WO2022255124A1 - Liquid composition for oral use - Google Patents

Liquid composition for oral use Download PDF

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Publication number
WO2022255124A1
WO2022255124A1 PCT/JP2022/020907 JP2022020907W WO2022255124A1 WO 2022255124 A1 WO2022255124 A1 WO 2022255124A1 JP 2022020907 W JP2022020907 W JP 2022020907W WO 2022255124 A1 WO2022255124 A1 WO 2022255124A1
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Prior art keywords
liquid oral
component
refreshing feeling
mass ratio
oral composition
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PCT/JP2022/020907
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French (fr)
Japanese (ja)
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博久 田中
妥治 加藤
純一 天川
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ライオン株式会社
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Publication of WO2022255124A1 publication Critical patent/WO2022255124A1/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
    • A61K8/49Cosmetics 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
    • A61K8/73Polysaccharides
    • 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 potassium nitrate and cetylpyridinium chloride that has a stable appearance, gives a refreshing feeling in the oral cavity, and is excellent in use.
  • Potassium nitrate which has an effect of suppressing hypersensitivity, is known as an active ingredient for preventing dentin hypersensitivity in oral compositions.
  • cetylpyridinium chloride is widely used as a disinfectant against halitosis-causing bacteria, particularly in liquid oral compositions.
  • halitosis-causing bacteria particularly in liquid oral compositions.
  • it is effective to combine the two.
  • liquid oral compositions such as mouthwashes, it is effective not only to have good taste but also to give a refreshing feeling in the oral cavity from the viewpoint of continuous use and improvement of effect. A clean feeling is required.
  • potassium nitrate has a metallic taste and cetylpyridinium chloride has a bitter taste, when they are added to a liquid oral composition at the same time, they are perceived as unpleasant, and the feeling of use is significantly impaired. It was not possible to give a refreshing feeling.
  • potassium nitrate has low solubility and may form an insoluble complex with cetylpyridinium chloride. There was a problem of loss of sexuality.
  • Patent Document 1 Japanese Patent Application Laid-Open No. 2016-150912 discloses that when a nonionic surfactant and an amphoteric surfactant are added to an ethanol-free liquid oral composition containing potassium nitrate and cetylpyridinium chloride, an insoluble precipitate is formed. It is proposed that the precipitation of substances is suppressed, the appearance stability is improved, and the feeling of use is that the bitterness is improved, but the refreshing feeling has not been studied and is unknown.
  • Patent Document 2 Japanese Patent Application Laid-Open No.
  • Patent Document 3 Japanese Unexamined Patent Application Publication No. 2012-12303 discloses that when a specific amount of sucralose is added to cetylpyridinium chloride in an oral composition, the unpleasant taste (bitterness, harshness) of cetylpyridinium chloride is eliminated. However, the refreshing feeling was low.
  • the present inventors have found that (C) a nonionic surfactant is added to a liquid oral composition containing (A) potassium nitrate and (B) cetylpyridinium chloride. and (D) when sucralose is blended, the appearance stability is improved even after storage at high or low temperature, and furthermore, the oral cavity is provided with a unique and remarkable refreshing feeling without unpleasant feeling, and the feeling of use is excellent. In addition, they found that the bactericidal effect was high, and came to make the present invention.
  • the metallic taste derived from the component (A) and the bitter taste derived from the component (B) are unpleasant.
  • a complex of the components (A) and (B) is formed to form an insoluble precipitate over time, resulting in a decrease in appearance stability.
  • the nonionic surfactant (C) was added to improve the properties, an off-taste due to the oiliness derived from the component (C) was developed, and the offensive taste was further enhanced.
  • a liquid oral composition containing components (A), (B), (C) and (D) it has an effect of suppressing hypersensitivity and can be preserved even after storage at high or low temperatures. It has a stable appearance, can give a unique and remarkable refreshing feeling in the oral cavity without an unpleasant taste, is excellent in use feeling, and can also give a high bactericidal effect. As shown in Comparative Examples below, when the components (A), (B) and (C) are contained and the component (D) is absent, even if the sweetener saccharin sodium or acesulfame potassium is added, it can be used. The feeling of refreshment after use is low and the lack of sarcasm is inferior (Comparative Examples 3 to 5).
  • the liquid oral composition in which the components (A), (B), (C) and (D) of the present invention are combined has high temperature appearance stability. And it had excellent low temperature appearance stability, excellent refreshing feeling after use, almost no unpleasant taste after use, high bactericidal effect, hypersensitivity suppressing effect and bactericidal effect.
  • Patent Document 1 does not describe the blending of sucralose
  • Patent Documents 2 and 3 do not describe a specific composition example in which cetylpyridinium chloride is blended with potassium nitrate.
  • Patent Documents 1 to 3 which do not focus on or mention a refreshing feeling, the combination of the components (A), (B), (C) and (D) of the present invention gives a unique refreshing feeling, It is unpredictable that securing the appearance stability and imparting a refreshing feeling are compatible.
  • the present invention provides the following liquid oral compositions.
  • (C) a nonionic surfactant and (D) sucralose [2] The liquid composition for oral cavity according to [1], wherein ⁇ (A)+(B) ⁇ /(C) is 2.5 to 25 as a mass ratio.
  • ⁇ (A)+(B) ⁇ /(D) is 30 to 6,000 as a mass ratio.
  • (C) The nonionic surfactant is one or more selected from polyoxyethylene hydrogenated castor oil, polyoxyethylene alkyl ether, polyethylene glycol fatty acid ester, glycerin fatty acid ester and polyoxyethylene polyoxypropylene glycol.
  • a liquid oral composition containing components A) and (B) can be provided.
  • the liquid composition for oral cavity of the present invention has an effect of suppressing hypersensitivity and a bactericidal effect due to the components (A) and (B), and is particularly effective for suppressing and preventing halitosis.
  • Potassium nitrate is an active ingredient for preventing or suppressing dentine hypersensitivity, and has an effect of suppressing hypersensitivity.
  • Potassium nitrate can be used, for example, commercially available products such as Otsuka Chemical Co., Ltd.'s product name; Potassium Nitrate Super Tablets.
  • the content of potassium nitrate is preferably 2 to 8% (% by mass, hereinafter the same), more preferably 3 to 7%, and even more preferably 4 to 6% of the total composition.
  • the amount is 2% or more, the effect of suppressing hypersensitivity is obtained, sufficient appearance stability is obtained, and a moderate metallic taste gives a unique refreshing feeling (hereinafter also abbreviated as "refreshing feeling") There is enough).
  • the appearance stability and refreshing feeling can be sufficiently secured, and it is possible to sufficiently prevent the metallic taste from being perceived as unpleasant.
  • Cetylpyridinium chloride is a cationic bactericide and has a bactericidal effect against intraoral airborne bacteria.
  • cetylpyridinium chloride commercially available products such as cetylpyridinium chloride (trade name, manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.) can be used.
  • the content of cetylpyridinium chloride is preferably 0.01 to 0.1%, more preferably 0.02 to 0.08%, and still more preferably 0.03 to 0.07% of the total composition. be.
  • the blending amount is 0.01% or more, sufficient bactericidal activity and appearance stability can be obtained, and moderate bitterness can sufficiently provide a refreshing feeling.
  • it is 0.1% or less, the appearance stability and refreshing feeling can be sufficiently ensured, and bitterness can be sufficiently prevented from being felt as a sarcasm.
  • Nonionic surfactants are polyoxyethylene hydrogenated castor oil, polyoxyethylene alkyl ether, polyethylene glycol fatty acid ester, glycerin fatty acid ester, in terms of imparting appearance stability and refreshing feeling, and further imparting bactericidal power. , polyoxyethylene polyoxypropylene glycol and the like are preferred. These may be used singly or in combination of two or more.
  • the polyoxyethylene hydrogenated castor oil preferably has an average added molar number of ethylene oxide (E.O. added molar number) of 40 to 100 mol, more preferably 60 to 100 mol.
  • Polyoxyethylene alkyl ethers are available from E.I. O.
  • the number of added moles is 7 to 20 mol, especially 10 to 20 mol, and the number of carbon atoms in the alkyl group is 12 to 22, especially 12 to 18.
  • the polyethylene glycol fatty acid ester preferably has 16 to 20 carbon atoms, such as polyethylene glycol oleate.
  • the glycerol fatty acid ester preferably has 16 to 20 carbon atoms.
  • Polyoxyethylene polyoxypropylene glycol is available from E.I. O. It is preferable that the added mole number is 150 to 200 moles and the average added mole number of propylene oxide is 50 to 100 moles.
  • component (C) the polyoxyethylene hydrogenated castor oil and polyoxyethylene alkyl ether (especially polyoxyethylene cetyl ether) may be used in combination.
  • Nonionic surfactants include, for example, polyoxyethylene hydrogenated castor oil, a trade name of Nikko Chemicals Co., Ltd.; Nikkor HCO; a trade name of Nihon Emulsion Co., Ltd.; is a product name of Aoki Oil Industry Co., Ltd.; Braunon CH-315L; polyethylene glycol oleate is a product name of Nippon Emulsion Co., Ltd.; Trade name: EMALEX GMS, and as polyoxyethylene polyoxypropylene glycol, commercially available products such as ADEKA's trade name: ADEKA (registered trademark) Pluronic can be used.
  • the content of the nonionic surfactant is preferably 0.3 to 0.9%, more preferably 0.4 to 0.8% of the total composition. Appearance stability is fully obtained as a compounding quantity is 0.3% or more. When it is 0.9% or less, a refreshing feeling is sufficiently ensured, and the bactericidal power of the component (B) is sufficiently ensured.
  • Sucralose refers to trichlorogalactosucrose, which is a sucrose derivative in which three hydroxyl groups of sucrose are substituted with chlorine. Sucralose is a sweetener having a sweetness similar to that of sugar. It has the effect of imparting a feeling.
  • sucralose commercially available products such as sucralose (trade name, manufactured by San-Eigen FFI Co., Ltd.) can be used.
  • the content of sucralose is preferably 0.001 to 0.1%, more preferably 0.005 to 0.08%, and still more preferably 0.01 to 0.05% of the total composition.
  • the blending amount is 0.001% or more, a sufficiently refreshing feeling is obtained, and the unpleasant taste derived from the components (A) and (B) is also suppressed.
  • the content is 0.1% or less, the refreshing feeling is sufficiently maintained, and it is possible to sufficiently prevent the sweetness from being felt as an unpleasant taste.
  • this effect is more excellent when the amount ratio of each component is within the range shown below.
  • ⁇ (A) + (B) ⁇ /(C) which indicates the ratio of the total amount of components (A) and (B) to the amount of component (C), is 2.5 to 25 as a mass ratio. It is preferably 3 to 20, still more preferably 6 to 11. Within this range, the appearance stability is particularly excellent.
  • ⁇ (A)+(B) ⁇ /(D) which indicates the ratio of the total amount of components (A) and (B) to the amount of component (D), is 30 to 6,000 as a mass ratio. It is preferably 50 to 1,000, still more preferably 80 to 600. Within this range, the refreshing feeling is particularly excellent, and the unpleasant taste is further suppressed.
  • (A)/(D), which indicates the ratio of the amount of component (A) to the amount of component (D), is preferably 30 to 6,000, more preferably 50 to 2,000 as a mass ratio. More preferably 80-600. Within this range, the refreshing feeling is particularly excellent, and the unpleasant taste is further suppressed.
  • (B)/(D) which indicates the ratio of the amount of component (B) to the amount of component (D), is preferably 0.3 to 60, more preferably 0.5 to 16, as a mass ratio. It is more preferably 0.7-7. Within this range, the refreshing feeling is particularly excellent, and the unpleasant taste is further suppressed. It is more preferable that all of the above-mentioned ratios are within the above-mentioned ranges from the viewpoint of appearance stability, refreshing feeling, and suppression of unpleasant taste.
  • (C)/(B), which indicates the ratio between the amount of component (B) and the amount of component (C), is preferably 4 to 80, more preferably 5 to 60, and still more preferably 6 as a mass ratio. ⁇ 50. Within this range, the bactericidal power of the component (B) is particularly enhanced.
  • the liquid oral composition of the present invention is prepared as a formulation in which ingredients are solubilized or emulsified, such as mouthwash, liquid dentifrice, mouth freshener, concentrated type mouthwash, and especially mouthwash. can be applied.
  • appropriate known components can be blended according to the dosage form as needed.
  • the liquid composition for oral cavity of the present invention does not substantially contain an abrasive, and can be prepared as an abrasive-free formulation.
  • the blending amount is the amount with respect to the entire composition.
  • Wetting agents include, for example, sugar alcohols such as sorbitol and xylitol, and polyhydric alcohols such as glycerin, ethylene glycol and polyethylene glycol.
  • the content of the wetting agent is preferably 2 to 20%.
  • Thickeners include xanthan gum, carrageenan, hydroxyethylcellulose, sodium alginate, polyvinyl alcohol, carboxymethylcellulose, and the like.
  • the blending amount of the thickener is usually 0 to 1%.
  • Anionic surfactants and amphoteric surfactants can be blended as optional surfactants, but they do not have to be blended. When any of these surfactants are blended, it is preferable that the total amount of the surfactants is 0.1 to 4%, particularly 0.1 to 2%, when combined with the blended amount of component (C).
  • Sweeteners include saccharin, saccharin sodium and the like.
  • highly safe water-soluble dyes such as Blue No. 1, Green No. 3, Yellow No. 4 and Red No. 105 can be added.
  • Natural essential oils 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, paracress oil, etc.
  • l-carvone cinnamic aldehyde, orange oil, anethole, 1,8-cineol, methyl salicylate, eugenol, thymol, linalool, limonene, menthone, menthyl acetate, citral, camphor, borneol, pinene, spiranthol
  • Perfume ingredients contained in the above natural essential oils such as ethyl acetate, ethyl butyrate, isoamyl acetate, hexanal, hexenal, methyl anthranilate, ethyl methyl phenylglycidate, benzaldehyde, vanillin, ethyl vanillin, furaneol, maltol , ethyl maltol, gamma/delta decalactone, gamma/delta decalactone, N-ethyl-p-
  • Optional active ingredients include nonionic bactericides such as isopropylmethylphenol, anti-inflammatory agents such as tranexamic acid and allantoin, enzymes such as dextranase, fluorine-containing compounds such as sodium fluoride and sodium monofluorophosphate, water inorganic salts such as sodium chloride and aluminum lactate; vitamins such as ascorbic acid and tocopherol acetate; plant extracts; anticalculus agents and antiplaque agents. Any active ingredient can be added in an effective amount within a range that does not impair the effects of the present invention.
  • nonionic bactericides such as isopropylmethylphenol
  • anti-inflammatory agents such as tranexamic acid and allantoin
  • enzymes such as dextranase
  • fluorine-containing compounds such as sodium fluoride and sodium monofluorophosphate
  • water inorganic salts such as sodium chloride and aluminum lactate
  • vitamins such as ascorbic acid and tocopherol acetate
  • pH adjusters include phthalic acid, phosphoric acid, citric acid, succinic acid, acetic acid, fumaric acid, malic acid and carbonic acid and potassium, sodium and ammonium salts thereof, ribonucleic acid and salts thereof, sodium hydroxide and the like.
  • a combination of citric acid, phosphoric acid and their sodium salts is particularly preferred.
  • the liquid oral composition of the present invention is adjusted to a pH of 4.0 to 9.0, particularly 5.0 to 8.0, especially 5.5 to 7.5 at 25°C. , and a combination of citric acid and sodium citrate, or a combination of sodium dihydrogen phosphate and sodium monohydrogen phosphate can be used as a pH adjuster in this vicinity.
  • Water is generally used as the solvent.
  • the water content is preferably 60% or more, more preferably 60-95%, still more preferably 70-90%.
  • a lower monohydric alcohol having 2 or 3 carbon atoms such as ethanol, propylene glycol, or the like may be blended.
  • the lower monohydric alcohol is suitable for imparting a refreshing feeling during use. It may be absent, and even if the amount is 0%, the refreshing feeling is excellent.
  • Liquid oral compositions mouthwashes having compositions shown in Tables 1 to 4 were prepared by conventional methods and evaluated by the methods shown in (1) to (5) below. The results are also shown in the table.
  • the liquid compositions for oral cavity of Examples had an effect of suppressing hypersensitivity, and the appearance immediately after preparation was clear.
  • the refreshing feeling is a sharp feeling that the inside of the oral cavity is clean and refreshing.
  • This refreshing feeling is due to (C) no peculiar offensive taste derived from nonionic surfactants, (D) refreshing and refreshing sweetness of sucralose, (A) metallic taste of potassium nitrate, and (B) cetylpyridinium chloride. Combined with the bitterness, it has a unique refreshing feeling.
  • the bacterial solution used was prepared by dissolving 30 g of THB (manufactured by BD Japan) as a culture solution in 1 L of purified water, and using Fusobacterium nucleatum ATCC 10953 strain as oral resident bacteria, anaerobic at 37 ° C. PBS was added to prepare a solution cultured for one day under the conditions (5% by volume carbon dioxide, 95% by volume nitrogen) so that the transmittance at 550 nm was 1.0.
  • SCDLP medium manufactured by BD Japan
  • Viable count is less than 10 4 ⁇ : Viable count is 10 4 or more and less than 10 5 ⁇ : Viable count is 10 5 or more and less than 10 7 ⁇ : Viable count is 10 7 or more
  • [Prescription Example 1] Mouthwash (A) Potassium nitrate 5.0 (B) cetylpyridinium chloride 0.03 (C) Polyoxyethylene hydrogenated castor oil 100 0.6 (D) Sucralose 0.02 Ethanol 10.0 Citric acid 0.01 Sodium citrate 0.3 Xylitol 3.0 Glycerin 5.0 Propylene glycol 5.0 Perfume 0.2 Purified water 70.84 Total 100% pH; 6.2 Mass ratio of ⁇ (A) + (B) ⁇ /(C); 8.4 ⁇ (A) + (B) ⁇ /(D) mass ratio; 251.5 (A) / (D) mass ratio; 250.0 (B) / (D) mass ratio; 1.5 Mass ratio of (C)/(B); 20.0 Appearance stability at high temperature; ⁇ , Appearance stability at low temperature; Refreshing feeling after use;
  • [Prescription Example 2] Mouthwash (A) Potassium nitrate 5.0 (B) cetylpyridinium chloride 0.05 (C) Polyoxyethylene hydrogenated castor oil 100 0.3 (D) Sucralose 0.02 Citric acid 0.01 Sodium citrate 0.3 Sorbit solution (70%) 10.0 Glycerin 5.0 Propylene glycol 5.0 Perfume 0.2 Purified water 74.12 Total 100% pH; 6.2 Mass ratio of ⁇ (A) + (B) ⁇ /(C); 16.8 ⁇ (A) + (B) ⁇ /(D) mass ratio; 251.5 (A) / (D) mass ratio; 250.0 Mass ratio of (B)/(D); 2.5 Mass ratio of (C)/(B); 6.0 High temperature appearance stability; ⁇ , Low temperature appearance stability; ⁇ , Refreshing feeling after use;
  • Mouthwash A) Potassium nitrate 5.0
  • B cetylpyridinium chloride 0.05
  • C Polyoxyethylene hydrogenated castor oil 100 0.4
  • D Sucralose 0.01 Citric acid 0.01 Sodium citrate 0.3 Sorbit solution (70%) 7.0 Glycerin 3.0 Propylene glycol 10.0 Perfume 0.2 Purified water 74.03 Total 100% pH; 6.2 Mass ratio of ⁇ (A) + (B) ⁇ /(C); 12.6 Mass ratio of ⁇ (A) + (B) ⁇ /(D); 505.0 (A) / (D) mass ratio; 500.0 Mass ratio of (B)/(D); 5.0 Mass ratio of (C)/(B); 8.0 Appearance stability at high temperature; ⁇ , Appearance stability at low temperature; Refreshing feeling after use;

Abstract

Provided is a liquid composition for oral use that has appearance stability after storage at a high temperature or a low temperature; that is capable of imparting a unique and prominent refreshing sensation without any unpleasant taste; has excellent texture; and contains (A) potassium nitrate and (B) cetylpyridinium chloride, which have strong bactericidal effects. This liquid composition for oral use contains (A) potassium nitrate, (B) cetylpyridinium chloride, (C) a nonionic surfactant, and (D) sucralose.

Description

液体口腔用組成物Liquid oral composition
 本発明は、外観安定性を有し、かつ口腔内にスッキリ感を与え、使用感に優れる硝酸カリウム及び塩化セチルピリジニウム含有の液体口腔用組成物に関する。 The present invention relates to a liquid oral composition containing potassium nitrate and cetylpyridinium chloride that has a stable appearance, gives a refreshing feeling in the oral cavity, and is excellent in use.
 口腔用組成物において、象牙質知覚過敏症予防の有効成分として、知覚過敏抑制効果を有する硝酸カリウムが知られている。また、特に液体口腔用組成物では、口臭原因菌に対する殺菌剤として、塩化セチルピリジニウムが広く用いられる。知覚過敏症予防機能と口臭原因菌に対する殺菌機能を兼ね備えるには、この両者を配合することが効果的である。
 ところで、洗口剤等の液体口腔用組成物では、継続使用や効果向上の点でも、味の良さだけでなく、口腔内にスッキリとした使用感を与えることが有効であり、特に使用感としてスッキリ感が求められている。
Potassium nitrate, which has an effect of suppressing hypersensitivity, is known as an active ingredient for preventing dentin hypersensitivity in oral compositions. Moreover, cetylpyridinium chloride is widely used as a disinfectant against halitosis-causing bacteria, particularly in liquid oral compositions. In order to combine the function of preventing hypersensitivity and the function of sterilizing bad breath-causing bacteria, it is effective to combine the two.
By the way, in liquid oral compositions such as mouthwashes, it is effective not only to have good taste but also to give a refreshing feeling in the oral cavity from the viewpoint of continuous use and improvement of effect. A clean feeling is required.
 しかしながら、硝酸カリウムは金属味、塩化セチルピリジニウムは苦味を有しているため、これらを同時に液体口腔用組成物に配合すると、これらが嫌味として感じられ、使用感が顕著に損なわれるという問題もあり、スッキリ感を与えることはできなかった。
 一方、硝酸カリウムは溶解性が低いことに加え、塩化セチルピリジニウムと不溶性の複合体を形成することがあるため、これらを同時に液体口腔用組成物に配合すると保存時に不溶性沈殿物が析出し、外観安定性が損なわれるという問題があった。
However, since potassium nitrate has a metallic taste and cetylpyridinium chloride has a bitter taste, when they are added to a liquid oral composition at the same time, they are perceived as unpleasant, and the feeling of use is significantly impaired. It was not possible to give a refreshing feeling.
On the other hand, potassium nitrate has low solubility and may form an insoluble complex with cetylpyridinium chloride. There was a problem of loss of sexuality.
 特許文献1(特開2016-150912号公報)は、硝酸カリウム及び塩化セチルピリジニウムが配合されたエタノール無配合の液体口腔用組成物に非イオン性界面活性剤及び両性界面活性剤を配合すると、不溶性沈殿物の析出が抑制されて外観安定性が改善し、また、使用感として苦味が改善することを提案しているが、スッキリ感は検討されておらず不明である。
 特許文献2(特開2017-141178号公報)は、硝酸カリウム含有の歯磨剤組成物にα-オレフィンスルホン酸塩及びスクラロースを配合することで、発泡性能が改善し、使用感として塩味、苦味、えぐみも改善することを提案しているが、スッキリ感は不明である。特許文献3(特開2012-12303号公報)は、塩化セチルピリジニウムに対してスクラロースを特定量で口腔用組成物に配合すると、塩化セチルピリジニウムの不快な味(苦味、えぐみ)が解消することを開示し、スッキリ感について何ら言及されていないが、スッキリ感は低いものであった。
Patent Document 1 (Japanese Patent Application Laid-Open No. 2016-150912) discloses that when a nonionic surfactant and an amphoteric surfactant are added to an ethanol-free liquid oral composition containing potassium nitrate and cetylpyridinium chloride, an insoluble precipitate is formed. It is proposed that the precipitation of substances is suppressed, the appearance stability is improved, and the feeling of use is that the bitterness is improved, but the refreshing feeling has not been studied and is unknown.
Patent Document 2 (Japanese Patent Application Laid-Open No. 2017-141178) describes that by blending α-olefin sulfonate and sucralose in a dentifrice composition containing potassium nitrate, foaming performance is improved, and the feeling of use is salty, bitter, and harsh. It is also proposed to improve it, but the feeling of refreshment is unknown. Patent Document 3 (Japanese Unexamined Patent Application Publication No. 2012-12303) discloses that when a specific amount of sucralose is added to cetylpyridinium chloride in an oral composition, the unpleasant taste (bitterness, harshness) of cetylpyridinium chloride is eliminated. However, the refreshing feeling was low.
特開2016-150912号公報JP 2016-150912 A 特開2017-141178号公報JP 2017-141178 A 特開2012-12303号公報Japanese Patent Application Laid-Open No. 2012-12303
 本発明は、上記事情に鑑みなされたもので、外観安定性を有し、かつ口腔内にスッキリ感を与え、使用感に優れる硝酸カリウム及び塩化セチルピリジニウム含有の液体口腔用組成物を提供することを目的とする。 It is an object of the present invention to provide a liquid oral composition containing potassium nitrate and cetylpyridinium chloride, which has a stable appearance, gives a refreshing feeling in the oral cavity, and is excellent in use. aim.
 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)硝酸カリウム及び(B)塩化セチルピリジニウムを配合した液体口腔用組成物に、(C)ノニオン性界面活性剤を配合し、かつ(D)スクラロースを配合すると、高温又は低温で保存後も外観安定性が良好となり、しかも、口腔内に嫌味もない独特かつ顕著なスッキリ感を与えることができ、使用感に優れること、また、殺菌効果も高いことを知見し、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 (C) a nonionic surfactant is added to a liquid oral composition containing (A) potassium nitrate and (B) cetylpyridinium chloride. and (D) when sucralose is blended, the appearance stability is improved even after storage at high or low temperature, and furthermore, the oral cavity is provided with a unique and remarkable refreshing feeling without unpleasant feeling, and the feeling of use is excellent. In addition, they found that the bactericidal effect was high, and came to make the present invention.
 更に詳述すると、上述したように、(A)及び(B)成分を併用して液体口腔用組成物に配合すると、(A)成分由来の金属味、(B)成分由来の苦味等が嫌味として感じられ、味が悪くなり、また、(A)及び(B)成分の複合体が形成されて不溶性析出物が経時で発生し、外観安定性が低下するという問題が生じ、更に、外観安定性を改善するために、(C)ノニオン性界面活性剤を添加すると、(C)成分由来の油っぽさに起因する異味が発現し、嫌味がさらに強くなった。しかし、(A)、(B)及び(C)成分に(D)成分を組み合わせて配合すると、上記嫌味が感じられることもなく、高温又は低温で保存後も外観安定性を確保しながら、口腔内に嫌味もない独特かつ顕著なスッキリ感を付与することができた。
 この場合、本発明においては、(D)成分が持つ甘味だけではなく、それに加えて、(D)成分によって、(A)成分由来の金属味及び(B)成分由来の苦味がマスキングされて共に適度に抑えられ、また更に、(A)及び(B)成分の併用系に(C)成分が添加されることで生じる特有の嫌味がマスキングされることで、上記嫌味のない独特なスッキリ感を特異的に与えることができる。
 したがって、本発明では、(A)、(B)、(C)及び(D)成分を含有する液体口腔用組成物とすることによって、知覚過敏抑制効果を有すると共に、高温又は低温で保存後も外観安定性を有し、かつ口腔内に嫌味もない独特かつ顕著なスッキリ感を与えることができ、使用感に優れ、また、高い殺菌効果を与えることもできる。
 後述の比較例にも示すように、(A)、(B)及び(C)成分を含有し、(D)成分を欠く場合は、甘味剤のサッカリンナトリウム又はアセスルファムカリウムが添加されていても、使用後のスッキリ感が低く、嫌味のなさが劣り(比較例3~5)、また、(D)成分を含有していても、(A)又は(B)成分を欠く場合は、使用後のスッキリ感が低かった(比較例1、2)。これに対して、後述の実施例に示すように、本発明の(A)、(B)、(C)及び(D)成分が組み合わせて配合された液体口腔用組成物は、高温外観安定性及び低温外観安定性が優れ、かつ使用後のスッキリ感が優れ、使用後の嫌味がほとんどなく、高い殺菌効果を有し、また、知覚過敏抑制効果及び殺菌効果を有していた。
 なお、特許文献1は、スクラロースの配合について記載がなく、また、特許文献2、3は、具体的に硝酸カリウムに塩化セチルピリジニウムが配合された組成例が記載されていない。スッキリ感について着目しておらず言及されてもいない特許文献1~3から、本発明の(A)、(B)、(C)及び(D)成分を組み合わせることによって独特なスッキリ感を与え、外観安定性の確保及びスッキリ感の付与が両立することは予測し得ない。
More specifically, as described above, when the components (A) and (B) are used in combination in a liquid oral composition, the metallic taste derived from the component (A) and the bitter taste derived from the component (B) are unpleasant. In addition, a complex of the components (A) and (B) is formed to form an insoluble precipitate over time, resulting in a decrease in appearance stability. When the nonionic surfactant (C) was added to improve the properties, an off-taste due to the oiliness derived from the component (C) was developed, and the offensive taste was further enhanced. However, when the (A), (B) and (C) components are combined with the (D) component, the above-mentioned unpleasant taste is not felt, and the oral cavity is maintained while maintaining the appearance stability even after storage at high or low temperatures. It was possible to impart a unique and remarkable refreshing feeling without any sarcasm inside.
In this case, in the present invention, not only the sweetness of the component (D), but also the metallic taste derived from the component (A) and the bitter taste derived from the component (B) are masked by the component (D). Moderately suppressed, and furthermore, by masking the peculiar unpleasant taste caused by adding the (C) component to the combined system of the (A) and (B) components, a unique refreshing feeling without the above unpleasant taste. specific can be given.
Therefore, in the present invention, by making a liquid oral composition containing components (A), (B), (C) and (D), it has an effect of suppressing hypersensitivity and can be preserved even after storage at high or low temperatures. It has a stable appearance, can give a unique and remarkable refreshing feeling in the oral cavity without an unpleasant taste, is excellent in use feeling, and can also give a high bactericidal effect.
As shown in Comparative Examples below, when the components (A), (B) and (C) are contained and the component (D) is absent, even if the sweetener saccharin sodium or acesulfame potassium is added, it can be used. The feeling of refreshment after use is low and the lack of sarcasm is inferior (Comparative Examples 3 to 5). The feeling was low (Comparative Examples 1 and 2). On the other hand, as shown in the examples below, the liquid oral composition in which the components (A), (B), (C) and (D) of the present invention are combined has high temperature appearance stability. And it had excellent low temperature appearance stability, excellent refreshing feeling after use, almost no unpleasant taste after use, high bactericidal effect, hypersensitivity suppressing effect and bactericidal effect.
Patent Document 1 does not describe the blending of sucralose, and Patent Documents 2 and 3 do not describe a specific composition example in which cetylpyridinium chloride is blended with potassium nitrate. From Patent Documents 1 to 3, which do not focus on or mention a refreshing feeling, the combination of the components (A), (B), (C) and (D) of the present invention gives a unique refreshing feeling, It is unpredictable that securing the appearance stability and imparting a refreshing feeling are compatible.
 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)硝酸カリウム、
(B)塩化セチルピリジニウム、
(C)ノニオン性界面活性剤
及び
(D)スクラロース
を含有する液体口腔用組成物。
〔2〕
 {(A)+(B)}/(C)が質量比として2.5~25である〔1〕記載の液体口腔用組成物。
〔3〕
 {(A)+(B)}/(D)が質量比として30~6,000である〔1〕又は〔2〕記載の液体口腔用組成物。
〔4〕
 (A)成分を2~8質量%、(B)成分を0.01~0.1質量%、(C)成分を0.3~0.9質量%、(D)成分を0.001~0.1質量%含有する〔1〕~〔3〕のいずれかに記載の液体口腔用組成物。
〔5〕
 (C)ノニオン性界面活性剤が、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、ポリエチレングリコール脂肪酸エステル、グリセリン脂肪酸エステル及びポリオキシエチレンポリオキシプロピレングリコールから選ばれる1種又は2種以上である〔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。
Accordingly, the present invention provides the following liquid oral compositions.
[1]
(A) potassium nitrate,
(B) cetylpyridinium chloride;
A liquid oral composition containing (C) a nonionic surfactant and (D) sucralose.
[2]
The liquid composition for oral cavity according to [1], wherein {(A)+(B)}/(C) is 2.5 to 25 as a mass ratio.
[3]
The liquid composition for oral cavity according to [1] or [2], wherein {(A)+(B)}/(D) is 30 to 6,000 as a mass ratio.
[4]
2 to 8% by mass of component (A), 0.01 to 0.1% by mass of component (B), 0.3 to 0.9% by mass of component (C), and 0.001 to 0.001% of component (D) The liquid oral composition according to any one of [1] to [3] containing 0.1% by mass.
[5]
(C) The nonionic surfactant is one or more selected from polyoxyethylene hydrogenated castor oil, polyoxyethylene alkyl ether, polyethylene glycol fatty acid ester, glycerin fatty acid ester and polyoxyethylene polyoxypropylene glycol. The liquid oral composition according to any one of [1] to [4].
[6]
The liquid oral composition according to any one of [1] to [5], which is a mouthwash.
 本発明によれば、高温又は低温で保存後も外観安定性を有し、かつ口腔内に嫌味もない独特かつ顕著なスッキリ感を付与することができ、使用感に優れ、殺菌効果も高い(A)及び(B)成分含有の液体口腔用組成物を提供できる。本発明の液体口腔用組成物は、(A)及び(B)成分による知覚過敏抑制効果及び殺菌効果を有し、特に口臭の抑制及び予防に有効である。 According to the present invention, it has a stable appearance even after storage at high or low temperatures, and can impart a unique and remarkable refreshing feeling that does not have an unpleasant taste in the oral cavity. A liquid oral composition containing components A) and (B) can be provided. The liquid composition for oral cavity of the present invention has an effect of suppressing hypersensitivity and a bactericidal effect due to the components (A) and (B), and is particularly effective for suppressing and preventing halitosis.
 以下、本発明につき更に詳述する。
 (A)硝酸カリウムは、象牙質知覚過敏症の予防又は抑制の有効成分であり、知覚過敏抑制効果を有する。
 硝酸カリウムは、例えば大塚化学(株)製の商品名;硝酸カリウムスーパータブレット等の市販のものを使用することができる。
The present invention will be described in further detail below.
(A) Potassium nitrate is an active ingredient for preventing or suppressing dentine hypersensitivity, and has an effect of suppressing hypersensitivity.
Potassium nitrate can be used, for example, commercially available products such as Otsuka Chemical Co., Ltd.'s product name; Potassium Nitrate Super Tablets.
 (A)硝酸カリウムの配合量は、組成物全体の2~8%(質量%、以下同様)が好ましく、より好ましくは3~7%、更に好ましくは4~6%である。配合量が2%以上であると、知覚過敏抑制効果が得られると共に、十分な外観安定性が得られ、かつ適度な金属味によって独特なスッキリ感(以下、「スッキリ感」と略記することもある)が十分に得られる。8%以下であると、外観安定性及びスッキリ感が十分に確保され、また、金属味が嫌味として感じられるのを十分に防止できる。 (A) The content of potassium nitrate is preferably 2 to 8% (% by mass, hereinafter the same), more preferably 3 to 7%, and even more preferably 4 to 6% of the total composition. When the amount is 2% or more, the effect of suppressing hypersensitivity is obtained, sufficient appearance stability is obtained, and a moderate metallic taste gives a unique refreshing feeling (hereinafter also abbreviated as "refreshing feeling") There is enough). When it is 8% or less, the appearance stability and refreshing feeling can be sufficiently secured, and it is possible to sufficiently prevent the metallic taste from being perceived as unpleasant.
 (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効果を有する。
 塩化セチルピリジニウムは、例えば富士フィルム和光純薬(株)製の商品名;塩化セチルピリジニウム等の市販のものを使用することができる。
(B) Cetylpyridinium chloride is a cationic bactericide and has a bactericidal effect against intraoral airborne bacteria.
As cetylpyridinium chloride, commercially available products such as cetylpyridinium chloride (trade name, manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.) can be used.
 (B)塩化セチルピリジニウムの配合量は、組成物全体の0.01~0.1%が好ましく、より好ましくは0.02~0.08%、更に好ましくは0.03~0.07%である。配合量が0.01%以上であると、十分な殺菌力、外観安定性が得られ、かつ適度な苦味によってスッキリ感が十分に得られる。0.1%以下であると、外観安定性及びスッキリ感が十分に確保され、また、苦味が嫌味として感じられるのを十分に防止できる。 (B) The content of cetylpyridinium chloride is preferably 0.01 to 0.1%, more preferably 0.02 to 0.08%, and still more preferably 0.03 to 0.07% of the total composition. be. When the blending amount is 0.01% or more, sufficient bactericidal activity and appearance stability can be obtained, and moderate bitterness can sufficiently provide a refreshing feeling. When it is 0.1% or less, the appearance stability and refreshing feeling can be sufficiently ensured, and bitterness can be sufficiently prevented from being felt as a sarcasm.
 (C)ノニオン性界面活性剤は、外観安定性及びスッキリ感の付与、更には殺菌力の付与の点で、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、ポリエチレングリコール脂肪酸エステル、グリセリン脂肪酸エステル、ポリオキシエチレンポリオキシプロピレングリコール等が好ましい。これらは1種単独でも2種以上を組み合わせて使用してもよい。
 ポリオキシエチレン硬化ヒマシ油は、エチレンオキサイドの平均付加モル数(E.O.付加モル数)が40~100モル、特に60~100モルのものが好ましい。
 ポリオキシエチレンアルキルエーテルは、E.O.付加モル数が7~20モル、特に10~20モルであり、アルキル基の炭素数が12~22、特に12~18のものが好ましい。
 ポリエチレングリコール脂肪酸エステルは、脂肪酸の炭素数が16~20のものが好ましく、オレイン酸ポリエチレングリコール等が挙げられる。
 グリセリン脂肪酸エステルは、脂肪酸の炭素数が16~20のものが好ましい。
 ポリオキシエチレンポリオキシプロピレングリコールは、E.O.付加モル数150~200モルであり、プロピレンオキサイドの平均付加モル数が50~100モルであるものが好ましい。
 なお、(C)成分として、上記ポリオキシエチレン硬化ヒマシ油とポリオキシエチレンアルキルエーテル(特にポリオキシエチレンセチルエーテル)とを併用してもよい。
 ノニオン性界面活性剤は、例えば、ポリオキシエチレン硬化ヒマシ油としては日光ケミカルズ(株)製の商品名;ニッコール HCO、日本エマルジョン(株)製の商品名;エマレックスHC、ポリオキシエチレンアルキルエーテルとしては青木油脂工業(株)製の商品名;ブラウノンCH-315L、オレイン酸ポリエチレングリコールとしては日本エマルジョン(株)製の商品名;EMALEX OE-10、グリセリン脂肪酸エステルとしては日本エマルジョン(株)製の商品名;EMALEX GMS、ポリオキシエチレンポリオキシプロピレングリコールとしてはADEKA社製の商品名;アデカ(登録商標)プルロニック等の市販のものを使用することができる。
(C) Nonionic surfactants are polyoxyethylene hydrogenated castor oil, polyoxyethylene alkyl ether, polyethylene glycol fatty acid ester, glycerin fatty acid ester, in terms of imparting appearance stability and refreshing feeling, and further imparting bactericidal power. , polyoxyethylene polyoxypropylene glycol and the like are preferred. These may be used singly or in combination of two or more.
The polyoxyethylene hydrogenated castor oil preferably has an average added molar number of ethylene oxide (E.O. added molar number) of 40 to 100 mol, more preferably 60 to 100 mol.
Polyoxyethylene alkyl ethers are available from E.I. O. The number of added moles is 7 to 20 mol, especially 10 to 20 mol, and the number of carbon atoms in the alkyl group is 12 to 22, especially 12 to 18.
The polyethylene glycol fatty acid ester preferably has 16 to 20 carbon atoms, such as polyethylene glycol oleate.
The glycerol fatty acid ester preferably has 16 to 20 carbon atoms.
Polyoxyethylene polyoxypropylene glycol is available from E.I. O. It is preferable that the added mole number is 150 to 200 moles and the average added mole number of propylene oxide is 50 to 100 moles.
As component (C), the polyoxyethylene hydrogenated castor oil and polyoxyethylene alkyl ether (especially polyoxyethylene cetyl ether) may be used in combination.
Nonionic surfactants include, for example, polyoxyethylene hydrogenated castor oil, a trade name of Nikko Chemicals Co., Ltd.; Nikkor HCO; a trade name of Nihon Emulsion Co., Ltd.; is a product name of Aoki Oil Industry Co., Ltd.; Braunon CH-315L; polyethylene glycol oleate is a product name of Nippon Emulsion Co., Ltd.; Trade name: EMALEX GMS, and as polyoxyethylene polyoxypropylene glycol, commercially available products such as ADEKA's trade name: ADEKA (registered trademark) Pluronic can be used.
 (C)ノニオン性界面活性剤の配合量は、組成物全体の0.3~0.9%が好ましく、より好ましくは0.4~0.8%である。配合量が0.3%以上であると、外観安定性が十分に得られる。0.9%以下であると、スッキリ感が十分に確保され、また、(B)成分による殺菌力が十分に確保される。 (C) The content of the nonionic surfactant is preferably 0.3 to 0.9%, more preferably 0.4 to 0.8% of the total composition. Appearance stability is fully obtained as a compounding quantity is 0.3% or more. When it is 0.9% or less, a refreshing feeling is sufficiently ensured, and the bactericidal power of the component (B) is sufficiently ensured.
 (D)スクラロースは、トリクロロガラクトスクロースのことを指し、スクロースの水酸基3箇所が塩素に置き換わったスクロース誘導体である。スクラロースは、砂糖に似た甘みを持つ甘味剤であるが、本発明では、(C)スクラロースが、(A)、(B)及び(C)成分と組み合わせることで、使用後の口腔内にスッキリ感を付与する作用を奏する。
 スクラロースは、三栄源エフエフアイ(株)製の商品名;スクラロース等の市販のものを使用することができる。
(D) Sucralose refers to trichlorogalactosucrose, which is a sucrose derivative in which three hydroxyl groups of sucrose are substituted with chlorine. Sucralose is a sweetener having a sweetness similar to that of sugar. It has the effect of imparting a feeling.
As sucralose, commercially available products such as sucralose (trade name, manufactured by San-Eigen FFI Co., Ltd.) can be used.
 (D)スクラロースの配合量は、組成物全体の0.001~0.1%が好ましく、より好ましくは0.005~0.08%、更に好ましくは0.01~0.05%である。配合量が0.001%以上であると、十分にスッキリ感が得られ、(A)及び(B)成分由来の嫌味も抑制される。0.1%以下であると、スッキリ感が十分に維持され、また、甘味が嫌味として感じられるのも十分に防止できる。 (D) The content of sucralose is preferably 0.001 to 0.1%, more preferably 0.005 to 0.08%, and still more preferably 0.01 to 0.05% of the total composition. When the blending amount is 0.001% or more, a sufficiently refreshing feeling is obtained, and the unpleasant taste derived from the components (A) and (B) is also suppressed. When the content is 0.1% or less, the refreshing feeling is sufficiently maintained, and it is possible to sufficiently prevent the sweetness from being felt as an unpleasant taste.
 本発明では、各成分の量比が下記に示す範囲であると、本効果がより優れる。
 (A)及び(B)成分の合計配合量と(C)成分の配合量との量比を示す{(A)+(B)}/(C)は、質量比として2.5~25が好ましく、より好ましくは3~20、更に好ましくは6~11である。この範囲内であると、特に外観安定性がより優れる。
In the present invention, this effect is more excellent when the amount ratio of each component is within the range shown below.
{(A) + (B)}/(C), which indicates the ratio of the total amount of components (A) and (B) to the amount of component (C), is 2.5 to 25 as a mass ratio. It is preferably 3 to 20, still more preferably 6 to 11. Within this range, the appearance stability is particularly excellent.
 (A)及び(B)成分の合計配合量と(D)成分の配合量との量比を示す{(A)+(B)}/(D)は、質量比として30~6,000が好ましく、より好ましくは50~1,000、更に好ましくは80~600である。この範囲内であると、特にスッキリ感がより優れ、また、嫌味がより抑制される。
 (A)成分の配合量と(D)成分の配合量との量比を示す(A)/(D)は、質量比として30~6,000が好ましく、より好ましくは50~2,000、更に好ましくは80~600である。この範囲内であると、特にスッキリ感がより優れ、また、嫌味がより抑制される。
 (B)成分の配合量と(D)成分の配合量との量比を示す(B)/(D)は、質量比として0.3~60が好ましく、より好ましくは0.5~16、更に好ましくは0.7~7である。この範囲内であると、特にスッキリ感がより優れ、また、嫌味がより抑制される。
 上記量比全てが、それぞれ上記の範囲内であると、外観安定性及びスッキリ感、更には嫌味抑制の点で、一層好ましい。
{(A)+(B)}/(D), which indicates the ratio of the total amount of components (A) and (B) to the amount of component (D), is 30 to 6,000 as a mass ratio. It is preferably 50 to 1,000, still more preferably 80 to 600. Within this range, the refreshing feeling is particularly excellent, and the unpleasant taste is further suppressed.
(A)/(D), which indicates the ratio of the amount of component (A) to the amount of component (D), is preferably 30 to 6,000, more preferably 50 to 2,000 as a mass ratio. More preferably 80-600. Within this range, the refreshing feeling is particularly excellent, and the unpleasant taste is further suppressed.
(B)/(D), which indicates the ratio of the amount of component (B) to the amount of component (D), is preferably 0.3 to 60, more preferably 0.5 to 16, as a mass ratio. It is more preferably 0.7-7. Within this range, the refreshing feeling is particularly excellent, and the unpleasant taste is further suppressed.
It is more preferable that all of the above-mentioned ratios are within the above-mentioned ranges from the viewpoint of appearance stability, refreshing feeling, and suppression of unpleasant taste.
 (B)成分の配合量と(C)成分の配合量との量比を示す(C)/(B)は、質量比として4~80が好ましく、より好ましくは5~60、更に好ましくは6~50である。この範囲内であると、特に(B)成分による殺菌力がより発揮される。 (C)/(B), which indicates the ratio between the amount of component (B) and the amount of component (C), is preferably 4 to 80, more preferably 5 to 60, and still more preferably 6 as a mass ratio. ~50. Within this range, the bactericidal power of the component (B) is particularly enhanced.
 本発明の液体口腔用組成物は、配合成分が可溶化又は乳化された製剤として、例えば洗口剤、液体歯磨、口中清涼剤、濃縮タイプ洗口剤等の剤型、特に洗口剤に調製し、適用することができる。この場合、上記成分以外に、その剤型に応じて適宜な公知成分を必要に応じて配合することができ、例えば、湿潤剤、増粘剤、(C)ノニオン性界面活性剤以外の界面活性剤、(D)スクラロース以外の甘味剤、着色料、香料、(A)硝酸カリウム及び(B)塩化セチルピリジニウム以外の有効成分、pH調整剤、溶剤等を配合できる。なお、本発明の液体口腔用組成物は、研磨剤を実質的に含まず、研磨剤無配合の製剤とすることができる。
 本発明では、歯磨剤のようなペースト状製剤に比べて、配合成分由来の金属味、苦味等が比較的強く発現し、嫌味として感じられる傾向にある洗口剤等の液体口腔用組成物において、嫌味もない顕著なスッキリ感を与えることができる。
 以下、配合量は組成物全体に対する量である。
The liquid oral composition of the present invention is prepared as a formulation in which ingredients are solubilized or emulsified, such as mouthwash, liquid dentifrice, mouth freshener, concentrated type mouthwash, and especially mouthwash. can be applied. In this case, in addition to the above components, appropriate known components can be blended according to the dosage form as needed. (D) a sweetener other than sucralose, a coloring agent, a flavoring agent, an active ingredient other than (A) potassium nitrate and (B) cetylpyridinium chloride, a pH adjuster, a solvent, and the like. In addition, the liquid composition for oral cavity of the present invention does not substantially contain an abrasive, and can be prepared as an abrasive-free formulation.
In the present invention, compared to paste-like preparations such as dentifrices, in liquid oral compositions such as mouthwashes, which tend to exhibit a relatively strong metallic taste, bitterness, etc. derived from the ingredients and be perceived as a disgusting taste. , It can give a remarkable refreshing feeling without sarcasm.
Hereinafter, the blending amount is the amount with respect to the entire composition.
 湿潤剤は、例えばソルビトール、キシ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。湿潤剤の配合量は、2~20%が好ましい。 Wetting agents include, for example, sugar alcohols such as sorbitol and xylitol, and polyhydric alcohols such as glycerin, ethylene glycol and polyethylene glycol. The content of the wetting agent is preferably 2 to 20%.
 増粘剤は、キサンタンガム、カラギーナン、ヒドロキシエチルセルロース、アルギン酸ナトリウム、ポリビニルアルコール、カルボキシメチルセルロース等が挙げられる。増粘剤の配合量は、通常0~1%である。 Thickeners include xanthan gum, carrageenan, hydroxyethylcellulose, sodium alginate, polyvinyl alcohol, carboxymethylcellulose, and the like. The blending amount of the thickener is usually 0 to 1%.
 任意の界面活性剤は、アニオン性界面活性剤、両性界面活性剤を配合することができるが、配合しなくてもよい。これら任意の界面活性剤を配合する場合は、(C)成分の配合量と合算し、界面活性剤の総量が0.1~4%、特に0.1~2%であることが好ましい。 Anionic surfactants and amphoteric surfactants can be blended as optional surfactants, but they do not have to be blended. When any of these surfactants are blended, it is preferable that the total amount of the surfactants is 0.1 to 4%, particularly 0.1 to 2%, when combined with the blended amount of component (C).
 甘味剤は、サッカリン、サッカリンナトリウム等が挙げられる。
 着色料は、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を添加することができる。
Sweeteners include saccharin, saccharin sodium and the like.
As the colorant, highly safe water-soluble dyes such as Blue No. 1, Green No. 3, Yellow No. 4 and Red No. 105 can be added.
 香料は、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が挙げられる。これらは、1種単独で又は2種以上を使用することができる。香料の配合量は、通常、0.00001~3%である。 Natural essential oils 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, paracress oil, etc. , and l-menthol, l-carvone, cinnamic aldehyde, orange oil, anethole, 1,8-cineol, methyl salicylate, eugenol, thymol, linalool, limonene, menthone, menthyl acetate, citral, camphor, borneol, pinene, spiranthol Perfume ingredients contained in the above natural essential oils such as ethyl acetate, ethyl butyrate, isoamyl acetate, hexanal, hexenal, methyl anthranilate, ethyl methyl phenylglycidate, benzaldehyde, vanillin, ethyl vanillin, furaneol, maltol , ethyl maltol, gamma/delta decalactone, gamma/delta decalactone, N-ethyl-p-menthane-3-carboxamide, menthyl lactate, ethylene glycol-l-menthyl carbonate and other fragrance ingredients, and furthermore, some Mixed flavors such as apple, banana, strawberry, blueberry, melon, peach, pineapple, grape, muscat, wine, cherry, squash, coffee, brandy, yogurt, etc., which are obtained by combining flavoring ingredients and natural essential oils. These can be used individually by 1 type or 2 types or more. The blending amount of perfume is usually 0.00001 to 3%.
 任意の有効成分は、イソプロピルメチルフェノール等の非イオン性殺菌剤、トラネキサム酸、アラントイン等の抗炎症剤、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素含有化合物、水溶性リン酸化合物、塩化ナトリウム、乳酸アルミニウム等の無機塩類、アスコルビン酸、酢酸トコフェロール等のビタミン類、植物抽出物、歯石防止剤、歯垢防止剤が挙げられる。任意の有効成分は、本発明の効果を妨げない範囲で有効量配合できる。 Optional active ingredients include nonionic bactericides such as isopropylmethylphenol, anti-inflammatory agents such as tranexamic acid and allantoin, enzymes such as dextranase, fluorine-containing compounds such as sodium fluoride and sodium monofluorophosphate, water inorganic salts such as sodium chloride and aluminum lactate; vitamins such as ascorbic acid and tocopherol acetate; plant extracts; anticalculus agents and antiplaque agents. Any active ingredient can be added in an effective amount within a range that does not impair the effects of the present invention.
 pH調整剤は、フタル酸、リン酸、クエン酸、コハク酸、酢酸、フマル酸、リンゴ酸及び炭酸並びにそれらのカリウム塩、ナトリウム塩及びアンモニウム塩、リボ核酸及びその塩類、更に水酸化ナトリウムなどの1種又は2種以上を用いることができ、特にクエン酸、リン酸とそれらのナトリウム塩とを組み合わせたものが好ましい。
 本発明の液体口腔用組成物は、25℃におけるpHを4.0~9.0、特に5.0~8.0、とりわけ5.5~7.5に調整することが、本効果発現性の点からも好ましく、この付近のpH調整剤としてクエン酸とクエン酸ナトリウム、あるいはリン酸二水素ナトリウムとリン酸一水素ナトリウムを組み合わせたものを用いることができる。
pH adjusters include phthalic acid, phosphoric acid, citric acid, succinic acid, acetic acid, fumaric acid, malic acid and carbonic acid and potassium, sodium and ammonium salts thereof, ribonucleic acid and salts thereof, sodium hydroxide and the like. A combination of citric acid, phosphoric acid and their sodium salts is particularly preferred.
The liquid oral composition of the present invention is adjusted to a pH of 4.0 to 9.0, particularly 5.0 to 8.0, especially 5.5 to 7.5 at 25°C. , and a combination of citric acid and sodium citrate, or a combination of sodium dihydrogen phosphate and sodium monohydrogen phosphate can be used as a pH adjuster in this vicinity.
 溶剤としては、水(精製水)が一般的に用いられる。
 水分量は、好ましくは60%以上、より好ましくは60~95%、更に好ましくは70~90%である。
 また、溶剤して、エタノール等の炭素数2又は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。上記低級一価アルコールは、使用時のスッキリとした使用感の付与に好適であるが、本発明では、上記低級一価アルコールの配合は25%以下、特に10%以下でもよく、また、配合しなくてもよく、配合量が0%であっても、スッキリ感が優れる。
Water (purified water) is generally used as the solvent.
The water content is preferably 60% or more, more preferably 60-95%, still more preferably 70-90%.
As a solvent, a lower monohydric alcohol having 2 or 3 carbon atoms such as ethanol, propylene glycol, or the like may be blended. The lower monohydric alcohol is suitable for imparting a refreshing feeling during use. It may be absent, and even if the amount is 0%, the refreshing feeling is excellent.
 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。 Examples, Comparative Examples, and Formulation Examples are shown below to specifically describe the present invention, but the present invention is not limited to the following Examples. In the following examples, % indicates % by mass unless otherwise specified.
 [実施例、比較例]
 表1~4に示す組成の液体口腔用組成物(洗口剤)を常法によって調製し、下記(1)~(5)に示す方法で評価した。結果を表に併記した。
 なお、実施例の液体口腔用組成物は、知覚過敏抑制効果を有し、また、調製直後の外観は澄明であった。
[Examples, Comparative Examples]
Liquid oral compositions (mouthwashes) having compositions shown in Tables 1 to 4 were prepared by conventional methods and evaluated by the methods shown in (1) to (5) below. The results are also shown in the table.
The liquid compositions for oral cavity of Examples had an effect of suppressing hypersensitivity, and the appearance immediately after preparation was clear.
(1)高温外観安定性
 サンプル(液体口腔用組成物)を満注量80mLの無色透明なPET容器((株)吉野工業所製)に70mL充填し、50℃恒温槽に1ヶ月間保存した後、外観安定性を目視判定し、下記の評価基準で評価し、◎、○、△、×で示した。3本のサンプルを評価し、このうち最も低い評価を採用した。
 評価基準
  ◎:ニゴリが全くなかった
  ○:ニゴリがわずかにあった
  △:ニゴリがややあった
  ×:ニゴリがかなりあった
(1) Appearance Stability at High Temperature 70 mL of a sample (liquid oral composition) was filled in an 80 mL colorless and transparent PET container (manufactured by Yoshino Kogyosho Co., Ltd.) and stored in a constant temperature bath at 50° C. for 1 month. After that, the appearance stability was visually evaluated and evaluated according to the following evaluation criteria, and indicated by ⊚, ◯, Δ, and ×. Three samples were evaluated and the lowest evaluation was adopted.
Evaluation criteria ◎: There was no cloudiness at all ○: There was a slight cloudiness △: There was a little cloudiness ×: There was a lot of cloudiness
(2)低温外観安定性
 サンプル(液体口腔用組成物)を満注量80mLの無色透明なPET容器((株)吉野工業所製)に70mL充填し、-5℃恒温槽に1ヶ月保存した後、外観安定性を目視判定し、下記の評価基準で評価し、◎、○、△、×で示した。3本のサンプルを評価し、このうち最も低い評価を採用した。
 評価基準
  ◎:オリが全くなかった
  ○:オリがわずかにあった
  △:オリがややあった
  ×:オリがかなりあった
(2) Low temperature appearance stability Sample (liquid oral composition) was filled in 70 mL of a colorless and transparent PET container (manufactured by Yoshino Kogyosho Co., Ltd.) with a full amount of 80 mL and stored in a -5 ° C constant temperature bath for 1 month. After that, the appearance stability was visually evaluated and evaluated according to the following evaluation criteria, and indicated by ⊚, ◯, Δ, and ×. Three samples were evaluated and the lowest evaluation was adopted.
Evaluation Criteria ◎: There was no residue ○: There was a slight amount of residue △: There was some amount of residue ×: There was a lot of residue
(3)使用後のスッキリ感
 被験者パネラー5名が、サンプル(液体口腔用組成物)20mLを口に含み、20秒洗口後、吐き出し、使用後の口腔内のスッキリ感を下記の評点基準で判定した。5名の平均点から、下記の評価基準で評価し、◎、○、△、×で示した。
 ここで、スッキリ感とは、口腔内がきれいになってスッキリとしたと感じられる切れのよい感覚である。このスッキリ感は、(C)ノニオン性界面活性剤由来の特有の異味がなく、(D)スクラロースの清涼感のあるスッキリした甘味と、(A)硝酸カリウムの金属味、(B)塩化セチルピリジニウムの苦味とが相まって得られる、独特なスッキリ感である。
 評点基準
  4点:スッキリ感がかなりあった
  3点:スッキリ感があった
  2点:スッキリ感がほとんどなかった
  1点:スッキリ感が全くなかった
 評価基準
  ◎:平均点3.5点以上
  ○:平均点2.5点以上3.5点未満
  △:平均点1.5点以上2.5点未満
  ×:平均点1.5点未満
(3) Refreshing feeling after use Five subject panelists put 20 mL of the sample (liquid oral composition) in their mouths, rinsed their mouths for 20 seconds, and then spit it out. Judged. Based on the average score of 5 people, evaluation was made according to the following evaluation criteria, and indicated by ⊚, ◯, Δ, and ×.
Here, the refreshing feeling is a sharp feeling that the inside of the oral cavity is clean and refreshing. This refreshing feeling is due to (C) no peculiar offensive taste derived from nonionic surfactants, (D) refreshing and refreshing sweetness of sucralose, (A) metallic taste of potassium nitrate, and (B) cetylpyridinium chloride. Combined with the bitterness, it has a unique refreshing feeling.
Rating criteria 4 points: considerably refreshing feeling 3 points: refreshing feeling 2 points: almost no refreshing feeling 1 point: no refreshing feeling Evaluation criteria ◎: average score of 3.5 points or more ○: Average score 2.5 points or more and less than 3.5 points △: Average score 1.5 points or more and less than 2.5 points ×: Average score less than 1.5 points
(4)使用後の嫌味のなさ
 被験者パネラー5名が、サンプル(液体口腔用組成物)20mLを口に含み、20秒間洗口後、吐き出し、使用後の嫌味(金属味、苦味及び異味による特有の嫌味)のなさを下記の評点基準で判定した。5名の平均点から、下記の評価基準で評価し、◎、○、△、×で示した。
 評点基準
  4点:嫌味がなかった
  3点:嫌味がほとんどなかった
  2点:嫌味がややあった
  1点:嫌味がかなりあった
 評価基準
  ◎:平均点3.5点以上
  ○:平均点2.5点以上3.5点未満
  △:平均点1.5点以上2.5点未満
  ×:平均点1.5点未満
(4) Absence of disgust after use Five subject panelists took 20 mL of the sample (liquid oral composition) in their mouths, washed their mouths for 20 seconds, and then spit it out. The following rating criteria were used to judge the lack of disgust. Based on the average score of 5 people, evaluation was made according to the following evaluation criteria, and indicated by ⊚, ◯, Δ, and ×.
Scoring criteria 4 points: no disgust 3 points: almost no disgust 2 points: slightly disgusting 1 point: considerable disgust Evaluation criteria ◎: average score of 3.5 points or more ○: average score of 2. 5 points or more and less than 3.5 points △: Average score of 1.5 points or more and less than 2.5 points ×: Average score of less than 1.5 points
(5)殺菌効果
 使用した菌液は、培養液としてTHB(日本BD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フゾバクテリウム・ヌクレアツムATCC10953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1.0になるようにPBSを加えて調製した。希釈用培地としてSCDLP培地(日本BD社製)を使用した。サンプル(液体口腔用組成物の30倍希釈液*)4.0mLに、菌液0.1mLを加え、撹拌後、37℃で3分間反応させ、再び撹拌後、予め4.0mLのSCDLP培地の入った試験管を7本用意し、その1番目の試験管に、上記菌液を加えたサンプル0.44mLを加え、撹拌した。この液0.44mL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3~7番目の試験管に順に行った。1~7番目の試験管中の培養液を撹拌後、10%馬無菌脱繊血含有THB寒天平板(日本BD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、残存するフゾバクテリウム・ヌクレアツム菌の生菌数(cfu)を求め、下記の評価基準で口腔内浮遊菌に対する殺菌効果を評価し、◎、○、△、×で示した。
*;洗口剤を使用して3時間経過後の口腔内での希釈率を想定した希釈倍率。
 なお、コントロール(サンプルの代わりに水を使用)の生菌数は108であった。
 評価基準
  ◎:生菌数が104未満
  ○:生菌数が104以上105未満
  △:生菌数が105以上107未満
  ×:生菌数が107以上
(5) Bactericidal effect The bacterial solution used was prepared by dissolving 30 g of THB (manufactured by BD Japan) as a culture solution in 1 L of purified water, and using Fusobacterium nucleatum ATCC 10953 strain as oral resident bacteria, anaerobic at 37 ° C. PBS was added to prepare a solution cultured for one day under the conditions (5% by volume carbon dioxide, 95% by volume nitrogen) so that the transmittance at 550 nm was 1.0. SCDLP medium (manufactured by BD Japan) was used as a medium for dilution. Add 0.1 mL of the bacterial solution to 4.0 mL of the sample (30-fold dilution of the liquid oral composition * ), stir, react at 37°C for 3 minutes, stir again, and add 4.0 mL of SCDLP medium in advance. Seven test tubes were prepared, and 0.44 mL of the sample containing the bacterial solution was added to the first test tube and stirred. 0.44 mL of this liquid was taken, added to a second test tube, and stirred. This operation was similarly performed on the 3rd to 7th test tubes in order. After stirring the culture solution in the 1st to 7th test tubes, 50 μL of the mixture was smeared on a THB agar plate containing 10% sterile defibrinated horse blood (manufactured by BD Japan) and cultured under anaerobic conditions.
The grown colonies were counted, the number of viable Fusobacterium nucleatum bacteria (cfu) remaining was determined, and the bactericidal effect on oral airborne bacteria was evaluated according to the following evaluation criteria.
*; Dilution rate assuming the dilution rate in the oral cavity after 3 hours using the mouthwash.
The number of viable bacteria in the control (using water instead of the sample) was 10 8 .
Evaluation Criteria ◎: Viable count is less than 10 4 ○: Viable count is 10 4 or more and less than 10 5 △: Viable count is 10 5 or more and less than 10 7 ×: Viable count is 10 7 or more
 使用原料の詳細を下記に示す。
(A)硝酸カリウム
   大塚化学(株)製
(B)塩化セチルピリジニウム
   富士フィルム和光純薬(株)製
(C)ポリオキシエチレン硬化ヒマシ油100
   商品名;EMALEX HC-100、E.O.付加モル数100、
   日本エマルジョン(株)製
(C)ポリオキシエチレン硬化ヒマシ油60
   商品名;EMALEX HC-60、E.O.付加モル数60、
   日本エマルジョン(株)製
(C)ポリオキシエチレンセチルエーテル15
   商品名;ブラウノンCH-315L、E.O.付加モル数15、
   青木油脂工業(株)製
(C)オレイン酸ポリエチレングリコール
   商品名;EMALEX OE-10、日本エマルジョン(株)製
(C)グリセリン脂肪酸エステル
   商品名;EMALEX GMS、日本エマルジョン(株)製
(C)ポリオキシエチレンポリオキシプロピレングリコール
   商品名;アデカ(登録商標)プルロニック、ADEKA社製
(D)スクラロース
   三栄源エフエフアイ(株)製
サッカリンナトリウム(比較品)
   愛三化学工業(株)製
アセスルファムカリウム(比較品)
   ニュートリノヴァ・ジャパン社製
Details of raw materials used are shown below.
(A) Potassium nitrate manufactured by Otsuka Chemical Co., Ltd. (B) Cetylpyridinium chloride manufactured by Fujifilm Wako Pure Chemical Industries, Ltd. (C) Polyoxyethylene hydrogenated castor oil 100
Trade name; EMALEX HC-100, E.M. O. Addition mole number 100,
Nippon Emulsion Co., Ltd. (C) polyoxyethylene hydrogenated castor oil 60
Trade name; EMALEX HC-60, E.M. O. number of added moles 60,
(C) polyoxyethylene cetyl ether 15 manufactured by Nippon Emulsion Co., Ltd.
Trade name; Brownon CH-315L, E.P. O. number of added moles 15,
(C) polyethylene glycol oleate manufactured by Aoki Yushi Kogyo Co., Ltd.; trade name; EMALEX OE-10; (C) glycerin fatty acid ester manufactured by Nippon Emulsion Co., Ltd. trade name; Oxyethylene polyoxypropylene glycol Trade name; ADEKA (registered trademark) Pluronic, (D) sucralose manufactured by ADEKA, saccharin sodium manufactured by San-Ei Gen FFI Co., Ltd. (comparative product)
Acesulfame potassium manufactured by Aisan Chemical Industry Co., Ltd. (comparative product)
Manufactured by Neutrinova Japan
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000003
Figure JPOXMLDOC01-appb-T000003
Figure JPOXMLDOC01-appb-T000004
Figure JPOXMLDOC01-appb-T000004
 [処方例1]洗口剤
(A)硝酸カリウム               5.0
(B)塩化セチルピリジニウム          0.03
(C)ポリオキシエチレン硬化ヒマシ油100   0.6
(D)スクラロース               0.02
エタノール                  10.0
クエン酸                    0.01
クエン酸ナトリウム               0.3
キシリトール                  3.0
グリセリン                   5.0
プロピレングリコール              5.0
香料                      0.2
精製水                    70.84
 計                    100%
 pH;6.2
 {(A)+(B)}/(C)の質量比;8.4
 {(A)+(B)}/(D)の質量比;251.5
 (A)/(D)の質量比;250.0
 (B)/(D)の質量比;1.5
 (C)/(B)の質量比;20.0
高温外観安定性;◎、低温外観安定性;◎、
使用後のスッキリ感;◎、使用後の嫌味のなさ;◎、殺菌効果;◎
[Prescription Example 1] Mouthwash (A) Potassium nitrate 5.0
(B) cetylpyridinium chloride 0.03
(C) Polyoxyethylene hydrogenated castor oil 100 0.6
(D) Sucralose 0.02
Ethanol 10.0
Citric acid 0.01
Sodium citrate 0.3
Xylitol 3.0
Glycerin 5.0
Propylene glycol 5.0
Perfume 0.2
Purified water 70.84
Total 100%
pH; 6.2
Mass ratio of {(A) + (B)}/(C); 8.4
{(A) + (B)}/(D) mass ratio; 251.5
(A) / (D) mass ratio; 250.0
(B) / (D) mass ratio; 1.5
Mass ratio of (C)/(B); 20.0
Appearance stability at high temperature; ◎, Appearance stability at low temperature;
Refreshing feeling after use;
 [処方例2]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硬化ヒマシ油100   0.3
(D)スクラロース               0.02
クエン酸                    0.01
クエン酸ナトリウム               0.3
ソルビット液(70%)            10.0
グリセリン                   5.0
プロピレングリコール              5.0
香料                      0.2
精製水                    74.12
 計                    100%
 pH;6.2
 {(A)+(B)}/(C)の質量比;16.8
 {(A)+(B)}/(D)の質量比;251.5
 (A)/(D)の質量比;250.0
 (B)/(D)の質量比;2.5
 (C)/(B)の質量比;6.0
高温外観安定性;〇、低温外観安定性;〇、
使用後のスッキリ感;◎、使用後の嫌味のなさ;◎、殺菌効果;◎
[Prescription Example 2] Mouthwash (A) Potassium nitrate 5.0
(B) cetylpyridinium chloride 0.05
(C) Polyoxyethylene hydrogenated castor oil 100 0.3
(D) Sucralose 0.02
Citric acid 0.01
Sodium citrate 0.3
Sorbit solution (70%) 10.0
Glycerin 5.0
Propylene glycol 5.0
Perfume 0.2
Purified water 74.12
Total 100%
pH; 6.2
Mass ratio of {(A) + (B)}/(C); 16.8
{(A) + (B)}/(D) mass ratio; 251.5
(A) / (D) mass ratio; 250.0
Mass ratio of (B)/(D); 2.5
Mass ratio of (C)/(B); 6.0
High temperature appearance stability; 〇, Low temperature appearance stability; 〇,
Refreshing feeling after use;
 [処方例3]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硬化ヒマシ油100   0.6
(D)スクラロース               0.005
クエン酸                    0.01
クエン酸ナトリウム               0.3
キシリトール                  1.0
ソルビット液(70%)             5.0
グリセリン                   5.0
プロピレングリコール              5.0
香料                      0.2
精製水                    77.835
 計                    100%
 pH;6.2
 {(A)+(B)}/(C)の質量比;8.4
 {(A)+(B)}/(D)の質量比;1010.0
 (A)/(D)の質量比;1000.0
 (B)/(D)の質量比;10.0
 (C)/(B)の質量比;12.0
高温外観安定性;◎、低温外観安定性;◎、
使用後のスッキリ感;◎、使用後の嫌味のなさ;〇、殺菌効果;◎
[Prescription Example 3] Mouthwash (A) Potassium nitrate 5.0
(B) cetylpyridinium chloride 0.05
(C) Polyoxyethylene hydrogenated castor oil 100 0.6
(D) Sucralose 0.005
Citric acid 0.01
Sodium citrate 0.3
Xylitol 1.0
Sorbit solution (70%) 5.0
Glycerin 5.0
Propylene glycol 5.0
Perfume 0.2
Purified water 77.835
Total 100%
pH; 6.2
Mass ratio of {(A) + (B)}/(C); 8.4
Mass ratio of {(A) + (B)}/(D); 1010.0
Mass ratio of (A) / (D); 1000.0
Mass ratio of (B)/(D); 10.0
Mass ratio of (C)/(B); 12.0
Appearance stability at high temperature; ◎, Appearance stability at low temperature;
Refreshing feeling after use;
 [処方例4]洗口剤
(A)硝酸カリウム               5.0
(B)塩化セチルピリジニウム          0.04
(C)ポリオキシエチレン硬化ヒマシ油100   0.6
(D)スクラロース               0.02
リン酸一水素ナトリウム             0.05
リン酸二水素ナトリウム             0.02
キシリトール                  3.0
グリセリン                   5.0
プロピレングリコール              5.0
香料                      0.2
精製水                    81.07
 計                    100%
 pH;6.8
 {(A)+(B)}/(C)の質量比;8.4
 {(A)+(B)}/(D)の質量比;252.0
 (A)/(D)の質量比;250.0
 (B)/(D)の質量比;2.0
 (C)/(B)の質量比;15.0
高温外観安定性;◎、低温外観安定性;◎、
使用後のスッキリ感;◎、使用後の嫌味のなさ;◎、殺菌効果;◎
[Prescription Example 4] Mouthwash (A) Potassium nitrate 5.0
(B) cetylpyridinium chloride 0.04
(C) Polyoxyethylene hydrogenated castor oil 100 0.6
(D) Sucralose 0.02
Sodium monohydrogen phosphate 0.05
Sodium dihydrogen phosphate 0.02
Xylitol 3.0
Glycerin 5.0
Propylene glycol 5.0
Perfume 0.2
Purified water 81.07
Total 100%
pH; 6.8
Mass ratio of {(A) + (B)}/(C); 8.4
Mass ratio of {(A) + (B)}/(D); 252.0
(A) / (D) mass ratio; 250.0
(B) / (D) mass ratio; 2.0
Mass ratio of (C)/(B); 15.0
Appearance stability at high temperature; ◎, Appearance stability at low temperature;
Refreshing feeling after use;
 [処方例5]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硬化ヒマシ油100   0.4
(D)スクラロース               0.01
クエン酸                    0.01
クエン酸ナトリウム               0.3
ソルビット液(70%)             7.0
グリセリン                   3.0
プロピレングリコール             10.0
香料                      0.2
精製水                    74.03
 計                    100%
 pH;6.2
 {(A)+(B)}/(C)の質量比;12.6
 {(A)+(B)}/(D)の質量比;505.0
 (A)/(D)の質量比;500.0
 (B)/(D)の質量比;5.0
 (C)/(B)の質量比;8.0
高温外観安定性;◎、低温外観安定性;◎、
使用後のスッキリ感;◎、使用後の嫌味のなさ;◎、殺菌効果;◎
[Prescription Example 5] Mouthwash (A) Potassium nitrate 5.0
(B) cetylpyridinium chloride 0.05
(C) Polyoxyethylene hydrogenated castor oil 100 0.4
(D) Sucralose 0.01
Citric acid 0.01
Sodium citrate 0.3
Sorbit solution (70%) 7.0
Glycerin 3.0
Propylene glycol 10.0
Perfume 0.2
Purified water 74.03
Total 100%
pH; 6.2
Mass ratio of {(A) + (B)}/(C); 12.6
Mass ratio of {(A) + (B)}/(D); 505.0
(A) / (D) mass ratio; 500.0
Mass ratio of (B)/(D); 5.0
Mass ratio of (C)/(B); 8.0
Appearance stability at high temperature; ◎, Appearance stability at low temperature;
Refreshing feeling after use;

Claims (6)

  1.  (A)硝酸カリウム、
    (B)塩化セチルピリジニウム、
    (C)ノニオン性界面活性剤
    及び
    (D)スクラロース
    を含有する液体口腔用組成物。
    (A) potassium nitrate,
    (B) cetylpyridinium chloride;
    A liquid oral composition containing (C) a nonionic surfactant and (D) sucralose.
  2.  {(A)+(B)}/(C)が質量比として2.5~25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 {(A) + (B)}/(C) is 2.5 to 25 as a mass ratio.
  3.  {(A)+(B)}/(D)が質量比として30~6,000である請求項1又は2記載の液体口腔用組成物。 The liquid oral composition according to claim 1 or 2, wherein {(A) + (B)}/(D) is 30 to 6,000 as a mass ratio.
  4.  (A)成分を2~8質量%、(B)成分を0.01~0.1質量%、(C)成分を0.3~0.9質量%、(D)成分を0.001~0.1質量%含有する請求項1~3のいずれか1項記載の液体口腔用組成物。 2 to 8% by mass of component (A), 0.01 to 0.1% by mass of component (B), 0.3 to 0.9% by mass of component (C), and 0.001 to 0.001% of component (D) The liquid oral composition according to any one of claims 1 to 3, containing 0.1% by mass.
  5.  (C)ノニオン性界面活性剤が、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、ポリエチレングリコール脂肪酸エステル、グリセリン脂肪酸エステル及びポリオキシエチレンポリオキシプロピレングリコールから選ばれる1種又は2種以上である請求項1~4のいずれか1項記載の液体口腔用組成物。 (C) The nonionic surfactant is one or more selected from polyoxyethylene hydrogenated castor oil, polyoxyethylene alkyl ether, polyethylene glycol fatty acid ester, glycerin fatty acid ester and polyoxyethylene polyoxypropylene glycol. The liquid oral composition according to any one of claims 1-4.
  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.
PCT/JP2022/020907 2021-06-03 2022-05-20 Liquid composition for oral use WO2022255124A1 (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013035792A (en) * 2011-08-09 2013-02-21 Kao Corp Composition for oral cavity
JP2013066490A (en) * 1998-10-28 2013-04-18 Sanei Gen Ffi Inc Compositions containing sucralose and application thereof
JP2013155166A (en) * 2012-02-01 2013-08-15 Lion Corp Dentifrice composition
JP2016150912A (en) * 2015-02-17 2016-08-22 ライオン株式会社 Liquid oral composition
JP2017141178A (en) * 2016-02-09 2017-08-17 ライオン株式会社 Dentifrice composition
JP2019052110A (en) * 2017-09-15 2019-04-04 第一三共ヘルスケア株式会社 Oral composition

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013066490A (en) * 1998-10-28 2013-04-18 Sanei Gen Ffi Inc Compositions containing sucralose and application thereof
JP2013035792A (en) * 2011-08-09 2013-02-21 Kao Corp Composition for oral cavity
JP2013155166A (en) * 2012-02-01 2013-08-15 Lion Corp Dentifrice composition
JP2016150912A (en) * 2015-02-17 2016-08-22 ライオン株式会社 Liquid oral composition
JP2017141178A (en) * 2016-02-09 2017-08-17 ライオン株式会社 Dentifrice composition
JP2019052110A (en) * 2017-09-15 2019-04-04 第一三共ヘルスケア株式会社 Oral composition

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