate ester or a salt thereof (D) is more reliably prevented from forming a precipitate or clouding. It is preferable that content is 0.0001 mass% or less in the composition for liquid oral cavity of this invention.
本発明の液体口腔用組成物は、香味や爽快感の点から香料(E)を含有することが好ましい。香料(E)としては、メントール、カルボン、アネトール、オイゲノール、シネオール、チモール、サリチル酸メチル、プレゴン、メントン、ピネン、リモネン、メンチルアセテート等の合成香料の他に、ペパーミント油、スペアミント油、ハッカ油等のミント油;レモン、オレンジ、グレープフルーツ、ライムなどの柑橘油;ユーカリ、セージ、ローズマリー、タイム、ローレル、バジル、シソ、ベイ、エストラゴン、パセリ、セロリ、コリアンダー等のハーブ油;シナモン、ペッパー、ナツメグ、メース、クローブ、ジンジャー、カルダモン、アニスなどのスパイス油などのような天然精油;アップル、バナナ、メロン、グレープ、ピーチ、ストロベリー、ブルーベリー、ラズベリー、ブラックカラント、ライチ、スターフルーツ、パッションフルーツ、プラム、パイナップル、マスカットなどのフルーツフレーバーなどから選ばれる2種以上を用いることができる。これら香料の中でも、口腔内へ爽快感や清涼感を付与する点から、メントール、カルボン、ペパーミント油、スペアミント油、ハッカ油、サリチル酸メチル、シネオール、リモネン、ピネンから選ばれる1種又は2種以上の香料を含むことが好ましく、2種以上を組み合わせて含有することが好ましい。香料(E)の含有量は、安定性と味、及び香味の点から、本発明の液体口腔用組成物中に0.05〜1質量%であることが好ましく、0.1〜0.6質量%がより好ましい。 The liquid oral composition of the present invention preferably contains a fragrance (E) from the viewpoint of flavor and refreshment. As the fragrance (E), in addition to synthetic fragrances such as menthol, carvone, anethole, eugenol, cineol, thymol, methyl salicylate, plegon, menthone, pinene, limonene, menthyl acetate, peppermint oil, spearmint oil, mint oil, etc. Mint oil; citrus oils such as lemon, orange, grapefruit, lime; herbal oils such as eucalyptus, sage, rosemary, thyme, laurel, basil, perilla, bay, estragon, parsley, celery, coriander; cinnamon, pepper, nutmeg, Natural essential oils such as spice oil such as mace, clove, ginger, cardamom, anise; apple, banana, melon, grape, peach, strawberry, blueberry, raspberry, blackcurrant, lychee, star fruit, puff Yonfurutsu, can be used plum, pineapple, two or more selected from fruit flavors, such as Muscat. Among these fragrances, one or more kinds selected from menthol, carvone, peppermint oil, spearmint oil, peppermint oil, methyl salicylate, cineol, limonene, and pinene from the viewpoint of imparting a refreshing feeling and a refreshing feeling to the oral cavity. It preferably contains a fragrance, and preferably contains two or more in combination. It is preferable that content of a fragrance | flavor (E) is 0.05-1 mass% in the liquid oral cavity composition of this invention from the point of stability, a taste, and a flavor, 0.1-0.6 The mass% is more preferable.
本発明の液体口腔用組成物は、アシルサルコシン又はその塩(A)に対するポリリン酸又はその塩(B)の含有量と香料(E)の含有量との合計の質量比((B+E)/A)は、外因性着色除去効果、及び安定性の点から、3〜50であることが好ましく、4〜40であることがより好ましい。さらに、香料(E)の含有量に対するポリリン酸又はその塩(B)の含有量の質量比(B/E)は、安定性、外因性着色汚れ除去と塩味抑制の両立の点から、2〜20が好ましく、3〜16がより好ましく、3.5〜10がさらに好ましい。 The composition for liquid oral cavity of the present invention is the total mass ratio ((B + E) / A) of the content of polyphosphoric acid or its salt (B) and the content of fragrance (E) to acyl sarcosine or its salt (A). ) Is preferably from 3 to 50, more preferably from 4 to 40, from the standpoint of exogenous color removal effect and stability. Furthermore, the mass ratio (B / E) of the content of the polyphosphoric acid or its salt (B) to the content of the fragrance (E) is 2 to 2 in terms of stability, exogenous coloring stain removal and salty taste suppression. 20 is preferable, 3 to 16 is more preferable, and 3.5 to 10 is more preferable.
本発明の液体口腔用組成物は、透明性を有する透明液体口腔用組成物であることが好ましい。本発明において透明性を有するとは、白濁しておらず、析出物や沈殿物が形成されていない、無色又は有色の透明又は半透明であることを意味し、具体的には、光路長10mmのセル(ポリスチレン製)における吸収波長550nmの光の透過率が80%以上であることが好ましく、透過率90%以上であることがさらに好ましい。 The liquid oral composition of the present invention is preferably a transparent liquid oral composition having transparency. In the present invention, having transparency means being colorless or colored, transparent or translucent, not being clouded, having no precipitate or precipitate formed therein, and specifically, an optical path length of 10 mm. In the cell (made of polystyrene), the transmittance of light having an absorption wavelength of 550 nm is preferably 80% or more, and more preferably 90% or more.
本発明の液体口腔用組成物は、アシルサルコシン又はその塩(A)及び硫酸エステル又はその塩(D)以外の他のアニオン界面活性剤を含有することができる。他のアニオン界面活性剤としては、アシルサルコシン以外のアシルアミノ酸又はその塩、ラウロイルメチルタウリンナトリウム等のアシルタウリン又はその塩、並びにアルキルリン酸エステル、ポリオキシアルキレン化アルキルリン酸エステル、ポリオキシアルキレン化アシルアミノ酸、アミノ脂肪酸、及びこれらの塩から選ばれる1種又は2種以上が好ましく、液体口腔用組成物の収容容器への充填性、使用時における爽快感を維持する観点から、含有する場合は1質量%以下であることが好ましく、0.5質量%以下がより好ましく、0.1質量%以下がさらに好ましく、或いは含有しなくてもよい。 The composition for liquid oral cavity of the present invention can contain an anionic surfactant other than acyl sarcosine or a salt thereof (A) and a sulfate ester or a salt thereof (D). Other anionic surfactants include acyl amino acids other than acyl sarcosine or salts thereof, acyl taurines or salts thereof such as sodium lauroylmethyltaurine, alkyl phosphate esters, polyoxyalkylenated alkyl phosphate esters, polyoxyalkylenated esters One or more selected from acylamino acids, amino fatty acids, and salts thereof are preferable. From the viewpoint of maintaining the filling property of the liquid oral composition into the container and the refreshing feeling during use, The content is preferably 1% by mass or less, more preferably 0.5% by mass or less, further preferably 0.1% by mass or less, or may not be contained.
本発明の液体口腔用組成物は、ノニオン界面活性剤を含有することができる。ノニオン界面活性剤は、ポリオキシエチレン硬化ヒマシ油、ポリオキシエチレンアルキルエーテル、ポリオキシエチレンポリオキシプロピレン共重合体、ショ糖脂肪酸エステル、ソルビタン脂肪酸エステル、グリセリン脂肪酸エステル、ポリグリセリン脂肪酸エステル、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ソルビット脂肪酸エステル、ポリオキシエチレングリセリン脂肪酸エステル、ポリオキシエチレングリコール脂肪酸エステル、ポリオキシエチレンフィトステロール及びフィトスタノール、ポリオキシエチレンラノリン及びラノリンアルコール、ポリオキシエチレンアルキルアミン及び脂肪酸アミド、ポリオキシエチレンアルキルフェニルホルムアルデヒド縮合物、ポリオキシエチレンポリオキシプロピレンアルキルエーテル、ポリオキシエチレンアルキルフェニルエーテル、ポリオキシエチレンアルキルフェニルエーテル及び脂肪酸エタノールアミドから選ばれる1種又は2種以上が好ましく、後味の点から、脂肪酸の炭素数が8〜20の脂肪酸エステル類が好ましく、安定性や香料(E)の溶解性の点、及び透明性の点から、ポリオキシエチレン硬化ヒマシ油、ポリグリセリン脂肪酸エステルから選ばれる1種又は2種以上が好ましい。ノニオン界面活性剤は、含有していなくてもよいが、本発明の液体口腔用組成物中に0.01〜1質量%含有することが好ましく、0.02〜0.7質量%含有することがより好ましく、0.05〜0.5質量%含有することがさらに好ましい。 The liquid oral cavity composition of the present invention can contain a nonionic surfactant. Nonionic surfactant is polyoxyethylene hydrogenated castor oil, polyoxyethylene alkyl ether, polyoxyethylene polyoxypropylene copolymer, sucrose fatty acid ester, sorbitan fatty acid ester, glycerin fatty acid ester, polyglycerin fatty acid ester, polyoxyethylene Sorbitan fatty acid ester, polyoxyethylene sorbit fatty acid ester, polyoxyethylene glycerin fatty acid ester, polyoxyethylene glycol fatty acid ester, polyoxyethylene phytosterol and phytostanol, polyoxyethylene lanolin and lanolin alcohol, polyoxyethylene alkylamine and fatty acid amide, Polyoxyethylene alkylphenyl formaldehyde condensate, polyoxyethylene polyoxypropylene 1 type or 2 or more types selected from polyalkylethylene, polyoxyethylene alkylphenyl ether, polyoxyethylene alkylphenyl ether and fatty acid ethanolamide are preferable, and fatty acid esters having 8 to 20 carbon atoms of fatty acid from the viewpoint of aftertaste From the viewpoint of stability, solubility of the fragrance (E), and transparency, one or more selected from polyoxyethylene hydrogenated castor oil and polyglycerin fatty acid ester are preferred. The nonionic surfactant may not be contained, but is preferably contained in the liquid oral composition of the present invention in an amount of 0.01 to 1% by mass, and 0.02 to 0.7% by mass. Is more preferable, and it is further more preferable to contain 0.05-0.5 mass%.
本発明の液体口腔用組成物のpHは、25℃におけるpHであって、味及び安定性の点から、5.5〜9であることが好ましい。 The pH of the liquid oral cavity composition of the present invention is a pH at 25 ° C., and is preferably 5.5 to 9 from the viewpoint of taste and stability.
本発明の液体口腔用組成物は、さらに味を良好にする点から、トレハロース及び/又はグリセリンを含有することが好ましい。トレハロース及びグリセリンの合計含有量は、0〜8質量%が好ましく、1〜7質量%がより好ましく、2〜6質量%がさらに好ましい。 The liquid oral composition of the present invention preferably contains trehalose and / or glycerin from the viewpoint of further improving the taste. 0-8 mass% is preferable, as for total content of a trehalose and glycerol, 1-7 mass% is more preferable, and 2-6 mass% is further more preferable.
本発明の液体口腔用組成物は、洗口剤、マウススプレー、塗布剤等として口腔内に適用することが可能であり、口腔内に適用することによって、外因性着色除去効果をもたらし、しかも低温において保存中に析出物の形成と白濁が抑制され、安定性に優れる。外因性着色の要因である着色汚れとしては、油や、タバコの汚れのほか、緑茶、紅茶、ウーロン茶などの茶渋の汚れ、及び現実の口腔内におけるこれらの混合着色汚れが挙げられ、いずれの着色汚れに対しても高い除去効果を有する。かかる効果を向上する点から、本発明の液体口腔用組成物は、口腔内に30秒〜5分間適用することが好ましく、30秒〜3分間適用することがより好ましい。 The liquid oral composition of the present invention can be applied to the oral cavity as a mouthwash, a mouse spray, a coating agent, etc., and when applied to the oral cavity, it provides an exogenous color removal effect, and at a low temperature. The formation of precipitates and white turbidity are suppressed during storage, and the stability is excellent. As coloring stains that are factors of extrinsic coloring, in addition to oil and tobacco stains, green tea, black tea, oolong tea and other tea stains, and actual mixed colored stains in the oral cavity can be mentioned. High removal effect against dirt. From the viewpoint of improving such effects, the liquid oral composition of the present invention is preferably applied in the oral cavity for 30 seconds to 5 minutes, more preferably 30 seconds to 3 minutes.
本発明の液体口腔用組成物は、上記成分の他、本発明の効果を損なわない範囲内で、甘味剤、湿潤剤、pH調整剤、エタノール、糖アルコール、殺菌剤、薬効成分、色素等を適宜含有することができる。甘味剤としては、サッカリンナトリウム、スクラロースが挙げられる。上記成分の他の湿潤剤としては、ポリエチレングリコール、プロピレングリコール、1、3-ブチレングリコール、ソルビトール等が挙げられる。pH調整剤としては、リンゴ酸、クエン酸、水酸化ナトリウム、水酸化カリウムが挙げられ、味の点からリンゴ酸、水酸化カリウムが好ましい。糖アルコールとしては、キシリトール、エリスリトール、還元パラチノース等が挙げられ、殺菌剤としては、塩化ベンゼトニウム、塩化セチルピリジニウム、イソプロピルメチルフェノール、トリクロサン等が挙げられる。 The liquid oral composition of the present invention contains, in addition to the above components, sweeteners, wetting agents, pH adjusters, ethanol, sugar alcohols, bactericides, medicinal ingredients, pigments, etc. within the range not impairing the effects of the present invention. It can contain suitably. Examples of the sweetening agent include saccharin sodium and sucralose. Other wetting agents for the above components include polyethylene glycol, propylene glycol, 1,3-butylene glycol, sorbitol and the like. Examples of the pH adjuster include malic acid, citric acid, sodium hydroxide, and potassium hydroxide. Malic acid and potassium hydroxide are preferable from the viewpoint of taste. Examples of sugar alcohols include xylitol, erythritol, and reduced palatinose. Examples of bactericides include benzethonium chloride, cetylpyridinium chloride, isopropylmethylphenol, and triclosan.
以下、本発明について、実施例に基づき具体的に説明するが、本発明はこれら実施例に限定されるものではない。 EXAMPLES Hereinafter, although this invention is demonstrated concretely based on an Example, this invention is not limited to these Examples.
[実施例1〜8及び比較例1〜8]
表1に示す処方にしたがって、液体口腔用組成物を調製した。これらの液体口腔用組成物を以下の外因性着色除去試験、保存安定性試験を行い、保存安定性試験前の組成物について以下の基準で味を評価した。結果を表1に示す。
[Examples 1-8 and Comparative Examples 1-8]
According to the formulation shown in Table 1, a liquid oral composition was prepared. These liquid oral compositions were subjected to the following exogenous color removal test and storage stability test, and the taste of the composition before the storage stability test was evaluated according to the following criteria. The results are shown in Table 1.
<外因性着色除去試験>
1 外因性着色モデルの作成
ハイドロキシアパタイトペレット(PENTAX製APP-100 1cm×1cm)を耐水性の研磨紙(360番)で研磨する。これを外因性着色前のハイドロキシアパタイトペレットとする。次に、ハイドロキシアパタイトペレットを、タンパク質溶液(BSA 10000ppm溶液)、紅茶(日東紅茶製 デイリークラブ)ティバッグ1つに対して50mLの沸騰させた熱湯で抽出した抽出液、人工唾液(20mM HEPES、1.5mL CaCl2、0.9mM KH2PO4)の各10mLに順に5分ずつ浸漬させた。この処理を10サイクル行った後に3時間自然乾燥させた。処理後のハイドロキシアパタイトペレットを、吸入路と吸引路とを備える密封容器(容量3L、プラスチック製)内におき、2本のタバコ(ピース 日本たばこ産業製)を1本づつ、一端を容器の外側から嵌めこみ、吸引路から1本が約2分で燃え尽きる程度に空気を吸引した。これにより、タバコを通して吸入路から密封容器内に空気が吸引される際に、タバコの煙が容器内に吸引され、容器内にタバコの煙が広がるが、吸入路から煙が積極的に排出されることを防止しつつ、密封容器内をタバコの煙で充満させることができる。1本目のタバコが消えてからすぐに2本目のタバコを挿入し、同様に吸引しつつタバコの煙で密封容器内を満たした。2本目のタバコの火が消えてから吸引を止めて1時間置くとタバコの煙が密封容器の下方に沈んだ状態となった。このように1時間置いた後に、ハイドロキシアパタイトペレットを密封容器から取り出し、外因性着色モデルとして、茶渋とタバコの汚れとが付着したハイドロキシアパタイトペレットを得た。
<Exogenous color removal test>
1 Creation of Exogenous Coloring Model Hydroxyapatite pellets (APP-100 manufactured by PENTAX 1 cm × 1 cm) are polished with water-resistant abrasive paper (No. 360). This is a hydroxyapatite pellet before exogenous coloring. Next, an extract obtained by extracting hydroxyapatite pellets with 50 mL of boiling hot water with respect to one protein solution (BSA 10000 ppm solution) and one black tea (Daily Club daily club) tea bag, artificial saliva (20 mM HEPES, 1 .5 mL CaCl 2 , 0.9 mM KH 2 PO 4 ) were immersed in 10 mL each for 5 minutes in order. After 10 cycles of this treatment, it was naturally dried for 3 hours. The treated hydroxyapatite pellets are placed in a sealed container (capacity 3L, made of plastic) with a suction channel and a suction channel. Two cigarettes (Peace Japan Tobacco Inc.) one by one, one end outside the container The air was sucked to such an extent that one burned out from the suction passage in about 2 minutes. As a result, when air is sucked into the sealed container from the suction path through the cigarette, the smoke of the cigarette is sucked into the container, and the smoke of the cigarette spreads into the container, but the smoke is actively discharged from the suction path. The inside of the sealed container can be filled with tobacco smoke. Immediately after the first cigarette disappeared, the second cigarette was inserted, and the inside of the sealed container was filled with cigarette smoke while sucking in the same manner. After the second cigarette was extinguished, the suction was stopped and left for 1 hour. The cigarette smoke sank below the sealed container. After leaving for 1 hour in this manner, the hydroxyapatite pellets were taken out from the sealed container to obtain hydroxyapatite pellets with tea astringent and tobacco stains attached as an exogenous coloring model.
2 外因性着色除去処理
外因性着色モデルのハイドロキシアパタイトペレットを、室温(25℃)において表1に示す各実施例又は比較例の液体口腔用組成物に30秒間浸漬して取り出し、水で洗った後、自然乾燥させた。
2 Exogenous coloring removal treatment The exogenous coloring model hydroxyapatite pellets were immersed in the liquid oral composition of each Example or Comparative Example shown in Table 1 at room temperature (25 ° C.) for 30 seconds and washed with water. After that, it was naturally dried.
3 外因性着色の除去率
外因性着色の程度は、ハイドロキシアパタイトペレットのL*a*b*表示におけるb*の値により判断した。b*は、歯科用色彩系シェードアイ(松風製)で測定し、外因性着色前のハイドロキシアパタイトペレットのb*値をb*0、着色汚れが付着した後の外因性着色モデルのb*値をb*1、実施例又は比較例の液体口腔用組成物により外因性着色除去処理を行った後の外因性着色モデルのb*値をb*2とし、以下の式(1)により外因性着色の除去率を求めた。
外因性着色の除去率=100×(1−(b*2−b*0)/(b*1−b*0))
・・・(1)
3. Exogenous coloring removal rate The degree of exogenous coloring was judged by the value of b * in the L * a * b * display of the hydroxyapatite pellets. b * is measured with a dental color shade eye (manufactured by Matsukaze). The b * value of the hydroxyapatite pellet before exogenous coloring is b * 0, and the b * value of the exogenous coloring model after coloring stains are attached. B * 1, the b * value of the extrinsic coloring model after performing the exogenous coloring removal treatment with the liquid oral composition of Example or Comparative Example is b * 2, and the exogenous by the following formula (1) The color removal rate was determined.
Exogenous coloring removal rate = 100 × (1- (b * 2-b * 0) / (b * 1-b * 0))
... (1)
<保存安定性試験>
保存安定性は、各液体組成物を5℃で1ヶ月保存し、保存後の組成物の状態を確認した。評価は以下の基準により行った。
○ :析出物、濁り、分離などがなく透明である。
× :析出物、濁り、分離などがみられた。
<Storage stability test>
For storage stability, each liquid composition was stored at 5 ° C. for 1 month, and the state of the composition after storage was confirmed. Evaluation was performed according to the following criteria.
○: Transparent with no precipitates, turbidity, separation, etc.
X: Precipitation, turbidity, separation, etc. were observed.
<味の評価>
味は、塩味がするか否かにより以下の基準で判断した。判断は専門パネラー2名により行い、協議により以下の基準で判断した。
4 :塩味は感じない。
3 :塩味を殆ど感じない(わずかには感じる)。
2 :塩味を感じる。
1 :塩味を強く感じる。
<Evaluation of taste>
The taste was judged according to the following criteria depending on whether or not it tastes salty. Judgment was made by two expert panelists, and the following criteria were determined through consultation.
4: Does not feel salty.
3: Almost no salty taste (feels slightly).
2: Feels salty.
1: Strongly salty.
表1に示すように、実施例1〜8の液体口腔用組成物は、たばこと茶渋の複数混在した頑固な着色汚れ(外因性着色汚れ)に対しても、70%以上の高い除去率を示し、しかも低温の保存安定性、味に優れ、爽快感のあるものであった。これに対して、比較例2、3、6、7は、これら着色汚れの除去率が低く、低温保存後に分離又は白濁が確認された。比較例1、4、8は保存安定性や味は良好であるものの、着色汚れの除去率は低く、比較例5は着色汚れの除去率は高いものの、保存後に組成物の析出物が確認された。 As shown in Table 1, the liquid oral compositions of Examples 1 to 8 have a high removal rate of 70% or more against stubborn colored stains (exogenous colored stains) in which a plurality of tobacco and tea astringents are mixed. In addition, it was excellent in storage stability at low temperature, excellent in taste, and refreshing. In contrast, Comparative Examples 2, 3, 6, and 7 had a low removal rate of these colored stains, and separation or cloudiness was confirmed after low-temperature storage. Comparative Examples 1, 4, and 8 have good storage stability and taste, but the removal rate of colored stains is low. In Comparative Example 5, the removal rate of colored stains is high, but deposits of the composition were confirmed after storage. It was.
[実施例9及び比較例9]
実施例1と同様にして、表2に示す処方にしたがって液体口腔用組成物を製造した。次いで、収容容器への充填性と、使用時における爽快感の有無によって使用感を評価した。収容容器への充填性は、製造した液体口腔用組成物を450gとり、500mLの収容容器(ポリエチレンテレフタレート製、容器本体は横断面が楕円の円柱型で吐出口の直径が20mmの容器)の吐出口から泡があふれることなく充填する際に要する最短時間について、20秒を基準時間として評価した。20秒よりも充填時間が長い場合を×とし、20秒以内に充填が可能な場合を○とした。評価結果を表2に示す。
[Example 9 and Comparative Example 9]
In the same manner as in Example 1, a liquid oral composition was produced according to the formulation shown in Table 2. Next, the feeling of use was evaluated based on the filling properties of the container and the presence or absence of a refreshing feeling during use. The filling property into the container is 450 g of the produced liquid oral composition, and the discharge of a 500 mL container (made of polyethylene terephthalate, the container body is a cylinder with an elliptical cross section and a discharge port diameter of 20 mm). The shortest time required for filling without bubbles overflowing from the outlet was evaluated using 20 seconds as a reference time. The case where the filling time was longer than 20 seconds was marked as x, and the case where filling was possible within 20 seconds was marked as ◯. The evaluation results are shown in Table 2.
表2に示すように、実施例9及び比較例9はいずれも塩味は感じられないものの、比較例9は口腔内に適用して含嗽した場合に、香味が感じにくく、爽快感に劣るのに対して、実施例9は香味が良好で、爽快感も感じられた。また、比較例9は収容容器への充填時間が基準時間を超え、製造性に課題があるのに対して、実施例9は収容容器への充填を基準時間内で速やかに行うことができた。 As shown in Table 2, although both Example 9 and Comparative Example 9 do not feel salty, Comparative Example 9 is difficult to feel the flavor and inferior in refreshment when applied to the oral cavity. In contrast, Example 9 had a good flavor and a refreshing feeling. Further, in Comparative Example 9, the filling time of the storage container exceeded the reference time, and there was a problem in manufacturability, whereas Example 9 was able to quickly fill the storage container within the reference time. .
Claims (7)
(A)アシルサルコシン又はその塩 0.02〜0.5質量%、
(B)ポリリン酸又はその塩 0.5〜5質量%、及び
(C)水 75〜95質量%
を含有し、かつ(D)アニオン界面活性剤としての硫酸エステル又はその塩を含有しないか、或いは含有量が0.001質量%以下であり、
成分(B)と成分(A)の含有量の質量比(B/A)が2〜50である液体口腔用組成物。 The following components (A), (B) and (C):
(A) acyl sarcosine or a salt thereof 0.02 to 0.5% by mass,
(B) polyphosphoric acid or its salt 0.5-5 mass%, and (C) water 75-95 mass%
And (D) does not contain a sulfate ester or a salt thereof as an anionic surfactant, or the content is 0.001% by mass or less,
Liquid oral cavity composition whose mass ratio (B / A) of content of a component (B) and a component (A) is 2-50.
成分(A)の含有量に対する、成分(B)及び成分(E)の含有量の合計の質量比((B+E)/A)が3〜50である請求項1に記載の液体口腔用組成物。 (E) containing a fragrance,
The composition for liquid oral cavity according to claim 1, wherein the total mass ratio ((B + E) / A) of the content of the component (B) and the component (E) to the content of the component (A) is 3 to 50. .
成分(E)の含有量に対する、成分(B)の含有量の質量比(B/E)が2〜20である請求項1又は2に記載の液体口腔用組成物。 (E) contains a fragrance,
The liquid oral cavity composition according to claim 1 or 2, wherein the mass ratio (B / E) of the content of the component (B) to the content of the component (E) is 2 to 20.
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Cited By (2)
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JP2013209311A (en) * | 2012-03-30 | 2013-10-10 | Sunstar Inc | Stain formation inhibiting liquid composition for oral cavity with excellent storage stability |
JPWO2014050851A1 (en) * | 2012-09-27 | 2016-08-22 | 大正製薬株式会社 | Oral liquid composition |
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JPH08301742A (en) * | 1995-04-28 | 1996-11-19 | Ezaki Glico Co Ltd | Composition for oral cavity for preventing reduction in ph(potential of hydrogen) of saliva |
JPH10182387A (en) * | 1996-12-25 | 1998-07-07 | Lion Corp | Remover for coating of tongue |
JPH1121216A (en) * | 1997-06-30 | 1999-01-26 | Lion Corp | Composition for oral cavity |
JP2010143843A (en) * | 2008-12-18 | 2010-07-01 | Lion Corp | Liquid composition for oral cavity |
JP2011168506A (en) * | 2010-02-16 | 2011-09-01 | Lion Corp | Method for producing composition for oral cavity |
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Patent Citations (5)
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JPH08301742A (en) * | 1995-04-28 | 1996-11-19 | Ezaki Glico Co Ltd | Composition for oral cavity for preventing reduction in ph(potential of hydrogen) of saliva |
JPH10182387A (en) * | 1996-12-25 | 1998-07-07 | Lion Corp | Remover for coating of tongue |
JPH1121216A (en) * | 1997-06-30 | 1999-01-26 | Lion Corp | Composition for oral cavity |
JP2010143843A (en) * | 2008-12-18 | 2010-07-01 | Lion Corp | Liquid composition for oral cavity |
JP2011168506A (en) * | 2010-02-16 | 2011-09-01 | Lion Corp | Method for producing composition for oral cavity |
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Publication number | Priority date | Publication date | Assignee | Title |
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JP2013209311A (en) * | 2012-03-30 | 2013-10-10 | Sunstar Inc | Stain formation inhibiting liquid composition for oral cavity with excellent storage stability |
JPWO2014050851A1 (en) * | 2012-09-27 | 2016-08-22 | 大正製薬株式会社 | Oral liquid composition |
JP2018039827A (en) * | 2012-09-27 | 2018-03-15 | 大正製薬株式会社 | Oral liquid composition |
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