WO2016133063A1 - Oral liquid composition - Google Patents

Oral liquid composition Download PDF

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Publication number
WO2016133063A1
WO2016133063A1 PCT/JP2016/054370 JP2016054370W WO2016133063A1 WO 2016133063 A1 WO2016133063 A1 WO 2016133063A1 JP 2016054370 W JP2016054370 W JP 2016054370W WO 2016133063 A1 WO2016133063 A1 WO 2016133063A1
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Prior art keywords
liquid oral
oral composition
potassium nitrate
mass
composition
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PCT/JP2016/054370
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French (fr)
Japanese (ja)
Inventor
友美子 平嶋
赤羽 康宏
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ライオン株式会社
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Priority to CN201680010823.XA priority Critical patent/CN107249546B/en
Priority to KR1020177021898A priority patent/KR102491340B1/en
Priority to MYPI2017702777A priority patent/MY183114A/en
Publication of WO2016133063A1 publication Critical patent/WO2016133063A1/en

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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/40Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/44Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/49Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/86Polyethers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses

Definitions

  • the present invention relates to a liquid oral composition containing no potassium nitrate and containing no ethanol, which is excellent in hypersensitivity suppression effect and bactericidal effect in the oral cavity.
  • Patent Documents 1 and 2 As a preventive measure against dentin hypersensitivity, known potassium nitrate is blended into the oral composition as an active ingredient (Patent Documents 1 and 2). This potassium nitrate has a problem that an insoluble precipitate is formed in the presence of sodium lauryl sulfate which is generally blended in an oral composition.
  • Patent Document 3 there are many oral compositions containing potassium nitrate and sodium lauryl sulfate. By adding a monohydric alcohol and an amphoteric surfactant, precipitation of potassium lauryl sulfate is prevented and low temperature precipitation is suppressed.
  • non-alcohol type liquid preparations with less mucosal irritation and low irritation are more suitable for suppressing hypersensitivity particularly in liquid oral compositions.
  • cetylpyridinium chloride a cationic fungicide
  • cetylpyridinium chloride has an excellent bactericidal effect on airborne bacteria in the oral cavity and is effective in preventing or suppressing oral diseases such as caries, but is easily affected by a surfactant.
  • Patent Document 4 a specific compound is added to an oral composition containing a biguanide-based cationic fungicide and a nonionic surfactant to prevent deactivation of the cationic fungicide by the nonionic surfactant. Then, a stabilized blending technique has been proposed.
  • non-alcohol type liquid oral preparation containing potassium nitrate can suppress hypersensitivity and at the same time exert high bactericidal power against oral floating bacteria, it is more effective for prevention or suppression of oral diseases.
  • the current situation is that it is difficult with conventional techniques, and the development of liquid oral preparations having such excellent characteristics has been desired.
  • the present invention has been made in view of the above circumstances, and an object of the present invention is to provide an ethanol-free liquid oral composition containing potassium nitrate, which is excellent in the hypersensitivity suppressing effect and the bactericidal effect of airborne bacteria in the oral cavity.
  • the present inventors have found that (A) potassium nitrate and (B) cetylpyridinium chloride are combined with an ethanol-free liquid oral composition, and (C) nonionic By blending a surfactant and (D) an amphoteric surfactant, (E) the water content is 55% by mass or more and less than 92% by mass, and the pH of the composition is 6.8 or more and less than 8.0 by ( A), non-alcohol-type liquid oral composition is obtained, in which precipitation of insoluble precipitates generated by the combined use of components (B) is suppressed, and the perceptual hypersensitivity suppressing effect and the bactericidal effect of airborne bacteria in the oral cavity are excellent.
  • the present inventors have found that it can be suitably used for caries suppression and have made the present invention.
  • potassium nitrate-containing cetyl chloride and potassium nitrate and cetyl chloride were expected to be added to the liquid oral composition containing potassium nitrate by adding cetylpyridinium chloride, a cationic fungicide, to prevent hypersensitivity and bactericidal bacteria.
  • cetylpyridinium chloride a cationic fungicide
  • the liquid oral composition of the present invention containing no ethanol shows almost no insoluble precipitate even after 4 weeks have passed since the preparation of the liquid oral composition. Appearance is stable over time, high sensitivity to hypersensitivity and bactericidal effect on airborne bacteria in the oral cavity, and bitterness after use is suppressed, resulting in a good feeling of good use.
  • Patent Document 3 suppresses precipitation of potassium lauryl sulfate caused by the combined use of potassium nitrate and sodium lauryl sulfate in the oral composition
  • Patent Document 4 describes a cationic bactericide using a nonionic surfactant. No mention is made of using a cationic bactericide in combination with potassium nitrate.
  • Patent Documents 5 and 6 describe liquid oral compositions containing potassium nitrate and cetylpyridinium chloride, but these are ethanol-containing compositions. From Patent Documents 3 to 6, the suppression of precipitation of insoluble precipitates caused by the combined use of potassium nitrate and cetylpyridinium chloride in a liquid oral composition containing no ethanol cannot be predicted.
  • the present invention provides the following liquid oral composition and a method for suppressing the precipitation of insoluble precipitates in the composition.
  • the nonionic surfactant is polyoxyethylene hydrogenated castor oil having an average addition mole number of ethylene oxide of 40 to 100 mol
  • the amphoteric surfactant is coconut oil fatty acid amidopropyl betaine [ 1] or [2] liquid oral composition.
  • [5] The liquid oral composition according to any one of [1] to [4], wherein 0.01 to 10% by mass of component (A) and 0.001 to 0.1% by mass of component (B) are blended.
  • [6] The liquid oral composition according to any one of [1] to [5], which is a mouthwash.
  • [7] The liquid oral composition according to any one of [1] to [6], which is used for suppressing hypersensitivity and caries.
  • [8] (A) A non-ethanol-containing liquid oral composition containing potassium nitrate and (B) cetylpyridinium chloride, (C) a nonionic surfactant and (D) an amphoteric surfactant, and (E) water content 55% by mass or more and less than 92% by mass, and the pH of the composition is 6.8 or more and less than 8.0, wherein (A) potassium nitrate and (B) cetylpyridinium chloride in the liquid oral composition A method for suppressing the precipitation of insoluble precipitates produced by the combined use.
  • liquid oral composition containing no potassium nitrate and containing no ethanol, which is excellent in the effect of suppressing hypersensitivity and the bactericidal effect of floating bacteria in the oral cavity.
  • composition for liquid oral cavity of the present invention contains (A) potassium nitrate, (B) cetylpyridinium chloride, (C) nonionic surfactant, (D) amphoteric surfactant, (E) water, and contains no ethanol It is.
  • (A) Potassium nitrate is blended as an active ingredient for preventing or treating dentin hypersensitivity, and is a hypersensitivity inhibitor.
  • the blending amount of the component (A) potassium nitrate is preferably 0.01 to 10% (mass%, hereinafter the same) of the whole composition, more preferably 0.1 to 7%. As the blending amount increases, the perceptual hypersensitivity suppression effect increases, but 10% or less is more suitable for sufficient precipitation suppression and bitterness suppression.
  • Cetylpyridinium chloride is a cationic bactericidal agent and a bactericidal agent against floating bacteria in the oral cavity.
  • a commercially available cetylpyridinium chloride can be used.
  • the amount of component (B) cetylpyridinium chloride is preferably 0.001 to 0.1%, more preferably 0.005 to 0.1%, still more preferably 0.01 to 0.05% of the total composition. %. The more the compound is added, the higher the bactericidal effect, but 0.1% or less is more suitable for sufficient precipitation suppression and bitterness suppression.
  • Examples of (C) nonionic surfactants include polyoxyethylene hydrogenated castor oil, polyoxyethylene alkyl ether, and polyglycerin fatty acid ester, and one or more of these may be used.
  • (E.O.) polyoxyethylene hydrogenated castor oil having an average added mole number of 40 to 100 moles, particularly 60 to 100 moles, and an alkyl group having 16 to 18 carbon atoms.
  • O. Preferred are polyoxyethylene alkyl ethers having an average addition mole number of 10 to 40 moles, particularly 20 to 40 moles, and decaglycerin monofatty acid esters polyglycerin fatty acid esters having a fatty acid number of 12 to 18, particularly 12 to 14, among others.
  • E. O. Polyoxyethylene hydrogenated castor oil having an average added mole number of 40 to 100 moles is preferred.
  • the blending amount of the nonionic surfactant as the component (C) is preferably 0.1 to 2% of the total composition, more preferably 0.1 to 1%, still more preferably 0.2 to 0.5%. is there.
  • 0.1% or more is blended, a sufficient precipitation suppressing effect, a hypersensitivity suppressing effect and a floating bacteria sterilizing effect are exhibited, and the bitterness can be sufficiently suppressed.
  • 2% or less is more suitable for preventing the perceptual hypersensitivity suppressing effect and the floating bacteria bactericidal effect from decreasing.
  • Amphoteric surfactants include alkylamidobetaines such as coconut oil fatty acid amidopropylbetaine or salts thereof, betaine acetates such as lauryldimethylaminoacetic acid betaine, N-fatty acid acyl-N-carboxymethyl-N-hydroxyethyl Examples include imidazoline type such as ethylenediamine salt, amino acid type such as N-fatty acid acyl-L-alginate salt, and the like, and one or more of these may be used, and alkylamide betaine or a salt thereof is particularly preferable. Among these, coconut oil fatty acid amidopropyl betaine is preferable.
  • TEGO Betaine CK OK (30% aqueous solution) manufactured by Degussa Co., Ltd.
  • Amphitol 55AB (30% aqueous solution) manufactured by Kao Corporation
  • the blending amount of the amphoteric surfactant as component (D) is preferably 0.1 to 2% of the total composition, more preferably 0.1 to 1%, and still more preferably 0.2 to 0.5%. .
  • a sufficient precipitation suppressing effect, a hypersensitivity suppressing effect and a floating bacteria sterilizing effect are exhibited, and the bitterness can be sufficiently suppressed.
  • 2% or less is more suitable for preventing the perceptual hypersensitivity suppressing effect and the floating bacteria bactericidal effect from decreasing.
  • the water content that is, the water content in the composition is 55% or more and less than 92% of the whole composition, preferably 60% or more and 91% or less. Preferably they are 60% or more and 70% or less.
  • the amount of water is within the above range, insoluble precipitates can be prevented from being precipitated, and excellent perceptual hypersensitivity suppressing effects and bitterness suppressing effects can be imparted. If it is less than 55%, the precipitation cannot be suppressed, and the perceptual hypersensitivity suppressing effect and the floating bacteria sterilizing effect are inferior. When it is 92% or more, the precipitation suppressing effect is inferior, the perceptual hypersensitivity suppressing effect and the floating bacteria sterilizing effect are also inferior, and the bitterness cannot be suppressed.
  • the liquid oral composition has a pH of 6.8 or more and less than 8.0, preferably pH 6.8 to 7.8, more preferably pH 6.8 to 7.5.
  • the precipitation suppression effect, the hypersensitivity suppression effect and the bitterness suppression effect are excellent.
  • the pH is less than 6.8 or pH 8.0 or more, the precipitation cannot be suppressed, and the perceptual hypersensitivity suppressing effect and the floating bacteria sterilizing effect are inferior.
  • the pH was measured immediately after preparation using a pH meter (model number Hm-30S) manufactured by Toa Denpa Kogyo Co., Ltd., and the value after 3 minutes at 25 ° C. (the same applies hereinafter).
  • a known pH adjusting agent may be added to adjust the pH of the composition within the above range.
  • examples thereof include alkali metal hydrogen phosphates such as sodium dihydrogen phosphate and alkali metal hydroxides such as sodium hydroxide.
  • the liquid oral cavity composition of the present invention contains no ethanol.
  • “ethanol-free formulation” is one in which ethanol is not blended, but in liquid oral compositions, there are cases where a small amount of ethanol derived from the raw material is contained in the fragrance blended in the composition. In consideration of these reasons, ethanol is not included in addition to ethanol contained in a trace amount in a fragrance.
  • the amount of ethanol in the composition is preferably 100 ppm or less, more preferably 50 ppm or less, still more preferably 10 ppm or less, and may be 0 ppm with respect to the entire composition.
  • such an ethanol-free composition suppresses the precipitation of insoluble precipitates, and exhibits an excellent perceptual hypersensitivity suppressing effect and a floating bacteria sterilizing effect.
  • the liquid oral cavity composition of the present invention is particularly suitable as a mouthwash.
  • other well-known components can be mix
  • a wetting agent, a solvent, and if necessary, a sweetening agent, a coloring agent, a preservative, a fragrance, an active ingredient, and the like are blended.
  • polishing agent are not normally mix
  • surfactant surfactants other than (C) nonionic surfactant and (D) amphoteric surfactant may not be added, but in the case of adding 0.5% or less (0 to 0.5%), particularly 0.05 to 0.2% is desirable.
  • wetting agent examples include sugar alcohols such as sorbitol, and polyhydric alcohols such as glycerin and polyethylene glycol.
  • sugar alcohols such as sorbitol
  • polyhydric alcohols such as glycerin and polyethylene glycol.
  • the blending amount of these wetting agents is usually 1 to 40%, particularly 2 to 40%.
  • purified water is generally used, and the water content in the composition can be added within the above range. Further, a lower monohydric alcohol having 1 to 3 carbon atoms such as ethanol, propylene glycol or the like may be blended.
  • sweetening agents xylitol, maltitol, saccharin, saccharin sodium, stevioside, aspartame, and the like can be blended.
  • a colorant a highly safe water-soluble pigment such as Blue No. 1, Green No. 3, Yellow No. 4, Red No. 105, or the like can be added.
  • the preservative include paraoxybenzoic acid ester, benzoic acid or a salt thereof.
  • Natural flavors such as peppermint oil, spearmint oil, eucalyptus oil, wintergreen oil, clove oil, thyme oil, sage oil, cardamom oil, rosemary oil, marjoram oil, lemon oil, nutmeg oil, lavender oil, paracres oil, etc.
  • Active ingredients include potassium nitrate, cetylpyridinium chloride, bactericides such as isopropylmethylphenol, anti-inflammatory agents such as tranexamic acid and epsilon-aminocaproic acid, enzymes such as dextranase, sodium fluoride, monofluorophosphoric acid Examples include fluorides such as sodium, allantoin, vitamins such as vitamin C, copper compounds, and plant extracts. In addition amount of these active ingredients can be made into the range which does not prevent the effect of this invention.
  • Liquid oral compositions having the compositions shown in Tables 1 and 2 were prepared by a conventional method.
  • mouthwash thus obtained was evaluated by the following methods and criteria, the results shown in Tables 1 and 2 were obtained.
  • the bacterial solution used was Streptococcus as an oral resident bacteria prepared by dissolving 30 g of Trypticase Soy Broth (Difco) in 1 L of purified water as a culture solution. Prepared by adding physiological saline so that the permeability at 550 nm of a solution cultured for 1 day under anaerobic conditions (5 vol% carbon dioxide gas, 95 vol% nitrogen) using mutans ATCC 10449 strain is 20 did. Add 0.3 mL of the bacterial solution to 2.7 mL of the sample (liquid oral composition), stir, react at 37 ° C. for 1 minute, stir again, and then add five test tubes containing 2.7 mL of the culture solution in advance.
  • the compounding quantity of alkylamide betaine is also a pure part conversion value also including the inside of a table
  • the raw materials used are the same as described above.
  • This mouthwash was all excellent in appearance stability (precipitation suppression effect), hypersensitivity suppression effect, airborne bacteria sterilization effect, and feeling of use (no bitterness).
  • mouthwash A
  • B Cetylpyridinium chloride 0.05
  • C Polyoxyethylene
  • D Alkylamidobetaine 0.3
  • Glycerin 3.0 Propylene glycol 8.0 Saccharin sodium 0.1 Sodium dihydrogen phosphate 0.5 Sodium hydroxide 0.16 Fragrance 0.2
  • E Purified water 82.19 Total 100.0% pH 6.8

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Abstract

Provided is an oral liquid composition which is prepared by adding, to an oral liquid composition being free from ethanol and comprising potassium nitrate (A)and cetyl pyridinium chloride (B), a nonionic surfactant (C) and an amphoteric surfactant (D), wherein the content of water (E) is controlled to 55 mass% or higher and lower than 92 mass% and the pH of the composition is adjusted to 6.8 or higher and lower than 8.0. The oral liquid composition, wherein the sedimentation of an insoluble precipitate, said precipitate being formed by the combined use of the components (A) and (B) in the aforesaid oral liquid composition, is suppressed, has excellent effects of suppressing hypersensitivity and preventing dental caries.

Description

液体口腔用組成物Liquid oral composition
 本発明は、知覚過敏抑制効果及び口腔内の浮遊菌殺菌効果が優れる、硝酸カリウムを含有するエタノール無配合の液体口腔用組成物に関する。 The present invention relates to a liquid oral composition containing no potassium nitrate and containing no ethanol, which is excellent in hypersensitivity suppression effect and bactericidal effect in the oral cavity.
 象牙質知覚過敏症の予防策として、有効成分として公知の硝酸カリウムが口腔用組成物に配合される(特許文献1、2)。この硝酸カリウムは、口腔用組成物に一般的に配合されるラウリル硫酸ナトリウム存在下で不溶性析出物を生成するという問題があり、特許文献3では、硝酸カリウム及びラウリル硫酸ナトリウム含有の口腔用組成物に多価アルコール、両性界面活性剤を配合することによって、ラウリル硫酸カリウムの析出を防止し、低温析出を抑制している。
 また、特に液体口腔用組成物での知覚過敏の抑制には、粘膜刺激が少なく低刺激性であるノンアルコールタイプの液体製剤がより好適である。
As a preventive measure against dentin hypersensitivity, known potassium nitrate is blended into the oral composition as an active ingredient (Patent Documents 1 and 2). This potassium nitrate has a problem that an insoluble precipitate is formed in the presence of sodium lauryl sulfate which is generally blended in an oral composition. In Patent Document 3, there are many oral compositions containing potassium nitrate and sodium lauryl sulfate. By adding a monohydric alcohol and an amphoteric surfactant, precipitation of potassium lauryl sulfate is prevented and low temperature precipitation is suppressed.
In addition, non-alcohol type liquid preparations with less mucosal irritation and low irritation are more suitable for suppressing hypersensitivity particularly in liquid oral compositions.
 一方、カチオン性殺菌剤の塩化セチルピリジニウムは、口腔内の浮遊細菌への殺菌効果が優れ、う蝕等の口腔疾患の予防又は抑制に有効であるが、界面活性剤の影響を受け易い。特許文献4には、ビグアニド系のカチオン性殺菌剤と非イオン性界面活性剤を含有する口腔用組成物に特定化合物を添加し、非イオン性界面活性剤によるカチオン性殺菌剤の失活を防止し安定化配合した技術が提案されている。 On the other hand, cetylpyridinium chloride, a cationic fungicide, has an excellent bactericidal effect on airborne bacteria in the oral cavity and is effective in preventing or suppressing oral diseases such as caries, but is easily affected by a surfactant. In Patent Document 4, a specific compound is added to an oral composition containing a biguanide-based cationic fungicide and a nonionic surfactant to prevent deactivation of the cationic fungicide by the nonionic surfactant. Then, a stabilized blending technique has been proposed.
米国特許第3,863,006号U.S. Pat. No. 3,863,006 特開平7-101842号公報Japanese Patent Laid-Open No. 7-101842 特開2005-68071号公報JP 2005-68071 A 特開昭60-255717号公報JP 60-255717 A 特開2013-35792号公報JP 2013-35792 A 特開2007-84471号公報JP 2007-84471 A
 従って、硝酸カリウムを配合したノンアルコールタイプの液体口腔用製剤で知覚過敏を抑制し、かつ同時に口腔内浮遊菌に対して高い殺菌力を発揮させることができれば、口腔疾患の予防又は抑制により有効であるが、今までの技術では難しいのが現状であり、このような優れた特性を有する液体口腔用製剤の開発が望まれた。 Therefore, if non-alcohol type liquid oral preparation containing potassium nitrate can suppress hypersensitivity and at the same time exert high bactericidal power against oral floating bacteria, it is more effective for prevention or suppression of oral diseases. However, the current situation is that it is difficult with conventional techniques, and the development of liquid oral preparations having such excellent characteristics has been desired.
 本発明は、上記事情に鑑みなされたもので、知覚過敏抑制効果及び口腔内の浮遊菌殺菌効果が優れる、硝酸カリウムを含有するエタノール無配合の液体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 an ethanol-free liquid oral composition containing potassium nitrate, which is excellent in the hypersensitivity suppressing effect and the bactericidal effect of airborne bacteria in the 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)硝酸カリウムと(B)塩化セチルピリジニウムとを配合したエタノール無配合の液体口腔用組成物に、(C)非イオン界面活性剤及び(D)両性界面活性剤を配合し、(E)水分量を55質量%以上92質量%未満とし、組成物のpHを6.8以上8.0未満とすることによって、(A)、(B)成分の併用によって生じる不溶性沈殿物の析出が抑制され、知覚過敏抑制効果及び口腔内の浮遊菌殺菌効果が優れるノンアルコールタイプの液体口腔用組成物が得られ、知覚過敏及びう蝕の抑制に好適に使用し得ることを知見し、本発明をなすに至った。 As a result of intensive studies to achieve the above object, the present inventors have found that (A) potassium nitrate and (B) cetylpyridinium chloride are combined with an ethanol-free liquid oral composition, and (C) nonionic By blending a surfactant and (D) an amphoteric surfactant, (E) the water content is 55% by mass or more and less than 92% by mass, and the pH of the composition is 6.8 or more and less than 8.0 by ( A), non-alcohol-type liquid oral composition is obtained, in which precipitation of insoluble precipitates generated by the combined use of components (B) is suppressed, and the perceptual hypersensitivity suppressing effect and the bactericidal effect of airborne bacteria in the oral cavity are excellent. The present inventors have found that it can be suitably used for caries suppression and have made the present invention.
 即ち、硝酸カリウム含有の液体口腔用組成物に、カチオン性殺菌剤の塩化セチルピリジニウムを配合することによって知覚過敏抑制効果及び口腔内の浮遊菌殺菌効果を付与できると予想されたが、硝酸カリウムと塩化セチルピリジニウムとをエタノール含有液体口腔用組成物中に配合する場合は特段問題が生じないにもかかわらず、低刺激のエタノール無配合の液体口腔用組成物に硝酸カリウムと塩化セチルピリジニウムとを併用して配合すると、不溶性沈殿物が産生されて析出し、これによって、知覚過敏抑制効果が低下し、殺菌効果も十分に発現しなくなるという問題が生じることを知見した。このため、エタノール無配合の液体口腔用組成物中で硝酸カリウムと塩化セチルピリジニウムとを不溶性沈殿物の析出なしに併用し、硝酸カリウム及び塩化セチルピリジニウムの作用効果を満足に発揮させるという新たな課題が浮上した。そこで、これらの課題を解決するため、本発明者らが更に検討を進めた結果、(C)非イオン界面活性剤と(D)両性界面活性剤とを組み合わせて添加し、組成物中の水分量、pHを上記範囲内にすることによって、上記した(A)、(B)成分の併用によって生じる不溶性沈殿物の析出が経時においても抑制され、高い知覚過敏抑制効果及び浮遊菌殺菌効果を同時に付与することができ、また、外観を安定に維持し、苦味を抑えて良好な使用感を与えることもできた。この場合、塩化セチルピリジニウムは非イオン界面活性剤等の界面活性剤による影響を受けて失活し易いにもかかわらず、本発明においては、(C)、(D)成分の界面活性剤の組み合わせが、組成物中の水分量、pHが特定範囲内で特異的に作用し、上記格別かつ顕著な作用効果を与える。
 従って、本発明のエタノール無配合の液体口腔用組成物は、後述の実施例からも明らかなように、液体口腔用組成物を調製して4週間経過しても不溶性沈殿物の析出がほとんどなく外観が経時で安定であり、知覚過敏抑制効果及び口腔内の浮遊菌殺菌効果が高く、また、使用後の苦味が抑制され味の良い良好な使用感を有する。
In other words, it was expected that potassium nitrate-containing cetyl chloride and potassium nitrate and cetyl chloride were expected to be added to the liquid oral composition containing potassium nitrate by adding cetylpyridinium chloride, a cationic fungicide, to prevent hypersensitivity and bactericidal bacteria. When pyridinium is blended into an ethanol-containing liquid oral composition, it is formulated with potassium nitrate and cetylpyridinium chloride in combination with a mild oral ethanol-free liquid oral composition, even though there are no particular problems. Then, it discovered that an insoluble precipitate was produced and precipitated, and this caused a problem that the hypersensitivity suppressing effect was lowered and the bactericidal effect was not sufficiently developed. For this reason, a new problem has emerged in which potassium nitrate and cetylpyridinium chloride are used in combination in a liquid oral composition containing no ethanol without precipitation of insoluble precipitates, and the effects of potassium nitrate and cetylpyridinium chloride are exhibited satisfactorily. did. Therefore, as a result of further investigation by the present inventors in order to solve these problems, (C) a nonionic surfactant and (D) an amphoteric surfactant are added in combination, and moisture in the composition is added. By setting the amount and pH within the above ranges, the precipitation of insoluble precipitates caused by the combined use of the above-described components (A) and (B) is suppressed over time, and a high perceptual hypersensitivity suppressing effect and a floating fungicidal effect are simultaneously achieved. In addition, it was possible to maintain a stable appearance, to suppress the bitterness and to give a good feeling of use. In this case, although cetylpyridinium chloride is easily deactivated due to the influence of a surfactant such as a nonionic surfactant, the combination of (C) and (D) surfactants is used in the present invention. However, the water content and pH in the composition act specifically within a specific range, and give the above-mentioned exceptional and remarkable effects.
Accordingly, as is clear from the examples described later, the liquid oral composition of the present invention containing no ethanol shows almost no insoluble precipitate even after 4 weeks have passed since the preparation of the liquid oral composition. Appearance is stable over time, high sensitivity to hypersensitivity and bactericidal effect on airborne bacteria in the oral cavity, and bitterness after use is suppressed, resulting in a good feeling of good use.
 なお、特許文献3は、口腔用組成物において硝酸カリウム及びラウリル硫酸ナトリウムの併用によって生じるラウリル硫酸カリウムの析出を抑制したものであり、また、特許文献4は、非イオン界面活性剤によるカチオン性殺菌剤の失活防止であり、カチオン性殺菌剤を硝酸カリウムに併用することについて言及されていない。特許文献5、6には、硝酸カリウム、塩化セチルピリジニウムを配合した液体口腔用組成物が記載されているが、これらはエタノール配合組成である。特許文献3~6から、エタノール無配合の液体口腔用組成物における硝酸カリウムと塩化セチルピリジニウムとの併用によって生じる不溶性沈殿物の析出抑制は予測できない。 Patent Document 3 suppresses precipitation of potassium lauryl sulfate caused by the combined use of potassium nitrate and sodium lauryl sulfate in the oral composition, and Patent Document 4 describes a cationic bactericide using a nonionic surfactant. No mention is made of using a cationic bactericide in combination with potassium nitrate. Patent Documents 5 and 6 describe liquid oral compositions containing potassium nitrate and cetylpyridinium chloride, but these are ethanol-containing compositions. From Patent Documents 3 to 6, the suppression of precipitation of insoluble precipitates caused by the combined use of potassium nitrate and cetylpyridinium chloride in a liquid oral composition containing no ethanol cannot be predicted.
 従って、本発明は、下記の液体口腔用組成物及び該組成物における不溶性沈殿物の析出抑制方法を提供する。
〔1〕
 (A)硝酸カリウム及び(B)塩化セチルピリジニウムを配合したエタノール無配合の液体口腔用組成物に、(C)非イオン界面活性剤及び(D)両性界面活性剤を配合し、(E)水分量を55質量%以上92質量%未満とし、組成物のpHを6.8以上8.0未満としたことを特徴とする液体口腔用組成物。
〔2〕
 (C)非イオン界面活性剤がポリオキシエチレン硬化ヒマシ油であり、(D)両性界面活性剤がアルキルアミドベタイン又はその塩である〔1〕記載の液体口腔用組成物。
〔3〕
 (C)非イオン界面活性剤が、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であり、(D)両性界面活性剤が、ヤシ油脂肪酸アミドプロピルベタインである〔1〕又は〔2〕記載の液体口腔用組成物。
〔4〕
 (C)成分を0.1~2質量%、(D)成分を0.1~2質量%配合した〔1〕、〔2〕又は〔3〕記載の液体口腔用組成物。
〔5〕
 (A)成分を0.01~10質量%、(B)成分を0.001~0.1質量%配合した〔1〕~〔4〕のいずれかに記載の液体口腔用組成物。
〔6〕
 洗口剤である〔1〕~〔5〕のいずれかに記載の液体口腔用組成物。
〔7〕
 知覚過敏及びう蝕抑制用である〔1〕~〔6〕のいずれかに記載の液体口腔用組成物。
〔8〕
 (A)硝酸カリウム及び(B)塩化セチルピリジニウムを配合したエタノール無配合の液体口腔用組成物に、(C)非イオン界面活性剤及び(D)両性界面活性剤を配合し、(E)水分量を55質量%以上92質量%未満とし、組成物のpHを6.8以上8.0未満とすることを特徴とする、前記液体口腔用組成物における(A)硝酸カリウム及び(B)塩化セチルピリジニウムの併用によって生じる不溶性沈殿物の析出抑制方法。
〔9〕
 液体口腔用組成物が洗口剤である、〔8〕記載の液体口腔用組成物における(A)硝酸カリウム及び(B)塩化セチルピリジニウムの併用によって生じる不溶性沈殿物の析出抑制方法。
Accordingly, the present invention provides the following liquid oral composition and a method for suppressing the precipitation of insoluble precipitates in the composition.
[1]
(A) A non-ethanol-containing liquid oral composition containing potassium nitrate and (B) cetylpyridinium chloride, (C) a nonionic surfactant and (D) an amphoteric surfactant, and (E) water content The composition for liquid oral cavity, wherein the pH of the composition is 6.8 or more and less than 8.0.
[2]
(C) The liquid oral composition according to [1], wherein the nonionic surfactant is polyoxyethylene hydrogenated castor oil, and (D) the amphoteric surfactant is alkylamide betaine or a salt thereof.
[3]
(C) The nonionic surfactant is polyoxyethylene hydrogenated castor oil having an average addition mole number of ethylene oxide of 40 to 100 mol, and (D) the amphoteric surfactant is coconut oil fatty acid amidopropyl betaine [ 1] or [2] liquid oral composition.
[4]
The liquid oral composition according to [1], [2] or [3], wherein 0.1 to 2% by mass of component (C) and 0.1 to 2% by mass of component (D) are blended.
[5]
The liquid oral composition according to any one of [1] to [4], wherein 0.01 to 10% by mass of component (A) and 0.001 to 0.1% by mass of component (B) are blended.
[6]
The liquid oral composition according to any one of [1] to [5], which is a mouthwash.
[7]
The liquid oral composition according to any one of [1] to [6], which is used for suppressing hypersensitivity and caries.
[8]
(A) A non-ethanol-containing liquid oral composition containing potassium nitrate and (B) cetylpyridinium chloride, (C) a nonionic surfactant and (D) an amphoteric surfactant, and (E) water content 55% by mass or more and less than 92% by mass, and the pH of the composition is 6.8 or more and less than 8.0, wherein (A) potassium nitrate and (B) cetylpyridinium chloride in the liquid oral composition A method for suppressing the precipitation of insoluble precipitates produced by the combined use.
[9]
The method for suppressing precipitation of insoluble precipitates produced by the combined use of (A) potassium nitrate and (B) cetylpyridinium chloride in the liquid oral composition according to [8], wherein the liquid oral composition is a mouthwash.
 本発明によれば、知覚過敏抑制効果及び口腔内の浮遊菌殺菌効果が優れる硝酸カリウム含有のエタノール無配合の液体口腔用組成物を提供できる。 According to the present invention, it is possible to provide a liquid oral composition containing no potassium nitrate and containing no ethanol, which is excellent in the effect of suppressing hypersensitivity and the bactericidal effect of floating bacteria in the oral cavity.
 以下、本発明について更に詳述する。本発明の液体口腔用組成物は、(A)硝酸カリウム、(B)塩化セチルピリジニウム、(C)非イオン界面活性剤、(D)両性界面活性剤、(E)水を含有し、エタノール無配合である。 Hereinafter, the present invention will be described in further detail. The composition for liquid oral cavity of the present invention contains (A) potassium nitrate, (B) cetylpyridinium chloride, (C) nonionic surfactant, (D) amphoteric surfactant, (E) water, and contains no ethanol It is.
 (A)硝酸カリウムは、象牙質知覚過敏症を予防又は治療するための有効成分として配合されるものであり、知覚過敏抑制剤である。
 (A)成分の硝酸カリウムの配合量は、組成物全体の0.01~10%(質量%、以下、同様。)が好ましく、より好ましくは0.1~7%である。配合量が多いほど知覚過敏抑制効果は高まるが、10%以下であることが、十分な析出抑制、苦味の抑制にはより好適である。
(A) Potassium nitrate is blended as an active ingredient for preventing or treating dentin hypersensitivity, and is a hypersensitivity inhibitor.
The blending amount of the component (A) potassium nitrate is preferably 0.01 to 10% (mass%, hereinafter the same) of the whole composition, more preferably 0.1 to 7%. As the blending amount increases, the perceptual hypersensitivity suppression effect increases, but 10% or less is more suitable for sufficient precipitation suppression and bitterness suppression.
 (B)塩化セチルピリジニウムは、カチオン性殺菌剤であり、口腔内浮遊菌に対する殺菌剤である。塩化セチルピリジニウムは、市販のものを使用できる。
 (B)成分の塩化セチルピリジニウムの配合量は、組成物全体の0.001~0.1%が好ましく、より好ましくは0.005~0.1%、さらに好ましくは0.01~0.05%である。多く配合するほど殺菌効果が高まるが、0.1%以下であることが、十分な析出抑制、苦味の抑制にはより好適である。
(B) Cetylpyridinium chloride is a cationic bactericidal agent and a bactericidal agent against floating bacteria in the oral cavity. A commercially available cetylpyridinium chloride can be used.
The amount of component (B) cetylpyridinium chloride is preferably 0.001 to 0.1%, more preferably 0.005 to 0.1%, still more preferably 0.01 to 0.05% of the total composition. %. The more the compound is added, the higher the bactericidal effect, but 0.1% or less is more suitable for sufficient precipitation suppression and bitterness suppression.
 本発明では、(C)非イオン界面活性剤及び(D)両性界面活性剤を組み合わせて配合することが効果発現に重要である。(C)成分又は(D)成分を欠くと、不溶性沈殿物が析出し、知覚過敏抑制効果及び浮遊菌殺菌効果が劣る。また、苦味が抑制されず使用感が劣る。 In the present invention, it is important for the expression of effects to combine (C) a nonionic surfactant and (D) an amphoteric surfactant in combination. When component (C) or component (D) is lacking, an insoluble precipitate is deposited, resulting in poor perceptual hypersensitivity suppressing effect and airborne fungicidal effect. Moreover, a bitter taste is not suppressed but a usability | use_condition is inferior.
 (C)非イオン界面活性剤としては、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、ポリグリセリン脂肪酸エステルが挙げられ、これらの1種又は2種以上を使用し得るが、特に、エチレンオキサイド(E.O.)の平均付加モル数が40~100モル、特に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16~18でE.O.の平均付加モル数が10~40モル、特に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、特に12~14のデカグリセリンモノ脂肪酸エステルポリグリセリン脂肪酸エステルが好ましく、中でもE.O.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が好ましい。 Examples of (C) nonionic surfactants include polyoxyethylene hydrogenated castor oil, polyoxyethylene alkyl ether, and polyglycerin fatty acid ester, and one or more of these may be used. (E.O.) polyoxyethylene hydrogenated castor oil having an average added mole number of 40 to 100 moles, particularly 60 to 100 moles, and an alkyl group having 16 to 18 carbon atoms. O. Preferred are polyoxyethylene alkyl ethers having an average addition mole number of 10 to 40 moles, particularly 20 to 40 moles, and decaglycerin monofatty acid esters polyglycerin fatty acid esters having a fatty acid number of 12 to 18, particularly 12 to 14, among others. E. O. Polyoxyethylene hydrogenated castor oil having an average added mole number of 40 to 100 moles is preferred.
 具体的には、商品化されている下記に示すような市販品を使用することができる。
 ポリオキシエチレン硬化ヒマシ油;
 日光ケミカルズ社製のNIKKOL HCO系、日本エマルジョン社製のエマレックスHC系、日本油脂社製のユニオックスHC系
 ポリオキシエチレンアルキルエーテル;
 日光ケミカルズ社製のNIKKOL BC系、NIKKOL BS系、日本エマルジョン社製のエマレックス100系、エマレックス600系
 デカグリセリンモノ脂肪酸エステル;
 日光ケミカルズ社製のNIKKOL Decagln系、三菱化学フーズ社製のリョートー(登録商標)ポリグリエステルDシリーズ
Specifically, commercialized products as shown below that are commercialized can be used.
Polyoxyethylene hydrogenated castor oil;
NIKKOL HCO manufactured by Nikko Chemicals, Emalex HC manufactured by Nippon Emulsion, UNIOX HC manufactured by Nippon Yushi Co., Ltd. polyoxyethylene alkyl ether;
NIKKOL BC series, NIKKOL BS series manufactured by Nikko Chemicals, Emalex 100 series, Emalex 600 series decaglycerin mono fatty acid ester manufactured by Nippon Emulsion Co., Ltd .;
NIKKOL Decagln series manufactured by Nikko Chemicals, Ryoto (registered trademark) polyglycerester D series manufactured by Mitsubishi Chemical Foods
 (C)成分の非イオン界面活性剤の配合量は、組成物全体の0.1~2%が好ましく、より好ましくは0.1~1%、さらに好ましくは0.2~0.5%である。0.1%以上配合すると、十分な析出抑制効果、知覚過敏抑制効果及び浮遊菌殺菌効果を奏し、また、苦味を十分に抑制できる。2%以下であることが、知覚過敏抑制効果及び浮遊菌殺菌効果が低下するのを防止するにはより好適である。 The blending amount of the nonionic surfactant as the component (C) is preferably 0.1 to 2% of the total composition, more preferably 0.1 to 1%, still more preferably 0.2 to 0.5%. is there. When 0.1% or more is blended, a sufficient precipitation suppressing effect, a hypersensitivity suppressing effect and a floating bacteria sterilizing effect are exhibited, and the bitterness can be sufficiently suppressed. 2% or less is more suitable for preventing the perceptual hypersensitivity suppressing effect and the floating bacteria bactericidal effect from decreasing.
(D)両性界面活性剤としては、ヤシ油脂肪酸アミドプロピルベタイン等のアルキルアミドベタイン又はその塩、ラウリルジメチルアミノ酢酸ベタイン等の酢酸ベタイン型、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等のイミダゾリン型、N-脂肪酸アシル-L-アルギネート塩等のアミノ酸型などが挙げられ、これらの1種又は2種以上を使用し得るが、特に、アルキルアミドベタイン又はその塩が好ましく、中でも、ヤシ油脂肪酸アミドプロピルベタインが好適である。
 具体的には、ヤシ油脂肪酸アミドプロピルベタイン(デグッサ社製のTEGO Betain CK OK(30%水溶液)、花王(株)製のアンヒトール55AB(30%水溶液))などの市販品を使用し得る。
(D) Amphoteric surfactants include alkylamidobetaines such as coconut oil fatty acid amidopropylbetaine or salts thereof, betaine acetates such as lauryldimethylaminoacetic acid betaine, N-fatty acid acyl-N-carboxymethyl-N-hydroxyethyl Examples include imidazoline type such as ethylenediamine salt, amino acid type such as N-fatty acid acyl-L-alginate salt, and the like, and one or more of these may be used, and alkylamide betaine or a salt thereof is particularly preferable. Among these, coconut oil fatty acid amidopropyl betaine is preferable.
Specifically, commercially available products such as coconut oil fatty acid amidopropyl betaine (TEGO Betaine CK OK (30% aqueous solution) manufactured by Degussa Co., Ltd., and Amphitol 55AB (30% aqueous solution) manufactured by Kao Corporation) can be used.
 (D)成分の両性界面活性剤の配合量は、組成物全体の0.1~2%が好ましく、より好ましくは0.1~1%、さらに好ましくは0.2~0.5%である。0.1%以上配合すると、十分な析出抑制効果、知覚過敏抑制効果及び浮遊菌殺菌効果を奏し、また、苦味を十分に抑制できる。2%以下であることが、知覚過敏抑制効果及び浮遊菌殺菌効果が低下するのを防止するにはより好適である。 The blending amount of the amphoteric surfactant as component (D) is preferably 0.1 to 2% of the total composition, more preferably 0.1 to 1%, and still more preferably 0.2 to 0.5%. . When 0.1% or more is blended, a sufficient precipitation suppressing effect, a hypersensitivity suppressing effect and a floating bacteria sterilizing effect are exhibited, and the bitterness can be sufficiently suppressed. 2% or less is more suitable for preventing the perceptual hypersensitivity suppressing effect and the floating bacteria bactericidal effect from decreasing.
 本発明の液体口腔用組成物は、(E)水の含有量、つまり組成物中の水分量が、組成物全体の55%以上92%未満であり、好ましくは60%以上91%以下、より好ましくは60%以上70%以下である。水分量が上記範囲内であると、不溶性沈殿物を析出抑制でき、優れた知覚過敏抑制効果及び苦味抑制効果を付与することができる。55%未満であると、析出抑制できず、知覚過敏抑制効果及び浮遊菌殺菌効果が劣る。92%以上であると、析出抑制効果が劣り、知覚過敏抑制効果及び浮遊菌殺菌効果も劣り、苦味を抑制することもできない。 In the liquid oral cavity composition of the present invention, (E) the water content, that is, the water content in the composition is 55% or more and less than 92% of the whole composition, preferably 60% or more and 91% or less. Preferably they are 60% or more and 70% or less. When the amount of water is within the above range, insoluble precipitates can be prevented from being precipitated, and excellent perceptual hypersensitivity suppressing effects and bitterness suppressing effects can be imparted. If it is less than 55%, the precipitation cannot be suppressed, and the perceptual hypersensitivity suppressing effect and the floating bacteria sterilizing effect are inferior. When it is 92% or more, the precipitation suppressing effect is inferior, the perceptual hypersensitivity suppressing effect and the floating bacteria sterilizing effect are also inferior, and the bitterness cannot be suppressed.
 本発明において、液体口腔用組成物のpHは6.8以上8.0未満であり、好ましくはpH6.8~7.8、より好ましくはpH6.8~7.5である。上記範囲内であると、析出抑制効果、知覚過敏抑制効果及び苦味抑制効果が優れる。pH6.8未満又はpH8.0以上であると、析出抑制できず、知覚過敏抑制効果及び浮遊菌殺菌効果が劣る。
 なお、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分後の値である(以下、同様。)。
In the present invention, the liquid oral composition has a pH of 6.8 or more and less than 8.0, preferably pH 6.8 to 7.8, more preferably pH 6.8 to 7.5. Within the above range, the precipitation suppression effect, the hypersensitivity suppression effect and the bitterness suppression effect are excellent. When the pH is less than 6.8 or pH 8.0 or more, the precipitation cannot be suppressed, and the perceptual hypersensitivity suppressing effect and the floating bacteria sterilizing effect are inferior.
The pH was measured immediately after preparation using a pH meter (model number Hm-30S) manufactured by Toa Denpa Kogyo Co., Ltd., and the value after 3 minutes at 25 ° C. (the same applies hereinafter).
 本発明では、組成物のpHを上記範囲内に調整するのに、公知のpH調整剤を添加してもよい。例えばリン酸二水素ナトリウム等のリン酸水素アルカリ金属塩、水酸化ナトリウム等のアルカリ金属の水酸化物などが挙げられる。 In the present invention, a known pH adjusting agent may be added to adjust the pH of the composition within the above range. Examples thereof include alkali metal hydrogen phosphates such as sodium dihydrogen phosphate and alkali metal hydroxides such as sodium hydroxide.
 本発明の液体口腔用組成物は、エタノール無配合である。ここで、「エタノール無配合」とは、エタノールが配合されないものであるが、液体口腔用組成物では、組成物中に配合される香料中に原料由来のエタノールが微量含まれる場合などがあるため、これらの理由を考慮した上で、香料中などに微量含有されるエタノール以外にエタノールを含まないものである。なお、この場合、組成物中のエタノール量は組成物全体に対して好ましくは100ppm以下、より好ましくは50ppm以下、さらに好ましくは10ppm以下であり、0ppmであってもよい。
 本発明では、このようなエタノール無配合の組成で、不溶性沈殿物の析出を抑制し、優れた知覚過敏抑制効果及び浮遊菌殺菌効果を奏する。
The liquid oral cavity composition of the present invention contains no ethanol. Here, “ethanol-free formulation” is one in which ethanol is not blended, but in liquid oral compositions, there are cases where a small amount of ethanol derived from the raw material is contained in the fragrance blended in the composition. In consideration of these reasons, ethanol is not included in addition to ethanol contained in a trace amount in a fragrance. In this case, the amount of ethanol in the composition is preferably 100 ppm or less, more preferably 50 ppm or less, still more preferably 10 ppm or less, and may be 0 ppm with respect to the entire composition.
In the present invention, such an ethanol-free composition suppresses the precipitation of insoluble precipitates, and exhibits an excellent perceptual hypersensitivity suppressing effect and a floating bacteria sterilizing effect.
 本発明の液体口腔用組成物は、特に洗口剤として好適である。また、本発明組成物には、上記成分に加えて、必要に応じてその他の公知成分を、本発明の効果を妨げない範囲で配合できる。具体的には、湿潤剤、溶剤、更に必要により甘味剤、着色剤、防腐剤、香料、有効成分等が配合される。
 なお、液体口腔用組成物、特に洗口剤には、研磨剤などの可溶化しない固形成分は通常配合されず、研磨剤は含まないことが好ましい。
 また、界面活性剤としては、(C)非イオン界面活性剤及び(D)両性界面活性剤以外の界面活性剤は配合しなくてもよいが、配合する場合は0.5%以下(0~0.5%)、特に0.05~0.2%が望ましい。
The liquid oral cavity composition of the present invention is particularly suitable as a mouthwash. Moreover, in addition to the said component, other well-known components can be mix | blended with this invention composition in the range which does not prevent the effect of this invention as needed. Specifically, a wetting agent, a solvent, and if necessary, a sweetening agent, a coloring agent, a preservative, a fragrance, an active ingredient, and the like are blended.
In addition, it is preferable that solid components which do not solubilize, such as an abrasive | polishing agent, are not normally mix | blended with a liquid oral composition, especially a mouthwash, and an abrasive | polishing agent is not included.
Further, as the surfactant, surfactants other than (C) nonionic surfactant and (D) amphoteric surfactant may not be added, but in the case of adding 0.5% or less (0 to 0.5%), particularly 0.05 to 0.2% is desirable.
 湿潤剤としては、例えばソルビトール等の糖アルコール、グリセリン、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。これら湿潤剤の配合量は、通常、1~40%、特に2~40%である。 Examples of the wetting agent include sugar alcohols such as sorbitol, and polyhydric alcohols such as glycerin and polyethylene glycol. The blending amount of these wetting agents is usually 1 to 40%, particularly 2 to 40%.
 溶剤としては、精製水が一般的に用いられ、組成物中の水分量が上記範囲内で添加することができる。また、エタノール等の炭素数1~3の低級一価アルコール、プロピレングリコール等を配合してもよい。 As the solvent, purified water is generally used, and the water content in the composition can be added within the above range. Further, a lower monohydric alcohol having 1 to 3 carbon atoms such as ethanol, propylene glycol or the like may be blended.
 甘味剤としては、キシリトール、マルチトール、サッカリン、サッカリンナトリウム、ステビオサイド、アスパルテーム等を配合することができる。着色剤として、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を添加することができる。防腐剤としては、パラオキシ安息香酸エステル、安息香酸又はその塩が挙げられる。 As sweetening agents, xylitol, maltitol, saccharin, saccharin sodium, stevioside, aspartame, and the like can be blended. As a colorant, a highly safe water-soluble pigment such as Blue No. 1, Green No. 3, Yellow No. 4, Red No. 105, or the like can be added. Examples of the preservative include paraoxybenzoic acid ester, benzoic acid or a salt thereof.
 香料としては、ペパーミント油、スペアミント油、ユーカリ油、ウィンターグリーン油、クローブ油、タイム油、セージ油、カルダモン油、ローズマリー油、マジョラム油、レモン油、ナツメグ油、ラベンダー油、パラクレス油等の天然精油、及びl-メントール、l-カルボン、シンナミックアルデヒド、オレンジオイル、アネトール、1,8-シネオール、メチルサリシレート、オイゲノール、チモール、リナロール、リモネン、メントン、メンチルアセテート、シトラール、カンファー、ボルネオール、ピネン、スピラントール等の上記天然精油中に含まれる香料成分、また、エチルアセテート、エチルブチレート、イソアミルアセテート、ヘキサナール、ヘキセナール、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、ベンツアルデヒド、バニリン、エチルバニリン、フラネオール、マルトール、エチルマルトール、ガンマ/デルタデカラクトン、ガンマ/デルタウンデカラクトン、N-エチル-p-メンタン-3-カルボキサミド、メンチルラクテート、エチレングリコール-l-メンチルカーボネート等の香料成分、更には、いくつかの香料成分や天然精油を組み合わせてなる、アップル、バナナ、ストロベリー、ブルーベリー、メロン、ピーチ、パイナップル、グレープ、マスカット、ワイン、チェリー、スカッシュ、コーヒー、ブランデー、ヨーグルト等の調合フレーバーの1種又は2種以上を、組成物中0.00001~3%で、本発明の効果を妨げない範囲で使用することができる。 Natural flavors such as peppermint oil, spearmint oil, eucalyptus oil, wintergreen oil, clove oil, thyme oil, sage oil, cardamom oil, rosemary oil, marjoram oil, lemon oil, nutmeg oil, lavender oil, paracres oil, etc. Essential oils and l-menthol, l-carvone, cinnamic aldehyde, orange oil, anethole, 1,8-cineole, methyl salicylate, eugenol, thymol, linalool, limonene, menthone, menthyl acetate, citral, camphor, borneol, pinene, Perfume ingredients contained in the above-mentioned natural essential oils such as spiranthol, ethyl acetate, ethyl butyrate, isoamyl acetate, hexanal, hexenal, methylanthranilate, ethylmethylphenylglycidide , Benzaldehyde, vanillin, ethyl vanillin, furaneol, maltol, ethyl maltol, gamma / delta decalactone, gamma / deltown decalactone, N-ethyl-p-menthane-3-carboxamide, menthyl lactate, ethylene glycol-1-menthyl Perfume ingredients such as carbonate, and also a combination of several perfume ingredients and natural essential oils, apple, banana, strawberry, blueberry, melon, peach, pineapple, grape, muscat, wine, cherry, squash, coffee, brandy, One or more kinds of blended flavors such as yogurt can be used within the range of 0.00001 to 3% in the composition without impairing the effects of the present invention.
 有効成分としては、硝酸カリウム、塩化セチルピリジニウムに加えて、イソプロピルメチルフェノール等の殺菌剤、トラネキサム酸、イプシロン-アミノカプロン酸等の抗炎症剤、デキストラナーゼ等の酵素、フッ化ナトリウム、モノフルオロリン酸ナトリウム等のフッ化物、アラントイン、ビタミンC等のビタミン類、銅化合物、植物抽出物等が挙げられる。なお、これらの有効成分の添加量は、本発明の効果を妨げない範囲とすることができる。 Active ingredients include potassium nitrate, cetylpyridinium chloride, bactericides such as isopropylmethylphenol, anti-inflammatory agents such as tranexamic acid and epsilon-aminocaproic acid, enzymes such as dextranase, sodium fluoride, monofluorophosphoric acid Examples include fluorides such as sodium, allantoin, vitamins such as vitamin C, copper compounds, and plant extracts. In addition, the addition amount of these active ingredients can be made into the range which does not prevent the effect of this invention.
 以下、実施例及び比較例、処方例を示し、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、pHは上記と同様に25℃において測定した。 Hereinafter, although an Example, a comparative example, and a formulation example are shown and this invention is demonstrated concretely, this invention is not restrict | limited to the following Example. In the following examples, “%” means “% by mass” unless otherwise specified. The pH was measured at 25 ° C. as described above.
 [実施例、比較例]
 表1、2に示す組成の液体口腔用組成物(洗口剤)を常法により調製した。得られた洗口剤について、下記の方法及び基準により評価を行ったところ、表1、2のような結果が得られた。
[Examples and Comparative Examples]
Liquid oral compositions (mouthwashes) having the compositions shown in Tables 1 and 2 were prepared by a conventional method. When the mouthwash thus obtained was evaluated by the following methods and criteria, the results shown in Tables 1 and 2 were obtained.
(1)外観安定性(析出抑制効果)の評価方法
 表に記載の各洗口剤を100mLのペットボトル中に80mL入れ、25℃恒温槽中に静置保存し、4週間後の外観を下記の評点基準に従い目視で判定した。5サンプルの平均値を求め、下記の評価基準に従って評価した。
 評点基準:
  4点:析出物が全くなかった
  3点:析出物がわずかにあった
  2点:析出物がややあった
  1点:析出物がかなりあった
 外観安定性(析出抑制効果)の評価基準:
  ◎:平均点3.5点以上4.0点以下
  ○: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
(1) Evaluation method of appearance stability (precipitation suppression effect) Each mouthwash described in the table is put in 80 mL in a 100 mL PET bottle and stored in a constant temperature bath at 25 ° C., and the appearance after 4 weeks is shown below. It was judged visually according to the rating criteria. The average value of 5 samples was calculated and evaluated according to the following evaluation criteria.
Score criteria:
4 points: no precipitates 3 points: slight precipitates 2 points: some precipitates 1 point: considerable precipitates Evaluation criteria for appearance stability (precipitation suppression effect):
◎: Average point 3.5 points or more and 4.0 points or less ○: Average point 3.0 points or more and less than 3.5 points △: Average point 2.0 points or more and less than 3.0 points ×: Average point 2.0 points Less than
(2)知覚過敏抑制効果の評価方法
 表に記載の各洗口剤を、象牙質知覚過敏を有する人5名に1ヶ月間、通常の方法で洗口して使用させ、知覚過敏の抑制効果を下記評点基準で判定した。被験者5名の平均値を求め、下記の評価基準に従って評価した。
 知覚過敏抑制効果の評点基準:
  3点:痛みを感じなくなった
  2点:ほとんど痛みを感じなくなった
  1点:痛みを感じる
 知覚過敏抑制効果の評価基準:
  ◎:2.5点以上3.0点以下
  ○:2.0点以上2.5点未満
  △:1.5点以上2.0点未満
  ×:1.5点未満
(2) Evaluation method of hypersensitivity suppression effect Each mouthwash listed in the table was used by 5 people with dentin hypersensitivity for 1 month by mouthwashing in a normal manner, and the suppression effect of hypersensitivity Was determined according to the following criteria. An average value of five subjects was obtained and evaluated according to the following evaluation criteria.
Evaluation criteria for hypersensitivity suppression:
3 points: no longer feel pain 2 points: almost no pain 1 point: feel pain Evaluation criteria for hypersensitivity suppression effect:
◎: 2.5 points or more and 3.0 points or less ○: 2.0 points or more and less than 2.5 points △: 1.5 points or more and less than 2.0 points ×: Less than 1.5 points
(3)口腔内浮遊菌に対する殺菌効果の評価方法
 使用した菌液は、培養液としてトリプチケースソイブロス(Difco社製)30gを1Lの精製水に溶解したものを、口腔常在細菌としてストレプトコッカス ミュータンスATCC10449株を用い、37℃、嫌気条件下(5容量%炭酸ガス、95容量%窒素)で1日培養した液の550nmでの透過度が20になるように生理食塩水を加えて調製した。サンプル(液体口腔用組成物)2.7mLに菌液0.3mLを加え、撹拌後、37℃で1分間反応させ、再び撹拌後、予め2.7mLの培養液の入った試験管を5本用意し、その1番目の試験管に、前記菌液を加えたサンプル0.3mLを加え、撹拌した。この液0.3mLを採取し、2番目の試験管に加え、撹拌した。この操作を同様に3~5番目の試験管に順に行った。1、3、5番目の試験管中の培養液を撹拌後、10%綿羊脱繊血含有トリプチケースソイ寒天平板(Difco社製)に50μL塗沫し、嫌気条件下で培養した。生育したコロニーを計測し、残存するストレプトコッカス ミュータンス菌の生菌数(cfu)を求め、下記の基準に則り、浮遊菌殺菌効果を判定した。
 判定基準:
  ◎:生菌数が102未満
  ○:生菌数が102以上103未満
  △:生菌数が103以上104未満
  ×:生菌数が104以上
(3) Method for evaluating bactericidal effect against oral floating bacteria The bacterial solution used was Streptococcus as an oral resident bacteria prepared by dissolving 30 g of Trypticase Soy Broth (Difco) in 1 L of purified water as a culture solution. Prepared by adding physiological saline so that the permeability at 550 nm of a solution cultured for 1 day under anaerobic conditions (5 vol% carbon dioxide gas, 95 vol% nitrogen) using mutans ATCC 10449 strain is 20 did. Add 0.3 mL of the bacterial solution to 2.7 mL of the sample (liquid oral composition), stir, react at 37 ° C. for 1 minute, stir again, and then add five test tubes containing 2.7 mL of the culture solution in advance. Prepared and added to the first test tube 0.3 mL of the sample with the bacterial solution added, and stirred. 0.3 mL of this solution was collected, added to the second test tube, and stirred. This operation was similarly performed in order on the third to fifth test tubes. After stirring the culture solution in the first, third, and fifth test tubes, 50 μL of the culture solution was spread on a 10% cotton defibrinated blood-containing trypticase soy agar plate (manufactured by Difco) and cultured under anaerobic conditions. The grown colonies were counted, the number of surviving Streptococcus mutans bacteria (cfu) was determined, and the bactericidal effect of planktonic bacteria was determined according to the following criteria.
Judgment criteria:
◎: Viable count is less than 10 2 ○: Viable count is 10 2 or more and less than 10 3 △: Viable count is 10 3 or more and less than 10 4 ×: Viable count is 10 4 or more
(4)使用感(苦味のなさ)の評価方法
 表に記載の各洗口剤10mLを口に含み、30秒間すすいだ後、洗口後の苦味について判定士5名が下記の評点基準により判定した。5名の平均値を求め、下記の評価基準に従って評価した。
 評点基準:
  4点:苦味がなかった
  3点:苦味がほとんどなかった
  2点:苦味がややあった。
  1点:苦味がかなりあった
 使用感(洗口後の苦味のなさ)の評価基準:
  ◎:平均点3.5点以上4.0点以下
  ○: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
(4) Evaluation method of feeling of use (no bitterness) Each mouthwash containing 10 mL of mouthwashes listed in the table was rinsed for 30 seconds, and after the mouthwash, 5 judges were judged according to the following scoring standards. did. The average value of 5 persons was calculated | required and evaluated according to the following evaluation criteria.
Score criteria:
4 points: no bitterness 3 points: little bitterness 2 points: Some bitterness
1 point: There was considerable bitterness Evaluation criteria for feeling of use (no bitterness after mouthwash):
◎: Average point 3.5 points or more and 4.0 points or less ○: Average point 3.0 points or more and less than 3.5 points △: Average point 2.0 points or more and less than 3.0 points ×: Average point 2.0 points Less than
 使用原料の詳細を下記に示す。
(A)硝酸カリウム;硝酸カリウムスーパータブレット(大塚食品化学社製
   )
(B)塩化セチルピリジニウム;塩化セチルピリジニウム(和光純薬工業社
   製)
(C)ポリオキシエチレン(100)硬化ヒマシ油;
   エチレンオキサイドの平均付加モル数100(日光ケミカルズ社製)
   ポリオキシエチレン(40)硬化ヒマシ油;
   エチレンオキサイドの平均付加モル数40(日光ケミカルズ社製)
(D)アルキルアミドベタイン;
   ヤシ油脂肪酸アミドプロピルベタインの30%水溶液、TEGO B
   etain CK OK(デグッサ社製)
 なお、表中も含め、アルキルアミドベタインの配合量は、純分換算値である(以下、同様。)。
Details of the raw materials used are shown below.
(A) Potassium nitrate; potassium nitrate super tablet (manufactured by Otsuka Food Chemical Co., Ltd.)
(B) Cetylpyridinium chloride; cetylpyridinium chloride (manufactured by Wako Pure Chemical Industries, Ltd.)
(C) polyoxyethylene (100) hydrogenated castor oil;
Average number of moles of ethylene oxide added (Nikko Chemicals)
Polyoxyethylene (40) hydrogenated castor oil;
Average addition mole number of ethylene oxide 40 (manufactured by Nikko Chemicals)
(D) an alkylamidobetaine;
30% aqueous solution of palm oil fatty acid amidopropyl betaine, TEGO B
etain CK OK (Degussa)
In addition, the compounding quantity of alkylamide betaine is also a pure part conversion value also including the inside of a table | surface (following, the same).
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000002
 *;比較例8のエタノール配合組成では、(A)、(B)成分が配合されていても不溶性沈殿物の析出がなく、知覚過敏抑制効果、浮遊菌殺菌効果が低下することもなかった。
Figure JPOXMLDOC01-appb-T000002
*: In the ethanol blending composition of Comparative Example 8, even when the components (A) and (B) were blended, there was no precipitation of insoluble precipitates, and the hypersensitivity suppressing effect and the floating fungicidal effect were not reduced.
 以下、処方例を示す。使用原料は上記と同様である。この洗口剤は、外観安定性(析出抑制効果)、知覚過敏抑制効果、浮遊菌殺菌効果、使用感(苦味のなさ)が全て優れた。 The following are examples of prescriptions. The raw materials used are the same as described above. This mouthwash was all excellent in appearance stability (precipitation suppression effect), hypersensitivity suppression effect, airborne bacteria sterilization effect, and feeling of use (no bitterness).
 [処方例]洗口剤
(A)硝酸カリウム                 5.0%
(B)塩化セチルピリジニウム            0.05
(C)ポリオキシエチレン(60)硬化ヒマシ油    0.5
(D)アルキルアミドベタイン            0.3
グリセリン                     3.0
プロピレングリコール                8.0
サッカリンナトリウム                0.1
リン酸二水素ナトリウム               0.5
水酸化ナトリウム                  0.16
香料                        0.2
(E)精製水                   82.19
計                       100.0%
 pH 6.8
[Prescription example] mouthwash (A) potassium nitrate 5.0%
(B) Cetylpyridinium chloride 0.05
(C) Polyoxyethylene (60) hydrogenated castor oil 0.5
(D) Alkylamidobetaine 0.3
Glycerin 3.0
Propylene glycol 8.0
Saccharin sodium 0.1
Sodium dihydrogen phosphate 0.5
Sodium hydroxide 0.16
Fragrance 0.2
(E) Purified water 82.19
Total 100.0%
pH 6.8

Claims (9)

  1.  (A)硝酸カリウム及び(B)塩化セチルピリジニウムを配合したエタノール無配合の液体口腔用組成物に、(C)非イオン界面活性剤及び(D)両性界面活性剤を配合し、(E)水分量を55質量%以上92質量%未満とし、組成物のpHを6.8以上8.0未満としたことを特徴とする液体口腔用組成物。 (A) A non-ethanol-containing liquid oral composition containing potassium nitrate and (B) cetylpyridinium chloride, (C) a nonionic surfactant and (D) an amphoteric surfactant, and (E) water content The composition for liquid oral cavity, wherein the pH of the composition is 6.8 or more and less than 8.0.
  2.  (C)非イオン界面活性剤がポリオキシエチレン硬化ヒマシ油であり、(D)両性界面活性剤がアルキルアミドベタイン又はその塩である請求項1記載の液体口腔用組成物。 The liquid oral composition according to claim 1, wherein (C) the nonionic surfactant is polyoxyethylene hydrogenated castor oil, and (D) the amphoteric surfactant is alkylamide betaine or a salt thereof.
  3.  (C)非イオン界面活性剤が、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であり、(D)両性界面活性剤が、ヤシ油脂肪酸アミドプロピルベタインである請求項1又は2記載の液体口腔用組成物。 (C) The nonionic surfactant is polyoxyethylene hydrogenated castor oil having an average addition mole number of ethylene oxide of 40 to 100 mol, and (D) the amphoteric surfactant is coconut oil fatty acid amidopropyl betaine. Item 3. The liquid oral composition according to Item 1 or 2.
  4.  (C)成分を0.1~2質量%、(D)成分を0.1~2質量%配合した請求項1、2又は3記載の液体口腔用組成物。 4. The composition for liquid oral cavity according to claim 1, wherein 0.1 to 2% by mass of component (C) and 0.1 to 2% by mass of component (D) are blended.
  5.  (A)成分を0.01~10質量%、(B)成分を0.001~0.1質量%配合した請求項1~4のいずれか1項記載の液体口腔用組成物。 5. The liquid oral composition according to any one of claims 1 to 4, wherein 0.01 to 10% by mass of component (A) and 0.001 to 0.1% by mass of component (B) are blended.
  6.  洗口剤である請求項1~5のいずれか1項記載の液体口腔用組成物。 The liquid oral composition according to any one of claims 1 to 5, which is a mouthwash.
  7.  知覚過敏及びう蝕抑制用である請求項1~6のいずれか1項記載の液体口腔用組成物。 The liquid oral composition according to any one of claims 1 to 6, which is used for suppressing hypersensitivity and caries.
  8.  (A)硝酸カリウム及び(B)塩化セチルピリジニウムを配合したエタノール無配合の液体口腔用組成物に、(C)非イオン界面活性剤及び(D)両性界面活性剤を配合し、(E)水分量を55質量%以上92質量%未満とし、組成物のpHを6.8以上8.0未満とすることを特徴とする、前記液体口腔用組成物における(A)硝酸カリウム及び(B)塩化セチルピリジニウムの併用によって生じる不溶性沈殿物の析出抑制方法。 (A) A non-ethanol-containing liquid oral composition containing potassium nitrate and (B) cetylpyridinium chloride, (C) a nonionic surfactant and (D) an amphoteric surfactant, and (E) water content 55% by mass or more and less than 92% by mass, and the pH of the composition is 6.8 or more and less than 8.0, wherein (A) potassium nitrate and (B) cetylpyridinium chloride in the liquid oral composition A method for suppressing the precipitation of insoluble precipitates produced by the combined use.
  9.  液体口腔用組成物が洗口剤である、請求項8記載の液体口腔用組成物における(A)硝酸カリウム及び(B)塩化セチルピリジニウムの併用によって生じる不溶性沈殿物の析出抑制方法。 The method for suppressing precipitation of insoluble precipitates produced by the combined use of (A) potassium nitrate and (B) cetylpyridinium chloride in the liquid oral composition according to claim 8, wherein the liquid oral composition is a mouthwash.
PCT/JP2016/054370 2015-02-17 2016-02-16 Oral liquid composition WO2016133063A1 (en)

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