JP5999173B2 - Oral composition - Google Patents
Oral composition Download PDFInfo
- Publication number
- JP5999173B2 JP5999173B2 JP2014503784A JP2014503784A JP5999173B2 JP 5999173 B2 JP5999173 B2 JP 5999173B2 JP 2014503784 A JP2014503784 A JP 2014503784A JP 2014503784 A JP2014503784 A JP 2014503784A JP 5999173 B2 JP5999173 B2 JP 5999173B2
- Authority
- JP
- Japan
- Prior art keywords
- composition
- liquid oral
- component
- mass
- oral cavity
- 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.)
- Expired - Fee Related
Links
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- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 229960002920 sorbitol Drugs 0.000 description 1
- 235000010356 sorbitol Nutrition 0.000 description 1
- 235000019721 spearmint oil Nutrition 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 235000019408 sucralose Nutrition 0.000 description 1
- BAQAVOSOZGMPRM-QBMZZYIRSA-N sucralose Chemical compound O[C@@H]1[C@@H](O)[C@@H](Cl)[C@@H](CO)O[C@@H]1O[C@@]1(CCl)[C@@H](O)[C@H](O)[C@@H](CCl)O1 BAQAVOSOZGMPRM-QBMZZYIRSA-N 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229960003080 taurine Drugs 0.000 description 1
- 229960000984 tocofersolan Drugs 0.000 description 1
- 239000000811 xylitol Substances 0.000 description 1
- 235000010447 xylitol Nutrition 0.000 description 1
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 description 1
- 229960002675 xylitol Drugs 0.000 description 1
- GVJHHUAWPYXKBD-IEOSBIPESA-N α-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-IEOSBIPESA-N 0.000 description 1
Classifications
-
- 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
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
- A61K8/347—Phenols
-
- 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
- A61K8/67—Vitamins
- A61K8/676—Ascorbic acid, i.e. vitamin C
-
- 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
- A61K8/86—Polyethers
-
- 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
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Emergency Medicine (AREA)
- Cosmetics (AREA)
Description
本発明は、アスコルビン酸リン酸エステル又はその塩を含有する口腔用組成物に関し、更に詳述すると、中性領域におけるアスコルビン酸リン酸エステル又はその塩の溶解性が向上し、低温保存時のオリ・にごりが抑制され、澄明外観が維持される口腔用組成物に関する。 The present invention relates to a composition for oral cavity containing an ascorbic acid phosphate or a salt thereof. More specifically, the solubility of an ascorbic acid phosphate or a salt thereof in a neutral region is improved, so that -It is related with the composition for oral cavity in which a dust is suppressed and a clear appearance is maintained.
アスコルビン酸は生体中で種々の酵素活性発現に重要な役割を演じ、多様な生理活性を持つことが知られている。特に、プロリル及びリジルヒドロキシラーゼの補酵素として作用し、コラーゲン合成に必須であるとされている。このため、コラーゲンの破壊を伴う歯肉炎、歯周炎の予防、治療に有用であり、従来からアスコルビン酸誘導体が種々開発され、特にアスコルビン酸リン酸エステル及びその塩が注目されている。 Ascorbic acid is known to play an important role in the expression of various enzyme activities in the living body and to have various physiological activities. In particular, it acts as a coenzyme for prolyl and lysyl hydroxylase, and is essential for collagen synthesis. For this reason, it is useful for prevention and treatment of gingivitis and periodontitis accompanied by collagen destruction, and various ascorbic acid derivatives have been conventionally developed, and in particular, ascorbic acid phosphates and salts thereof have attracted attention.
しかし、中性領域において、アスコルビン酸リン酸エステル類を口腔用組成物に配合した場合、低温で長期保存するとアスコルビン酸リン酸エステル類が不溶化しオリやにごりが発生するという課題があった。特に洗口液、液体歯磨等の液体口腔用組成物では、不溶化によるオリやにごりが析出しやすく、低温で長期間保存した後のオリやにごりを抑制することは非常に困難であった。また、アスコルビン酸リン酸エステル類はアルカリ側では安定とされるが、とりわけ液体口腔用組成物では、pHが8を超えると口に含んだときにヌルつきや異味などの違和感が感じられたり、オリが更に発生しやすくなるなど、製剤化に問題が生じるという課題があった。 However, when ascorbic acid phosphates are blended in the oral composition in the neutral region, there is a problem that ascorbic acid phosphates are insolubilized and oliage and dust are generated when stored for a long time at a low temperature. In particular, liquid oral compositions such as mouthwashes and liquid dentifrices are liable to deposit oliage and dirt due to insolubilization, and it is very difficult to suppress oliage and dirt after being stored at low temperatures for a long period of time. In addition, ascorbic acid phosphates are stable on the alkali side, but in particular for liquid oral compositions, when the pH exceeds 8, when the mouth contains it, a feeling of discomfort such as nulliness or taste is felt, There is a problem that problems occur in the formulation, such as the occurrence of orientation more easily.
出願人は、口腔用組成物へのアスコルビン酸リン酸エステル又はその塩の配合技術として特許文献1〜3を提案したが、特許文献1〜3には、上記課題について言及されていない。 Although the applicant has proposed Patent Documents 1 to 3 as a technique for blending an ascorbic acid phosphate ester or a salt thereof into the oral composition, Patent Documents 1 to 3 do not mention the above problem.
従って、アスコルビン酸リン酸エステル又はその塩を含有する口腔用組成物においては、中性領域でのアスコルビン酸リン酸エステル又はその塩の溶解性向上、オリやにごり発生の抑制が技術課題であった。
本発明は、上記事情に鑑みなされたもので、中性領域においてアスコルビン酸リン酸エステル又はその塩の溶解性が向上し、低温保存時のオリ・にごりが抑制され、澄明外観が維持される上記口腔用組成物を提供することを目的とする。Therefore, in the composition for oral cavity containing ascorbic acid phosphate ester or a salt thereof, improvement in solubility of ascorbic acid phosphate ester or a salt thereof in a neutral region, and suppression of occurrence of orientation and dustiness were technical problems. .
The present invention has been made in view of the above circumstances, the solubility of ascorbic acid phosphate ester or a salt thereof is improved in a neutral region, the orientation and dustiness during low-temperature storage is suppressed, and a clear appearance is maintained. It aims at providing the composition for oral cavity.
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、(A)アスコルビン酸リン酸エステル又はその塩(以下、APEと略記する。)を含有する口腔用組成物に、(B)特定の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及びポリグリセリン脂肪酸エステルから選ばれる非イオン性界面活性剤と、(C)イソプロピルメチルフェノール、トリクロサン及びチモールから選ばれる芳香族化合物とを配合し、(A)成分と(C)成分の配合比率(A)/(C)が質量比として1〜50であり、かつ25℃の時のpHが6.5〜8.0であることによって、かかるpH領域でAPEの溶解性が向上し、特に液体口腔用組成物で、低温保存時のオリ・にごりが抑制され、澄明な外観を調製直後から長期に亘って維持できることを見出した。また、製剤を口に含んだときの違和感のなさに優れることを見出した。 As a result of intensive studies to achieve the above object, the present inventors have developed (B) an ascorbic acid phosphate ester or a salt thereof (hereinafter abbreviated as APE) into an oral composition (B). ) Blended with specific polyoxyethylene hydrogenated castor oil, polyoxyethylene alkyl ether and non-ionic surfactant selected from polyglycerin fatty acid ester and (C) aromatic compound selected from isopropylmethylphenol, triclosan and thymol When the blending ratio (A) / (C) of the component (A) and the component (C) is 1 to 50 as a mass ratio, and the pH at 25 ° C. is 6.5 to 8.0. In such a pH range, the solubility of APE is improved, especially in the liquid oral composition, the orientation and dustiness during low-temperature storage is suppressed, and a clear appearance is maintained for a long time immediately after preparation. It was found to be able to equity. Moreover, it discovered that it was excellent in the uncomfortable feeling when a formulation was included in the mouth.
なお、特許文献1〜3には、APE含有口腔用組成物として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等の非イオン性界面活性剤、イソプロピルメチルフェノールが配合された組成が開示されている。しかし、引用文献1〜3に開示された技術は、中性領域でのAPEの溶解性を改善し低温保存時のオリ・にごりの発生を抑制したものではない。このような引用文献1〜3から、本発明の構成によって中性領域でのAPEの溶解性が改善し、低温保存時のオリ・にごり発生を抑制し得ることは予測できない。
本発明では、意外なことに(C)成分の芳香族化合物に、中性領域でのAPEの溶解性改善作用があり、(B)、(C)成分の併用で、中性領域におけるAPEの溶解性改善、低温保存でのオリ・にごりの抑制、澄明外観の維持、更には違和感の抑制をなし得たものである。とりわけAPEを含有する液体製剤においては、低温保存すると製剤を単独で目視しただけでは認識できず対照と比較することで初めて認識できるようなオリ・にごりが発生し、このようなオリ・にごりを抑えることは従来の技術ではできなかったが、本発明によれば、かかるオリ・にごりを抑制し、澄明性の高い液体製剤を与えることができる。なお、このようなオリ・にごりの抑制は、(C)成分の芳香族化合物に特異的なもので、他の芳香族化合物や殺菌剤ではなし得ない格別なものである。Patent Documents 1 to 3 disclose a composition in which a nonionic surfactant such as polyoxyethylene hydrogenated castor oil and polyoxyethylene alkyl ether and isopropylmethylphenol are blended as an APE-containing oral composition. Yes. However, the techniques disclosed in Cited Documents 1 to 3 do not improve the solubility of APE in the neutral region and do not suppress the occurrence of orientation and dust during low-temperature storage. From these cited references 1 to 3, it is not predictable that the structure of the present invention improves the solubility of APE in the neutral region and can suppress the occurrence of orientation and dust during low-temperature storage.
In the present invention, surprisingly, the aromatic compound (C) has an effect of improving the solubility of APE in the neutral region, and the combined use of the components (B) and (C) results in the APE in the neutral region. It was able to improve solubility, suppress orientation and dirt during low-temperature storage, maintain a clear appearance, and suppress discomfort. In particular, in liquid preparations containing APE, when stored at low temperature, the preparation cannot be recognized only by visually observing the preparation alone. However, according to the present invention, it is possible to suppress such squeeze and to provide a liquid formulation with high clarity. In addition, such suppression of the orientation and dust is specific to the aromatic compound of component (C), and is a special thing that cannot be achieved with other aromatic compounds or fungicides.
また、上記組成物に更に(D)アルキル硫酸ナトリウムを配合すると、オリ・にごりの抑制効果をより向上できる。 In addition, when (D) sodium alkyl sulfate is further added to the above composition, the effect of suppressing the dirt and dust can be further improved.
従って、本発明は下記の液体口腔用組成物を提供する。
〔1〕
(A)アスコルビン酸リン酸エステルマグネシウム塩を0.1〜2質量%含有する液体口腔用組成物であって、
(B)エチレンオキサイドの平均付加モル数が40〜100モルのポリオキシエチレン硬化ヒマシ油、アルキル基の炭素数が16〜18でエチレンオキサイドの平均付加モル数が20〜40モルのポリオキシエチレンアルキルエーテル及び脂肪酸の炭素数が12〜18の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種以上の非イオン性界面活性剤を0.2〜1.0質量%と、
(C)イソプロピルメチルフェノール、トリクロサン及びチモールから選ばれる1種又は2種以上の芳香族化合物を0.02〜0.07質量%と
を含有してなり、(A)成分と(C)成分の配合比率(A)/(C)が質量比として3〜30であり、かつ25℃の時のpHが6.5〜7.8であることを特徴とする液体口腔用組成物。
〔2〕
(C)成分がイソプロピルメチルフェノールである〔1〕に記載の液体口腔用組成物。
〔3〕
更に、(D)アルキル硫酸ナトリウムを0.05〜1.0質量%含有してなる〔1〕又は〔2〕に記載の液体口腔用組成物。
〔4〕
組成物中の界面活性剤総量が0.2〜1.3質量%である〔1〕〜〔3〕のいずれかに記載の液体口腔用組成物。
〔5〕
液体歯磨又は洗口剤である〔1〕〜〔4〕のいずれかに記載の液体口腔用組成物。
〔6〕
研磨剤を含有しない〔1〕〜〔5〕のいずれかに記載の液体口腔用組成物。
〔7〕
澄明な外観を有する〔1〕〜〔6〕のいずれかに記載の液体口腔用組成物。
Accordingly, the present invention provides the following liquid oral composition.
[1]
(A) A liquid oral composition ascorbic acid phosphate ester magnesium salt containing 0.1 to 2 wt%,
(B) Polyoxyethylene hydrogenated castor oil having an average addition mole number of ethylene oxide of 40 to 100 moles, polyoxyethylene alkyl having an alkyl group of 16 to 18 carbon atoms and an average addition mole number of ethylene oxide of 20 to 40 moles 0.2 to 1.0% by mass of one or more nonionic surfactants selected from ether and fatty acid esters having 12 to 18 carbon atoms of fatty acid,
(C) One or two or more aromatic compounds selected from isopropylmethylphenol, triclosan, and thymol are contained in an amount of 0.02 to 0.07% by mass, and the components (A) and (C) A composition for liquid oral cavity, wherein the blending ratio (A) / (C) is 3 to 30 as a mass ratio, and the pH at 25 ° C. is 6.5 to 7.8 .
[2]
(C) Liquid oral cavity composition as described in [1] whose component is isopropylmethylphenol.
[3 ]
Furthermore, (D) Liquid oral cavity composition as described in [1] or [2] which contains 0.05-1.0 mass% of sodium alkyl sulfate.
[ 4 ]
Surfactants The total amount of the composition is from 0.2 to 1.3 wt% (1) to the liquid oral composition according to any one of [3].
[5 ]
The liquid oral composition according to any one of [ 1] to [4], which is a liquid dentifrice or mouthwash .
[6]
The liquid oral composition according to any one of [1] to [5], which does not contain an abrasive.
[7]
The liquid oral composition according to any one of [1] to [6], which has a clear appearance.
本発明によれば、アスコルビン酸リン酸エステル又はその塩を含有する口腔用組成物において、中性領域でのアスコルビン酸リン酸エステル又はその塩の溶解性が向上し、低温保存時のオリ・にごりが抑制され、澄明な外観を調製直後から長期に亘って維持することができる。また、違和感のない製剤を与えることができる。 According to the present invention, in an oral composition containing an ascorbic acid phosphate or a salt thereof, the solubility of the ascorbic acid phosphate or a salt thereof in the neutral region is improved, so Is suppressed, and a clear appearance can be maintained for a long time immediately after preparation. Moreover, the formulation without a sense of incongruity can be given.
以下、本発明につき更に詳述する。本発明の口腔用組成物は、(A)アスコルビン酸リン酸エステル又はその塩、(B)特定の非イオン性界面活性剤、(C)イソプロピルメチルフェノール、トリクロサン及びチモールから選ばれる芳香族化合物を含有し、(A)成分/(C)成分の配合比率、pHが適切範囲であることを特徴とする。 The present invention will be described in further detail below. The composition for oral cavity of the present invention comprises an aromatic compound selected from (A) ascorbic acid phosphate or a salt thereof, (B) a specific nonionic surfactant, (C) isopropylmethylphenol, triclosan and thymol. And the mixing ratio of component (A) / component (C) and pH are in an appropriate range.
(A)アスコルビン酸リン酸エステル又はその塩は、アスコルビン酸の2,3,5,6位のいずれかの水酸基の1つ又は2つ以上がリン酸、ポリリン酸等の化合物のエステルとなったものであり、例えば、アスコルビン酸リン酸エステルとしてアスコルビン酸−2−リン酸エステル、アスコルビン酸−3−リン酸エステル、アスコルビン酸−6−リン酸エステル、アスコルビン酸−2−ポリリン酸エステル等が挙げられる。その塩類としては、ナトリウム塩、カリウム塩、カルシウム塩、マグネシウム塩等のアルカリ金属塩、アルカリ土類金属塩が挙げられる。これらの中で、特に組成物の安定性の点から、アスコルビン酸の2位又は3位の水酸基がリン酸エステル化された誘導体が好ましく、より好ましくはアスコルビン酸−2−リン酸エステルのマグネシウム塩やナトリウム塩である。特にアスコルビン酸−2−リン酸エステルのマグネシウム塩は、液体製剤に配合すると低温保存時にオリ・にごりが生じ易いが、本発明によればかかる液体製剤のオリ・にごりの発生を抑え、澄明性を維持できる。 (A) Ascorbic acid phosphate or a salt thereof is an ester of a compound such as phosphoric acid or polyphosphoric acid in which one or more of the hydroxyl groups at positions 2, 3, 5, and 6 of ascorbic acid For example, ascorbic acid-2-phosphate, ascorbic acid-3-phosphate, ascorbic acid-6-phosphate, ascorbic acid-2-polyphosphate, etc. It is done. Examples of the salts include alkali metal salts such as sodium salt, potassium salt, calcium salt, and magnesium salt, and alkaline earth metal salts. Among these, from the viewpoint of the stability of the composition, a derivative in which the hydroxyl group at the 2-position or 3-position of ascorbic acid is converted to a phosphate ester is preferable, and a magnesium salt of ascorbic acid-2-phosphate is more preferable. Or sodium salt. In particular, the magnesium salt of ascorbic acid-2-phosphate is liable to cause odor and dust when stored at a low temperature when blended in a liquid formulation, but according to the present invention, the occurrence of odor and dust in such a liquid formulation is suppressed and the clarity is improved. Can be maintained.
(A)アスコルビン酸リン酸エステル又はその塩の配合量は、組成物全体の0.1〜2%(質量%、以下同様。)が好ましく、より好ましくは0.2〜2%、さらに好ましくは0.2〜1%である。配合量が多いほど、歯周疾患の予防効果といった配合効果が十分に発揮されるが、2%以下であることが、低温保存でのオリ・にごりを抑制するには好適である。また、異味等による口に含んだ時の違和感を抑えて良好な使用感を維持するには好適である。 (A) The compounding quantity of ascorbic acid phosphate ester or its salt is preferably 0.1 to 2% (mass%, the same applies hereinafter) of the whole composition, more preferably 0.2 to 2%, and still more preferably. 0.2 to 1%. The larger the blending amount, the more the blending effect such as periodontal disease preventive effect is exhibited. However, the content of 2% or less is suitable for suppressing the squeeze and dirt at low temperature storage. Moreover, it is suitable for maintaining a good feeling of use while suppressing a sense of incongruity when it is put in the mouth due to a nasty taste or the like.
(B)成分は、エチレンオキサイドの平均付加モル数(以下、E.O.付加モル数と略記する。)が40〜100モルのポリオキシエチレン硬化ヒマシ油、アルキル基の炭素数が16〜18でE.O.付加モル数が20〜40モルのポリオキシエチレンアルキルエーテル、脂肪酸の炭素数が12〜18のポリグリセリン脂肪酸エステルから選ばれる非イオン性界面活性剤である。
(B)成分は、安定化剤として配合されるもので、(C)成分と併用して配合することで、(A)成分を含有する口腔用組成物の調製直後の外観を澄明にし、また、低温保存後のオリ・にごり発生及び違和感発現を抑制する効果を与える。The component (B) is a polyoxyethylene hydrogenated castor oil having an average added mole number of ethylene oxide (hereinafter abbreviated as EO added mole number) of 40 to 100 moles, and an alkyl group having 16 to 18 carbon atoms. In E. O. It is a nonionic surfactant selected from polyoxyethylene alkyl ethers having an addition mole number of 20 to 40 moles and polyglycerol fatty acid esters having a fatty acid carbon number of 12 to 18.
The component (B) is blended as a stabilizer. By blending with the component (C), the appearance immediately after preparation of the oral composition containing the component (A) is clarified, and In addition, it has the effect of suppressing the occurrence of orientation and tingling and the appearance of discomfort after low-temperature storage.
(B)成分としては、調製直後の澄明性、低温保存後のオリ・にごり抑制効果、口に含んだときの違和感のなさの点で、E.O.付加モル数が40〜100モル、好ましくは60〜100モルのポリオキシエチレン硬化ヒマシ油、アルキル基の炭素数が16(セチル)〜18(ステアリル)でE.O.付加モル数が20〜40モルのポリオキシエチレンアルキルエーテル、脂肪酸の炭素数が12(ラウリン酸)〜18(ステアリン酸)、好ましくは12(ラウリン酸)〜14(ミリスチン酸)のポリグリセリン脂肪酸エステルが好適であり、これらから選ばれる1種又は2種以上の非イオン性界面活性剤が用いられる。 As the component (B), E.C. has been disclosed in terms of clarity immediately after preparation, an effect of suppressing orientation and dustiness after low-temperature storage, and a sense of incongruity when contained in the mouth. O. A polyoxyethylene hydrogenated castor oil having an added mole number of 40 to 100 moles, preferably 60 to 100 moles, and an alkyl group having 16 (cetyl) to 18 (stearyl) carbon atoms. O. Polyoxyethylene alkyl ether having an addition mole number of 20 to 40 moles, polyglycerol fatty acid ester having a fatty acid carbon number of 12 (lauric acid) to 18 (stearic acid), preferably 12 (lauric acid) to 14 (myristic acid) And one or more nonionic surfactants selected from these are used.
ポリオキシエチレン硬化ヒマシ油のE.O.付加モル数が40モル未満では、可溶化力、それ自身の口腔用組成物への溶解性が低く、製剤調製直後の澄明性及び低温保存時のオリ・にごり抑制効果に劣る。100モルを超えるものは市販されていない。
ポリオキシエチレンアルキルエーテルのE.O.付加モル数が20モル未満では、可溶化力が低く、また、それ自身の口腔用組成物への溶解性が低く、(A)成分や(C)成分の可溶化、製剤調製直後の澄明性及び低温保存時のオリ・にごり抑制効果に劣る。40モルを超えるものは市販されていない。また、ポリオキシエチレンアルキルエーテルにおいてアルキル基の炭素数が16未満のものや18を超えるものでは、低温保存時のオリ・にごり抑制効果に劣る。
ポリグリセリン脂肪酸エステルの脂肪酸の炭素数が12未満のものや18を超えるものは可溶化力が低く、(A)成分や(C)成分の可溶化、製剤調製直後の澄明性及び低温保存時のオリ・にごりの抑制効果に劣る。E. of polyoxyethylene hydrogenated castor oil O. If the number of added moles is less than 40 moles, the solubilizing power and the solubility of the composition itself in the oral cavity are low, and the clarity immediately after preparation of the preparation and the effect of suppressing the squeeze and dusting during low-temperature storage are poor. Those exceeding 100 mol are not commercially available.
E. of polyoxyethylene alkyl ethers O. When the added mole number is less than 20 moles, the solubilizing power is low, the solubility in the oral composition itself is low, the solubilization of the component (A) and the component (C), and the clarity immediately after preparation of the preparation. In addition, it is inferior in the restraint effect on the orientation and dust during low temperature storage. Those exceeding 40 mol are not commercially available. In addition, when the number of carbon atoms of the alkyl group is less than 16 or more than 18 in the polyoxyethylene alkyl ether, it is inferior in the effect of suppressing the orientation and dust during low temperature storage.
Polyglycerin fatty acid esters whose fatty acids have less than 12 or more than 18 carbons have low solubilizing power, solubilization of components (A) and (C), clarity immediately after preparation and low-temperature storage It is inferior to the restraint effect of orientation and dust.
(B)成分の配合量は、組成物全体の0.1〜1.3%が好ましく、より好ましくは0.2〜1.3%、さらに好ましくは0.2〜1.0%である。配合量が多いほど、(A)成分や(C)成分の可溶化、低温保存時のオリ・にごり発生の抑制にはより好適である。また、調製直後の澄明性を得るにはより好適である。1.3%以下であると、(B)成分由来の味やべたつきが強くなるのを抑え、口に含んだときの違和感を抑えるには好適である。 The blending amount of the component (B) is preferably 0.1 to 1.3% of the entire composition, more preferably 0.2 to 1.3%, and still more preferably 0.2 to 1.0%. The larger the blending amount, the more suitable for solubilization of the component (A) and the component (C) and the suppression of occurrence of dirt and dust during low-temperature storage. Moreover, it is more suitable for obtaining clarity immediately after preparation. When the content is 1.3% or less, it is preferable to suppress an increase in taste and stickiness derived from the component (B) and to suppress a sense of discomfort when included in the mouth.
(C)成分は、イソプロピルメチルフェノール、トリクロサン、チモールから選ばれる芳香族化合物である。(C)成分は、安定化剤として配合されるもので、(B)成分と併用することで、(A)成分を含有する口腔用組成物の低温保存後のオリ・にごり発生及び違和感発現を抑制する効果を奏する。(C)成分の芳香族化合物としては、1種単独でも2種以上を組み合わせて配合してもよいが、特にイソプロピルメチルフェノールが好ましい。 The component (C) is an aromatic compound selected from isopropylmethylphenol, triclosan, and thymol. The component (C) is blended as a stabilizer, and when used in combination with the component (B), the oral composition containing the component (A) generates an odor / dirty occurrence and a sense of discomfort after low-temperature storage. There is an inhibitory effect. As the aromatic compound (C), one kind may be used alone, or two or more kinds may be used in combination, but isopropylmethylphenol is particularly preferred.
(C)成分の配合量は、組成物全体の0.01〜0.12%が好ましく、より好ましくは0.01〜0.1%、さらに好ましくは0.02〜0.07%である。配合量が上記範囲内であると、調製直後の澄明性、低温保存後のオリ・にごり発生の抑制効果がより優れる。また、0.12%以下であると、口に含んだときの苦味や刺激などの違和感を抑えるには好適である。 The amount of component (C) is preferably 0.01 to 0.12%, more preferably 0.01 to 0.1%, and still more preferably 0.02 to 0.07% of the entire composition. When the blending amount is within the above range, the clarity immediately after the preparation and the effect of suppressing the occurrence of dirt and dust after low-temperature storage are more excellent. Moreover, when it is 0.12% or less, it is suitable for suppressing unpleasant feelings such as bitterness and irritation when it is contained in the mouth.
本発明では、(A)成分と(C)成分とを適切比率で配合することが、効果発現、特に低温保存後のオリ・にごり発生を抑制するのに重要である。
(A)、(C)成分の配合比率は、(A)成分/(C)成分が質量比として1〜50であり、特に3〜50が好ましく、3〜30がより好ましい。配合比率が1未満では、製剤調製直後の澄明性が低下し、また、(C)成分自身が不溶化し、低温保存時にオリ・にごりが発生してしまう。50を超えると低温保存時のオリ・にごりの発生を抑制できない。In the present invention, it is important for the component (A) and the component (C) to be blended at an appropriate ratio in order to suppress the occurrence of effects, particularly the occurrence of orientation and dirt after low-temperature storage.
The blending ratio of the components (A) and (C) is such that the component (A) / component (C) is 1 to 50, particularly 3 to 50, and more preferably 3 to 30. If the blending ratio is less than 1, the clarity immediately after preparation of the preparation is lowered, and the component (C) itself is insolubilized, resulting in the occurrence of orientation and dirt during low-temperature storage. If it exceeds 50, it will not be possible to suppress the occurrence of orientation and dust during low temperature storage.
本発明では、更に(D)アルキル硫酸ナトリウムを配合することが好ましい。アルキル硫酸ナトリウムは安定化剤として作用し、配合により低温保存後のオリ・にごり発生を抑制する効果をより高めることができる。なお、アルキル硫酸ナトリウム以外のアニオン性界面活性剤の添加では、オリ・にごりが抑制されずむしろ発生してしまうもので、かかる効果の向上は、アルキル硫酸ナトリウムの特異的な作用によるものと推測される。
(D)成分としては、アルキル基の炭素数が8〜18、特に10〜16のものが好ましく、とりわけラウリル硫酸ナトリウムが好ましい。In the present invention, it is preferable to further blend (D) sodium alkyl sulfate. Sodium alkyl sulfate acts as a stabilizer, and can improve the effect of suppressing the occurrence of dirt and dust after low-temperature storage by blending. In addition, the addition of an anionic surfactant other than sodium alkylsulfate will cause the occurrence of odor and dust, rather than being suppressed, and this improvement in the effect is presumed to be due to the specific action of sodium alkylsulfate. The
As the component (D), an alkyl group having 8 to 18 carbon atoms, particularly 10 to 16 carbon atoms is preferable, and sodium lauryl sulfate is particularly preferable.
(D)成分を配合する場合、その配合量は、組成物全体の0.05〜1.0%が好ましく、より好ましくは0.1〜0.5%である。上記範囲内で配合すると、低温保存後のオリ・にごり発生の抑制力をより向上できる。また、1.0%以下であると、口に含んだときに苦味や刺激などの違和感を与え難いので好適である。 (D) When mix | blending a component, the compounding quantity has preferable 0.05-1.0% of the whole composition, More preferably, it is 0.1-0.5%. When blended within the above range, it is possible to further improve the ability to suppress the occurrence of orientation and dirt after low-temperature storage. Moreover, when it is 1.0% or less, it is difficult to give an uncomfortable feeling such as bitterness or irritation when it is contained in the mouth.
また、本発明では、組成物中の界面活性剤総量が適切量であることが、低温保存後のオリ・にごり発生を抑制し、また違和感を抑える点でより望ましく、(D)成分を配合する場合は、(B)及び(D)成分の総量が好ましくは0.1〜1.3%、より好ましくは0.2〜1.3%、さらに好ましくは0.2〜1.0%となる範囲内での添加が望ましい。総量が上記範囲内であると、(A)成分や(C)成分の可溶化、低温保存時のオリ・にごりの抑制効果がより優れる。また、1.3%以下であると、これら成分由来の味やべたつきを抑え、口に含んだときの違和感を抑えるには好適である。 In the present invention, it is more preferable that the total amount of the surfactant in the composition is an appropriate amount in terms of suppressing the occurrence of orientation and dirt after low-temperature storage, and also suppressing the uncomfortable feeling, and the component (D) is blended. In this case, the total amount of the components (B) and (D) is preferably 0.1 to 1.3%, more preferably 0.2 to 1.3%, and still more preferably 0.2 to 1.0%. Addition within the range is desirable. When the total amount is within the above range, the effects of solubilization of the component (A) and the component (C) and the restraint of dirt and dust during low-temperature storage are more excellent. Moreover, when it is 1.3% or less, it is suitable for suppressing the taste and stickiness derived from these components, and suppressing the uncomfortable feeling when included in the mouth.
組成物のpH(25℃)は6.5〜8.0であり、好ましくは7.0〜7.8である。pHが6.5未満では(A)成分の分解が促進されて低温保存時にオリ・にごりが発生しやすくなり、pHが8.0を超えた組成ではオリ・にごりを抑制できず、いずれの場合も(B)、(C)成分を配合してもオリ・にごりの発生を抑えることができない。また、pHが8.0を超えると口に含んだときにヌルつきや異味などの違和感が大きくなる。
なお、組成物のpHは、なりゆきで6.5〜8.0になるときもあるが、必要に応じてpH調整剤を用いて上記範囲内に調製してもよい。pH調整剤としては、水酸化ナトリウム、塩酸、炭酸ナトリウム、炭酸水素ナトリウム、ホウ酸又はその塩等のpH調整剤を使用でき、中でも水酸化ナトリウム、水酸化カリウム、塩酸が好適に用いられる。これらpH調整剤の配合量は、pHを上記範囲に調整できればよい。The pH (25 ° C.) of the composition is 6.5 to 8.0, preferably 7.0 to 7.8. If the pH is less than 6.5, the decomposition of the component (A) is promoted, so that it becomes easy to generate dirt and dust when stored at low temperatures, and if the composition has a pH exceeding 8.0, it cannot be suppressed. Even if (B) and (C) component are mix | blended, generation | occurrence | production of orientation and dust cannot be suppressed. Moreover, when pH exceeds 8.0, when it is included in the mouth, a sense of incongruity such as nulliness or a nasty taste increases.
In addition, although the pH of a composition may become 6.5-8.0 in some ways, you may adjust in the said range using a pH adjuster as needed. As the pH adjusting agent, a pH adjusting agent such as sodium hydroxide, hydrochloric acid, sodium carbonate, sodium hydrogen carbonate, boric acid or a salt thereof can be used, and among them, sodium hydroxide, potassium hydroxide and hydrochloric acid are preferably used. The blending amount of these pH adjusters only needs to be able to adjust the pH to the above range.
本発明組成物は、特に液体口腔用組成物として好適に調製され、具体的には液体歯磨、洗口剤等の液体製剤として好適に調製できる。なお、ここで液体口腔用組成物とは、配合成分が可溶化した透明又は半透明な製剤で、研磨剤などの可溶化しない固形成分は通常配合されない。 The composition of the present invention is particularly suitably prepared as a liquid oral composition, and specifically can be suitably prepared as a liquid formulation such as liquid dentifrice and mouthwash. Here, the liquid oral composition is a transparent or translucent preparation in which a compounding component is solubilized, and a solid component that is not solubilized such as an abrasive is generally not compounded.
また、本発明の口腔用組成物には、上記成分に加えて、本発明の効果を損なわない範囲でその剤型等に応じた適宜な公知の任意成分を配合することができる。任意成分として、液体口腔用組成物には、例えば溶剤、湿潤剤、増粘剤、界面活性剤、更に必要により防腐剤、甘味剤、香料、着色料、有効成分等が配合できる。 Moreover, in addition to the said component, the well-known arbitrary component according to the dosage form etc. can be mix | blended with the composition for oral cavity of this invention in the range which does not impair the effect of this invention. As an optional component, for example, a solvent, a wetting agent, a thickening agent, a surfactant, and, if necessary, a preservative, a sweetening agent, a fragrance, a coloring agent, an active ingredient, and the like can be added to the liquid oral composition.
溶剤としては、一般的に精製水が用いられる。また、プロピレングリコールや、エタノール等の炭素数2〜4の低級一価アルコールを配合することができるが、これらの溶剤の配合量は、通常、組成物全体の0〜30%であり、特に2〜20%が好ましい。
なお、本発明の口腔用組成物では、エタノールを実質的に含有しない(即ち、組成物中のエタノール含有量が0.01%以下、特に0〜0.0001%である)組成であっても、本発明の効果を得ることができる。As the solvent, purified water is generally used. Moreover, although C2-C4 lower monohydric alcohols, such as propylene glycol and ethanol, can be mix | blended, normally the compounding quantity of these solvents is 0-30% of the whole composition, and especially 2 ~ 20% is preferred.
In addition, even if the composition for oral cavity of this invention is a composition which does not contain ethanol substantially (namely, ethanol content in a composition is 0.01% or less, especially 0-0.0001%). The effects of the present invention can be obtained.
湿潤剤としては、ソルビトール、キシリトール、エリスリトール等の糖アルコール、グリセリン、エチレングリコール、ポリエチレングリコール等の多価アルコールが挙げられる。配合量は通常、組成物全体の0〜20%である。 Examples of the wetting agent include sugar alcohols such as sorbitol, xylitol, and erythritol, and polyhydric alcohols such as glycerin, ethylene glycol, and polyethylene glycol. A compounding quantity is 0 to 20% of the whole composition normally.
界面活性剤としては、本発明の効果を妨げない範囲で、(B)成分及び(D)成分以外の界面活性剤を配合してもよい。例えばラウロイルメチルタウリン、アシルアミノ酸塩、ドデシルベンゼンスルホン酸ナトリウム、α−スルホ脂肪酸アルキルエステル・ナトリウム、アルキルリン酸エステル塩等のアニオン性界面活性剤、アルキルジメチルアミノ酢酸ベタイン、脂肪酸アミドプロピルジメチルアミノ酢酸ベタインなどの酢酸ベタイン型両性界面活性剤、N−脂肪酸アシル−N−カルボキシメチル−N−ヒドロキシエチルエチレンジアミン塩などのイミダゾリン型両性界面活性剤、N−脂肪酸アシル−L−アルギネート塩等のアミノ酸型両性界面活性剤、ショ糖脂肪酸エステル、ソルビタン脂肪酸エステル、ポリオキシエチレンポリオキシプロピレンブロックコポリマー型ノニオン性界面活性剤、ポリオキシエチレン脂肪酸エステル、脂肪酸モノグリセライドなどが挙げられる。
なお、これら界面活性剤を配合する場合は、(B)成分、更には(D)成分を含めた界面活性剤の総量が0.1〜1.3%、特に0.2〜1.3%、とりわけ0.2〜1.0%となる範囲内で添加することが望ましい。As the surfactant, a surfactant other than the component (B) and the component (D) may be blended as long as the effects of the present invention are not hindered. For example, anionic surfactants such as lauroylmethyl taurine, acylamino acid salt, sodium dodecylbenzenesulfonate, α-sulfo fatty acid alkyl ester sodium, alkyl phosphate ester salt, alkyldimethylaminoacetic acid betaine, fatty acid amidopropyldimethylaminoacetic acid betaine Amino acid-type amphoteric surfactants such as betaine acetate-type amphoteric surfactants such as N-fatty acid acyl-N-carboxymethyl-N-hydroxyethylethylenediamine salts and imidazoline-type amphoteric surfactants such as N-fatty acid acyl-L-alginate salts Activator, sucrose fatty acid ester, sorbitan fatty acid ester, polyoxyethylene polyoxypropylene block copolymer type nonionic surfactant, polyoxyethylene fatty acid ester, fatty acid monoglyceride Etc., and the like.
When these surfactants are blended, the total amount of the surfactant including the component (B) and further the component (D) is 0.1 to 1.3%, particularly 0.2 to 1.3%. In particular, it is desirable to add in the range of 0.2 to 1.0%.
増粘剤としては、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等が挙げられる。増粘剤の配合量は通常0〜5%である。 Examples of the thickener include sodium carboxymethyl cellulose and hydroxyethyl cellulose. The blending amount of the thickener is usually 0 to 5%.
防腐剤としては、安息香酸ナトリウム等の安息香酸塩、ソルビン酸カリウム等が挙げられる。甘味剤としては、サッカリン、サッカリンナトリウム、ステビオサイト、スクラロース、アスパルテーム等が挙げられる。
香料としては、スペアミント油、ハッカ油等の天然香料、及びカルボン、アネトール等の単品香料、更に単品香料及び/又は天然香料も含む調合香料等の口腔衛生品に用いられる周知の香料を使用することができる。その配合量は通常、0.00001〜1%の範囲である。
着色料としては、青色1号、緑色3号、黄色4号、赤色105号など安全性の高い水溶性色素が挙げられる。Examples of the preservative include benzoates such as sodium benzoate, potassium sorbate and the like. Examples of the sweetener include saccharin, saccharin sodium, steviosite, sucralose, aspartame and the like.
As perfumes, natural perfumes such as spearmint oil and mint oil, and single perfumes such as carvone and anethole, as well as well-known perfumes used in oral hygiene products such as single perfumes and / or blended perfumes including natural perfumes are used. Can do. The blending amount is usually in the range of 0.00001 to 1%.
Examples of the coloring agent include highly safe water-soluble pigments such as Blue No. 1, Green No. 3, Yellow No. 4, and Red No. 105.
有効成分としては、アスコルビン酸リン酸エステル及びその塩、イソプロピルメチルフェノール、トリクロサン並びにチモール以外の公知成分、例えば抗炎症剤、酵素、フッ化物、殺菌剤などを、本発明の効果を妨げない範囲で有効量配合してもよい。 As active ingredients, ascorbic acid phosphates and salts thereof, isopropylmethylphenol, triclosan, and known ingredients other than thymol, such as anti-inflammatory agents, enzymes, fluorides, bactericides, and the like, in a range that does not interfere with the effects of the present invention. An effective amount may be blended.
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。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。
また、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において括弧内の数値はエチレンオキサイドの平均付加モル数を示す。なお、表中のPOEはポリオキシエチレンの略記である。pHは、組成物を調製直後に東亜電波工業社製のpHメーター(型番Hm−30S)を用いて測定し、25℃、3分後の値を示した。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 the following examples,% indicates mass% unless otherwise specified.
In the polyoxyethylene hydrogenated castor oil and polyoxyethylene alkyl ether, the numerical value in parentheses indicates the average number of moles of ethylene oxide added. In the table, POE is an abbreviation for polyoxyethylene. The pH was measured immediately after preparation using a pH meter (model number Hm-30S) manufactured by Toa Denpa Kogyo Co., Ltd., and showed a value after 3 minutes at 25 ° C.
[実施例、比較例]
表1〜3に示す組成の液体口腔用組成物を下記方法で調製した。得られた液体口腔用組成物について、下記方法で評価した。また、表4に示す組成の液体口腔用組成物を同様に調製し、製剤調製直後の澄明性、オリ・にごり抑制効果を同様に評価した。結果を表1〜4に併記した。[Examples and Comparative Examples]
Liquid oral compositions having the compositions shown in Tables 1 to 3 were prepared by the following method. The obtained liquid oral composition was evaluated by the following methods. Moreover, the liquid oral cavity composition of the composition shown in Table 4 was similarly prepared, and the clarity immediately after preparation preparation and the effect of suppressing scumming were evaluated in the same manner. The results are shown in Tables 1-4.
液体口腔用組成物の調製方法
液体口腔用組成物の調製は、表中の組成に応じ、精製水中に水溶性原料を溶解した後、湿潤剤や溶剤を配合する場合には湿潤剤や溶剤に油溶性原料と非イオン性界面活性剤を溶解した液を、攪拌しながら加え、均一に溶解させた。なお、製造にはスリーワンモーター(BL1200、HEIDON社製)を用いた。Preparation method of liquid oral composition The liquid oral composition is prepared by dissolving the water-soluble raw material in purified water according to the composition in the table and then adding the wetting agent or solvent to the wetting agent or solvent. A solution in which the oil-soluble raw material and the nonionic surfactant were dissolved was added with stirring to be uniformly dissolved. A three-one motor (BL1200, manufactured by HEIDON) was used for manufacturing.
製剤調製直後の澄明性試験
調製直後の組成物を満注量250mLの無色透明なPET容器に250mL充填し、精製水を充填したPET容器(対照品)と比較して下記基準に従い目視判定した。
調製直後の澄明性の評価基準
◎:にごりが全く認められない
○:にごりが僅かに認められるが、対照品がなければ判別できないレベ
ルであり問題ない
△:にごりが明らかに認められ、対照品がなくてもややにごりが認めら
れる
×:対照品と比較しなくても明らかににごりが認められ、PET容器の
向こう側を透かし見るのが困難な程にごっているClarity test immediately after preparation of preparation The composition immediately after preparation was filled in 250 mL of a colorless and transparent PET container having a full injection amount of 250 mL, and compared with a PET container (control product) filled with purified water, and visually judged according to the following criteria.
Evaluation criteria for clarity immediately after preparation ◎: No dust is observed ○: Slight dust is observed, but there is no problem because there is no control product △: Scratch is clearly recognized and control product Slight dust is observed even if there is no X ×: Slightly dust is observed without comparison with the control product, and it is difficult to see through the PET container.
オリ・にごり抑制効果の評価
組成物を満注量250mLのPET容器に250mL充填し、−10℃で1ヶ月保存後に室温に戻し、PET容器の外観としてのにごり状態や、緩やかに転置した際のオリについて、精製水を充填したPET容器(対照品)と比較して下記基準に従い目視判定した。B以上を合格とした。
オリ・にごり抑制効果の評価基準
A−1:オリ・にごりが全くない
A−2:オリ・にごりが殆ど認められない
B:単独での判定ではオリ・にごりが殆どわからず、対照品と比べては
じめてオリ・にごりが認識されるが、問題のないレベルである
C:対照品がなくても単独での判定でオリ・にごりがやや認められる
D:単独での判定でオリ・にごりが明らかに認められる
E:単独での判定でオリ・にごりがかなり認められるEvaluation of Ori-Nigori Suppression Effect 250 mL of the composition was filled in a 250 mL PET container, stored at −10 ° C. for 1 month, returned to room temperature, and when the PET container was in a dirty state or gently displaced The orientation was visually determined according to the following criteria in comparison with a PET container (control product) filled with purified water. B or higher was accepted.
Evaluation criteria for the effect of restraint against dirt and dust A-1: No dirt or dust is observed. A-2: Almost no dirt or dust is observed. At first, the orientation is recognized, but there is no problem. C: Even if there is no reference product, the orientation is slightly recognized by the judgment alone. D: The orientation is judged by the judgment alone. Clearly recognized E: Significant odor and dust are recognized by independent judgment
口に含んだときの違和感のなさの評価
口腔粘膜が過敏な10名の被験者が、調製直後の組成物約10mLを口に含み、20秒間程すすいでいる間に口腔内で感じる違和感について評価した。対照品(実施例1と同組成で、組成物のpHを、pH調整剤の水酸化ナトリウムでpH9に調整した組成)を2点として以下の基準に従って官能評価した。平均値を求めて下記基準で判定した。
口に含んだときの違和感のなさの評価基準
4:違和感がなかった
3:違和感が殆どなかった
2:対照品と同等な違和感があった
1:対照品よりも強い顕著な違和感を感じた
判定基準
◎:3.5点以上
○:3.0点以上3.5点未満
△:2.0点以上3.0点未満
×:2.0点未満Evaluation of no discomfort when in the mouth Ten subjects with sensitive oral mucosa evaluated the discomfort felt in the mouth while rinsing for about 20 seconds containing about 10 mL of the composition immediately after preparation. . Sensory evaluation was carried out according to the following criteria, with two control products (compositions having the same composition as in Example 1 and the pH of the composition adjusted to pH 9 with sodium hydroxide as a pH adjusting agent). The average value was obtained and judged according to the following criteria.
Evaluation Criteria for No Discomfort When Ingested 4: No Discomfort 3: Little Discomfort 2: Discomfort Equivalent to Control 1: Feeling Conspicuous Discomfort Stronger than Control Standard ◎: 3.5 points or more ○: 3.0 points or more and less than 3.5 points △: 2.0 points or more and less than 3.0 points ×: Less than 2.0 points
使用原料の詳細は下記の通りである。
アスコルビン酸リン酸エステルマグネシウム:和光純薬工業社製、リン酸−L−アスコルビルマグネシウム、生化学用
アスコルビン酸リン酸エステルナトリウム:DSMニュートリションジャパン社製、ステイC50
ポリオキシエチレン(40)硬化ヒマシ油:
日光ケミカルズ社製、NIKKOL HCO−40
ポリオキシエチレン(60)硬化ヒマシ油:
日光ケミカルズ社製、NIKKOL HCO−60
ポリオキシエチレン(100)硬化ヒマシ油:
日本エマルジョン社製、NIKKOL HCO−100
ポリオキシエチレン(20)セチルエーテル:
日光ケミカルズ社製、NIKKOL BC−20
ポリオキシエチレン(20)ステアリルエーテル:
日光ケミカルズ社製、NIKKOL BS−20
ポリオキシエチレン(40)セチルエーテル:
日光ケミカルズ社製、NIKKOL BC−40
モノラウリン酸ポリグリセリル:
日光ケミカルズ社製、NIKKOL Decaglyn 1−L
モノミリスチン酸デカグリセリル:
日光ケミカルズ社製、NIKKOL Decaglyn 1−M
イソプロピルメチルフェノール:大阪化成社製
トリクロサン:チバ・ジャパン社製
チモール:大阪化成社製
ラウリル硫酸ナトリウム:東邦化学工業社製
水酸化ナトリウム:関東化学社製、特級
塩酸:関東化学社製、特級
ポリオキシエチレン(5)硬化ヒマシ油:
日光ケミカルズ社製、NIKKOL HCO−5
ポリオキシエチレン(20)硬化ヒマシ油:
日光ケミカルズ社製、NIKKOL HCO−20
dl−α−トコフェロール:和光純薬工業社製
フェノール:和光純薬工業社製
サリチル酸メチル:和光純薬工業社製、和光一級
塩化ベンゼトニウム:関東化学社製Details of the raw materials used are as follows.
Ascorbic acid phosphate magnesium: manufactured by Wako Pure Chemical Industries, Ltd., phosphoric acid-L-ascorbyl magnesium, biochemical ascorbic acid sodium phosphate ester: manufactured by DSM Nutrition Japan, Stay C50
Polyoxyethylene (40) hydrogenated castor oil:
NIKKOL HCO-40, manufactured by Nikko Chemicals
Polyoxyethylene (60) hydrogenated castor oil:
NIKKOL HCO-60, manufactured by Nikko Chemicals
Polyoxyethylene (100) hydrogenated castor oil:
NIKKOL HCO-100, manufactured by Nippon Emulsion Co., Ltd.
Polyoxyethylene (20) cetyl ether:
NIKKOL BC-20 manufactured by Nikko Chemicals
Polyoxyethylene (20) stearyl ether:
NIKKOL BS-20, manufactured by Nikko Chemicals
Polyoxyethylene (40) cetyl ether:
NIKKOL BC-40, manufactured by Nikko Chemicals
Polyglyceryl monolaurate:
NIKKOL Decaglyn 1-L, manufactured by Nikko Chemicals
Decaglyceryl monomyristate:
NIKKOL Decaglyn 1-M, manufactured by Nikko Chemicals
Isopropylmethylphenol: Osaka Chemical Co., Ltd. Triclosan: Ciba Japan Co., Ltd. Timor: Osaka Kasei Co., Ltd. sodium lauryl sulfate: Toho Chemical Industry Co., Ltd. Sodium hydroxide: Kanto Chemical Co., Ltd. Ethylene (5) hydrogenated castor oil:
NIKKOL HCO-5, manufactured by Nikko Chemicals
Polyoxyethylene (20) hydrogenated castor oil:
NIKKOL HCO-20, manufactured by Nikko Chemicals
dl-α-tocopherol: manufactured by Wako Pure Chemical Industries, Ltd. phenol: manufactured by Wako Pure Chemical Industries, Ltd. methyl salicylate: manufactured by Wako Pure Chemical Industries, Ltd., Wako primary benzethonium chloride: manufactured by Kanto Chemical Co., Inc.
表3の結果から、(B)又は(C)成分を欠いたり、非イオン性界面活性剤又は芳香族化合物が不適切な場合(比較例1〜8)は、オリ・にごり発生を抑制できなかった。(B)、(C)成分が配合されていても、(A)、(C)成分の配合比率が不適切な場合(比較例9、10)はオリ・にごり発生を抑制できず、また、pHが特定範囲外の組成ではオリ・にごり発生を抑えることはできなかった(比較例11、12)。これらに対して、(A)、(B)、(C)成分を含有し、(A)/(C)比、pHが適切な液体口腔用組成物(表1、2の実施例)は、製剤調製直後の澄明性、−10℃で1ヶ月保存時のオリ・にごり発生の抑制効果、違和感のなさに優れ、特に製剤を単独で目視し判定したのではわからず対照品と比べて初めて認識できるようなオリ・にごりの発生を抑え、澄明性を調製直後から長期に亘って維持できることが確認された。また、表4に示すとおり、更に(D)成分を配合すると、オリ・にごり発生の抑制効果が向上することが確認された。 From the results shown in Table 3, when the component (B) or (C) is missing or the nonionic surfactant or the aromatic compound is inappropriate (Comparative Examples 1 to 8), it is not possible to suppress the occurrence of dirt and dust. It was. Even if the components (B) and (C) are blended, if the blending ratio of the components (A) and (C) is inappropriate (Comparative Examples 9 and 10), it is not possible to suppress the occurrence of clogging. When the composition had a pH outside the specific range, the occurrence of orientation and dust could not be suppressed (Comparative Examples 11 and 12). In contrast, (A), (B), (C) component, (A) / (C) ratio, liquid oral composition (Examples in Tables 1 and 2) with appropriate pH are as follows: Clarity immediately after preparation, excellent curbing effect when stored at -10 ° C for 1 month, and uncomfortable feeling. It was confirmed that the occurrence of orientation and dust could be suppressed, and the clarity could be maintained for a long time immediately after preparation. Further, as shown in Table 4, it was confirmed that when the component (D) was further blended, the effect of suppressing the occurrence of dirt and dust was improved.
Claims (7)
(B)エチレンオキサイドの平均付加モル数が40〜100モルのポリオキシエチレン硬化ヒマシ油、アルキル基の炭素数が16〜18でエチレンオキサイドの平均付加モル数が20〜40モルのポリオキシエチレンアルキルエーテル及び脂肪酸の炭素数が12〜18の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種以上の非イオン性界面活性剤を0.2〜1.0質量%と、
(C)イソプロピルメチルフェノール、トリクロサン及びチモールから選ばれる1種又は2種以上の芳香族化合物を0.02〜0.07質量%と
を含有してなり、(A)成分と(C)成分の配合比率(A)/(C)が質量比として3〜30であり、かつ25℃の時のpHが6.5〜7.8であることを特徴とする液体口腔用組成物。 (A) A liquid oral composition ascorbic acid phosphate ester magnesium salt containing 0.1 to 2 wt%,
(B) Polyoxyethylene hydrogenated castor oil having an average addition mole number of ethylene oxide of 40 to 100 moles, polyoxyethylene alkyl having an alkyl group of 16 to 18 carbon atoms and an average addition mole number of ethylene oxide of 20 to 40 moles 0.2 to 1.0% by mass of one or more nonionic surfactants selected from ether and fatty acid esters having 12 to 18 carbon atoms of fatty acid,
(C) One or two or more aromatic compounds selected from isopropylmethylphenol, triclosan, and thymol are contained in an amount of 0.02 to 0.07% by mass, and the components (A) and (C) A composition for liquid oral cavity, wherein the blending ratio (A) / (C) is 3 to 30 as a mass ratio, and the pH at 25 ° C. is 6.5 to 7.8 .
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