WO2016121650A1 - Dentifrice composition - Google Patents

Dentifrice composition Download PDF

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Publication number
WO2016121650A1
WO2016121650A1 PCT/JP2016/051874 JP2016051874W WO2016121650A1 WO 2016121650 A1 WO2016121650 A1 WO 2016121650A1 JP 2016051874 W JP2016051874 W JP 2016051874W WO 2016121650 A1 WO2016121650 A1 WO 2016121650A1
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Prior art keywords
dentifrice composition
mass
oil
sodium
composition according
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PCT/JP2016/051874
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French (fr)
Japanese (ja)
Inventor
深澤 哲
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ライオン株式会社
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Priority to CN201680007255.8A priority Critical patent/CN107205900A/en
Priority to KR1020177016627A priority patent/KR20170104996A/en
Publication of WO2016121650A1 publication Critical patent/WO2016121650A1/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
    • A61K8/24Phosphorous; Compounds 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
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/26Aluminium; Compounds 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
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
    • A61K8/365Hydroxycarboxylic acids; Ketocarboxylic acids
    • 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
    • A61K8/46Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur
    • 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 has a high dentinal tubule sealing effect and an excellent pH lowering suppression effect, suppresses the pH drop over time, has a good metallic feel and a good feeling of use, and contains aluminum lactate suitable for suppressing hypersensitivity It relates to a dentifrice composition.
  • Aluminum lactate has dentinal tubule stenosis occlusion and is effective in preventing or treating dentin hypersensitivity, but when aluminum lactate is added to the oral composition, the pH decreases over time, and it tends to become acidic. There have been problems of decalcification of the teeth and exfoliation of the oral mucosa and poor stability, and the appearance of a metallic taste peculiar to aluminum has also been a problem.
  • Patent Document 1 Japanese Patent Laid-Open No. 10-231237
  • Patent Document 2 Japanese Patent Laid-Open No. 2013-119520 discloses an anionic surfactant, a specific water-soluble polymer substance, a dentifrice composition containing potassium nitrate and / or aluminum lactate
  • Patent Document 3 Japanese Patent Laid-Open No. 7-165550 discloses that it is effective in preventing and treating dentinal hypersensitivity.
  • an oral composition an oral band (Example 7) containing aluminum lactate and sodium pyrophosphate is described.
  • Patent Document 4 Japanese Patent Application Laid-Open No. 2002-302429 proposes a non-aqueous oral composition in which aluminum lactate is blended as an acidic component together with a non-aqueous oral composition base material and baking soda to improve bitterness and itchiness.
  • Patent Document 5 Japanese Patent Application Laid-Open No. 2004-268166 discloses that aluminum lactate, sodium pyrophosphate, sodium polyphosphate, and the like can be blended in a solid dosage form oral composition.
  • the present invention has been made in view of the above circumstances.
  • Aluminum lactate exhibits a high dentinal tubule sealing effect and is excellent in pH lowering suppression effect, suppressed pH decrease over time, and suppressed metallic taste and good usability. It aims at providing the dentifrice composition containing.
  • the present inventor has found (A) a dentifrice composition containing 0.01 to 5% by mass of aluminum lactate and (B) 0.01 to 5% of condensed phosphate.
  • A a dentifrice composition containing 0.01 to 5% by mass of aluminum lactate and (B) 0.01 to 5% of condensed phosphate.
  • B 0.01 to 5% of condensed phosphate.
  • C ⁇ -olefin sulfonate
  • the metal taste was suppressed, the usability was improved, and it was found that it can be suitably used to suppress hypersensitivity, and the present invention has been made.
  • a dentifrice composition containing aluminum lactate does not contain pyrophosphate and ⁇ -olefin sulfonate, and does not contain anionic surfactant sodium lauryl sulfate.
  • the pH decreases over time, the pH fluctuates, the metal taste appears and the taste is poor (Comparative Example 7), and either pyrophosphate and ⁇ -olefin sulfonate are blended. If the amount is inadequate, the pH will drop, or a metallic taste or oily feeling will appear and the feeling of use will worsen (Comparative Examples 3 to 6).
  • the present invention provides the following dentifrice composition and a method for suppressing the decrease in pH and expression of metallic taste in the dentifrice composition.
  • [1] (A) 0.01-5% by mass of aluminum lactate, (B) 0.01-5% by mass of condensed phosphate, and (C) 0.1-3% by mass of ⁇ -olefin sulfonate.
  • a dentifrice composition characterized by comprising [2] The dentifrice composition according to [1], wherein the condensed phosphate of component (B) is pyrophosphate or tripolyphosphate.
  • (B) / (A) has a mass ratio of 0.005 to 50, and (C) / (A) has a mass ratio of 0.05 to 100, and the pH reduction in the dentifrice composition according to [8] A method for suppressing the expression of metallic taste.
  • (D) A method for suppressing a decrease in pH and expression of metallic taste in the dentifrice composition according to [8] or [9], wherein 0.1 to 7% by mass of potassium nitrate is blended.
  • a dentifrice composition containing aluminum lactate suitable for suppression can be provided.
  • the dentifrice composition of the present invention contains (A) aluminum lactate, (B) condensed phosphate, and (C) ⁇ -olefin sulfonate.
  • (A) Aluminum lactate is a reaction product of lactic acid and metallic aluminum, is represented by the chemical formula C 9 H 15 AlO 9 , and is a white, odorless powder. As an effect on the teeth, a dentinal tubule sealing effect that narrows or occludes the dentinal tubule is known, and has an effect of reducing dentinal hypersensitivity caused by exposure of the dentinal tubule.
  • Commercially available aluminum lactate can be used.
  • the blending amount of the component (A) aluminum lactate is 0.01 to 5% (mass%, hereinafter the same) of the whole composition, preferably 0.1 to 3%, more preferably 1 to 2%. It is.
  • the combination of (B) condensed phosphate and (C) ⁇ -olefin sulfonate gives a high dentinal tubule sealing effect and an excellent pH reduction inhibiting effect, and also provides a feeling of use. Improve. If the component (B) is absent, the pH drop cannot be suppressed, and if the component (C) is absent, the metallic taste is not suppressed and the usability is poor.
  • a linear or cyclic condensed phosphate represented by the following general formula (1) or (2) may be used.
  • M represents Na or K
  • n is an integer of 2 or more
  • m is an integer of 3 or more.
  • These condensed phosphates can be used singly or in combination of two or more, and among them, linear water-soluble condensed phosphates are preferable, and pyrophosphates, tripolyphosphates, especially pyrophosphoric acid are particularly preferable. A salt is more preferable, and a sodium salt is still more preferable.
  • commercially available products can be used, for example, sodium pyrophosphate (manufactured by Taihei Chemical Sangyo Co., Ltd., Tohoku Chemical Co., Ltd.), potassium pyrophosphate (manufactured by Taihei Chemical Sangyo Co., Ltd., Toagosei Co., Ltd.) ), Sodium tripolyphosphate (manufactured by Taihei Chemical Sangyo Co., Ltd., Central Glass Co., Ltd., Nippon Builder Co., Ltd.) and the like can be used.
  • sodium pyrophosphate manufactured by Taihei Chemical Sangyo Co., Ltd., Tohoku Chemical Co., Ltd.
  • potassium pyrophosphate manufactured by Taihei Chemical Sangyo Co., Ltd., Toagosei Co., Ltd.
  • Sodium tripolyphosphate manufactured by Taihei Chemical Sangyo Co., Ltd., Central Glass Co., Ltd., Nippon Builder Co., Ltd.
  • the blending amount of the (B) component condensed phosphate is 0.01 to 5%, preferably 0.1 to 1%, more preferably 0.3 to 0.5% of the entire composition. If the blending amount is 0.01% or more, a satisfactory pH reduction suppressing effect can be imparted. If too much is added, it is suitable for improving the feeling of use, and if it exceeds 5%, the metallic taste is strongly developed and the feeling of use is lowered.
  • an alkali metal salt such as a sodium salt or potassium salt of an ⁇ -olefin sulfonic acid having 14 to 16 carbon atoms can be used, and an ⁇ -olefin sulfonic acid having 14 carbon atoms can be used. Salts, particularly sodium salts (generic name; sodium tetradecenesulfonate) are preferred.
  • these ⁇ -olefin sulfonates commercially available products can be used.
  • sodium tetradecene sulfonate ( ⁇ -olefin (C14) sodium sulfonate, manufactured by Lion Specialty Chemicals Co., Ltd., “K Lipolane PJ-400CJ”) and the like can be used.
  • the ⁇ -olefin sulfonate may contain a hydroxyalkyl sulfonate as a by-product, and the ratio is not particularly limited, but is usually 20% or less. Acid salts can be used in the present invention.
  • the blending amount of the component (C) ⁇ -olefin sulfonate is 0.1 to 3% of the total composition, preferably 0.5 to 2%, more preferably 0.7 to 1.5%. is there. A feeling in use can be improved as it exists in the range of the said compounding quantity. If the blending amount is less than 0.1%, the metal taste cannot be suppressed, and if it exceeds 3%, an oily feeling is strongly expressed, the taste is poor and the feeling of use is inferior.
  • (B) / (A) indicating the blending amount of the component (B) with respect to the blending amount of the component (A) can be 0.005 to 50 as the mass ratio, preferably 0.005 to 5 More preferably, it is 0.1-3.
  • (C) / (A) indicating the blending amount of the component (C) with respect to the blending amount of the component (A) can be 0.05 to 100 as a mass ratio, preferably 0.05 to 3, More preferably, it is 0.3 to 1.
  • the effect of this invention is more excellent in (B) / (A) and / or (C) / (A) being in the range of the said ratio.
  • (D) potassium nitrate can be mix
  • the blending amount of component (D) potassium nitrate is preferably 0.1 to 7%, more preferably 0.5 to 5% of the total composition. Addition within this range is suitable for enhancing the effect of suppressing hypersensitivity. Moreover, it is suitable also in the suppression effect of pH fall of this invention, and suppression of expression of a metallic taste.
  • the dentifrice composition of the present invention preferably has a pH at 25 ° C. of 5 or more, particularly 5 to 10, more preferably 6 to 8, and is preferably adjusted to such a pH.
  • a pH adjuster for example, hydroxide of alkali metals, such as sodium hydroxide, hydrogencarbonate, carbonate, etc. can also be added.
  • the dentifrice composition of the present invention is suitably prepared as a toothpaste, such as a toothpaste, a liquid toothpaste, and a toothpaste.
  • a toothpaste such as a toothpaste, a liquid toothpaste, and a toothpaste.
  • another well-known component can be mix
  • an abrasive, a binder, a thickener, a surfactant, and a sweetener, a colorant, a preservative, a fragrance, an active ingredient, and the like can be blended as necessary.
  • water can be mix
  • abrasive examples include silica-based abrasives such as precipitated silica, aluminosilicate, zirconosilicate, calcium phosphate-based compounds, calcium carbonate, aluminum hydroxide, and synthetic resin-based abrasives.
  • the blending amount of the abrasive is usually 10 to 50% for toothpaste and 0 to 30% for liquid toothpaste.
  • binder examples include gums such as carrageenan and xanthan gum, organic binders such as cellulose derivatives such as carboxymethylcellulose sodium, and inorganic binders such as gelling silica and gelling aluminum silica.
  • the amount of the binder is usually 0.1 to 10%, preferably 0.1 to 5% for toothpaste and 0 to 5% for liquid toothpaste.
  • the thickener examples include sugar alcohols such as sorbit, xylit, and propylene glycol, and polyhydric alcohols.
  • the blending amount of the thickener is usually 5 to 50%, particularly preferably 20 to 45%.
  • an anionic surfactant As the surfactant, an anionic surfactant, a nonionic surfactant, a cationic surfactant, and an amphoteric surfactant can be blended.
  • the anionic surfactant include alkyl sulfates such as sodium lauryl sulfate.
  • Nonionic surfactants include polyoxyethylene fatty acid esters such as polyoxyethylene hydrogenated castor oil having an average addition mole number of ethylene oxide of 5 to 60, sugar fatty acid esters, sugar alcohol fatty acid esters, polyglycerin fatty acid esters, polyoxy Examples include ethylene higher alcohol ethers.
  • Examples of cationic surfactants include alkylammonium types, and examples of amphoteric surfactants include betaine types and imidazoline types. The blending amount of the surfactant can be adjusted according to the form, purpose of use, and the like, for example, 0 to 10% for toothpaste and 0 to 5% for liquid toothpaste.
  • sweeteners include sodium saccharin and the like, and examples of colorants include blue No. 1, yellow No. 4, and titanium dioxide.
  • colorants include blue No. 1, yellow No. 4, and titanium dioxide.
  • preservative include paraoxybenzoic acid esters such as methyl paraben and ethyl paraben, benzoic acid or a salt thereof.
  • Perfumes include peppermint oil, spearmint oil, anise oil, eucalyptus oil, winter green oil, cassia oil, clove oil, thyme oil, sage oil, lemon oil, orange oil, peppermint oil, cardamom oil, coriander oil, mandarin oil, Lime oil, lavender oil, rosemary oil, laurel oil, camomil oil, caraway oil, marjoram oil, bay oil, lemongrass oil, origanum oil, pine needle oil, neroli oil, rose oil, jasmine oil, grapefruit oil, sweetie Natural fragrances such as oil, bran oil, Iris concrete, absolute peppermint, absolute rose, orange flower, and processing of these natural fragrances (front reservoir cut, rear reservoir cut, fractional distillation, liquid-liquid extraction, essence, powder Perfumed, menthol, moss Bonn, Anethole, Cineol, Methyl salicylate, Synamic aldehyde, Eugenol, 3-l-Mentoxyprop
  • the blending amount is not particularly limited, but the above fragrance material is preferably used at 0.000001 to 1% in the preparation composition.
  • the flavoring fragrance using the fragrance material is preferably used in an amount of 0.1 to 2% in the preparation composition.
  • the active ingredient known ingredients that are usually blended in dentifrice compositions, such as bactericides, anti-inflammatory agents, enzymes, fluorides, plant extracts, tartar inhibitors, dental plaque inhibitors, and the like can be blended.
  • bactericides such as isopropylmethylphenol
  • cationic fungicides such as isopropylmethylphenol
  • cationic fungicides tranexamic acid
  • anti-inflammatory agents such as allantoin
  • enzymes such as dextranase, sodium fluoride, sodium monofluorophosphate, etc. Fluoride etc.
  • the said active ingredient can be mix
  • Dentifrice compositions having the compositions shown in Tables 1 to 3 were prepared by a conventional method and evaluated by the following methods. The results are shown in Tables 1 to 3. In addition, the dentifrice composition was adjusted so that pH in 25 degreeC might be set to 7.0.
  • ⁇ Evaluation method> Evaluation method of dentinal tubule sealing effect According to the method of Pashley et al. (J. Dent. Res. 57, 187-193, 1987), the permeability of dentinal tubule fluid was measured, and dentinal tubules by each dentifrice composition The degree of blockade of was evaluated. A dentin block was cut out from a human tooth root and polished with water-resistant abrasive paper # 2000 to prepare a sample, which was used as a sample.
  • Passability suppression rate (%) ((Amount of fluid before treatment -Amount of fluid after treatment) / (Amount of fluid before treatment)) ⁇ 100 Passage volume: Saline volume ( ⁇ L) passing in 10 minutes
  • the degree of dentinal tubule sealing was judged from the average value of the obtained permeability inhibition rate according to the following evaluation criteria, and the dentinal tubule sealing effect was evaluated. Evaluation criteria for ivory tubule sealing effect; A: The permeability inhibition rate is 90% or more. O: The permeability inhibition rate is 80% or more and less than 90%. ⁇ : The permeability inhibition rate is 60% or more and less than 80%. X: The permeability inhibition rate is 60. Less than%
  • pH change amount is less than 0.5 ⁇ : pH change amount is 0.5 or more and less than 1.0 ⁇ : pH change amount is 1.0 or more and less than 1.5 ⁇ : pH change amount is 1.5 or more
  • the raw materials used are the same as described above, and the pH of the preparation at 25 ° C. is in the range of 5-10.
  • Dentifrice (A) Aluminum lactate 1.5 (B) Sodium pyrophosphate 1 (C) Sodium ⁇ -olefin sulfonate 1 (D) Potassium nitrate 5 Sodium monofluorophosphate 1.1 Silicic anhydride 20 Sodium lauryl sulfate 1.5 70% sorbite solution 30 Propylene glycol 3 Xanthan gum 0.8 Saccharin sodium 0.3 Fragrance 1.4 Water balance Total 100.0%

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Abstract

Provided is a dentifrice composition that exhibits an excellent effect of sealing dentinal fine tubules, effectively suppresses a lowering of pH, shows a controlled lowering of pH with the passage of time, gives a suppressed metallic taste and a good feeling in use and is appropriately usable for inhibiting dentinal hyperesthesia, said dentifrice composition comprising: (A) 0.01-5 mass% of aluminum lactate; (B) 0.01-5 mass% of a fused phosphate; and (C) 0.1-3 mass% of an α-olein sulfonic acid. Also provided is a method for suppressing a lowering of pH and expression of a metallic taste in the aforesaid dentifrice composition, said method comprising blending a dentifrice composition containing 0.01-5 mass% of component (A) with 0.01-5 mass% of component (B) and 0.1-3 mass% of component (C).

Description

歯磨組成物Dentifrice composition
 本発明は、高い象牙細管封鎖効果を奏すると共にpH低下抑制効果が優れ、経時におけるpH低下が抑えられ、また、金属味が抑えられ使用感も良好な、知覚過敏抑制用として好適な乳酸アルミニウム含有の歯磨組成物に関する。 The present invention has a high dentinal tubule sealing effect and an excellent pH lowering suppression effect, suppresses the pH drop over time, has a good metallic feel and a good feeling of use, and contains aluminum lactate suitable for suppressing hypersensitivity It relates to a dentifrice composition.
 乳酸アルミニウムは、象牙細管狭窄閉塞作用を有し、象牙質知覚過敏症の予防又は治療に有効であるが、乳酸アルミニウムを口腔用組成物に配合すると経時でpH低下が生じ、酸性に傾くことによって歯の脱灰や口腔粘膜剥離を招いたり、安定性が悪くなる問題があり、また、アルミニウム特有の金属味の発現も問題となっていた。 Aluminum lactate has dentinal tubule stenosis occlusion and is effective in preventing or treating dentin hypersensitivity, but when aluminum lactate is added to the oral composition, the pH decreases over time, and it tends to become acidic. There have been problems of decalcification of the teeth and exfoliation of the oral mucosa and poor stability, and the appearance of a metallic taste peculiar to aluminum has also been a problem.
 このような問題に対して、特許文献1(特開平10-231237号公報)には、乳酸アルミニウム配合の液体口腔用組成物に糖アルコールを配合することで、白濁、沈殿を防止し安定性を向上した技術が提案され、特許文献2(特開2013-119520号公報)には、硝酸カリウム及び/又は乳酸アルミニウムを含有する歯磨剤組成物にアニオン性界面活性剤、特定の水溶性高分子物質、アルギン酸プロピレングリコールを配合することによって、十分な泡立ちを確保すると共に保存安定性(液分離安定性)を向上した技術が提案されているが、これらは経時におけるpH変動に関して言及がない。 In order to deal with such problems, Patent Document 1 (Japanese Patent Laid-Open No. 10-231237) describes that by adding a sugar alcohol to a liquid oral composition containing aluminum lactate, white turbidity and precipitation are prevented and stability is improved. An improved technique has been proposed, and Patent Document 2 (Japanese Patent Laid-Open No. 2013-119520) discloses an anionic surfactant, a specific water-soluble polymer substance, a dentifrice composition containing potassium nitrate and / or aluminum lactate, There have been proposed technologies that ensure sufficient foaming and improve storage stability (liquid separation stability) by blending propylene glycol alginate, but there is no mention of pH fluctuation over time.
 一方、口腔用組成物に乳酸アルミニウムと共に縮合リン酸塩を配合し得ることは公知であり、特許文献3(特開平7-165550号公報)には、象牙質知覚過敏症の予防、治療に有効な口腔用組成物として、乳酸アルミニウムとピロリン酸ナトリウムを配合した口腔用バンド(実施例7)が記載されている。特許文献4(特開2002-302429号公報)には、非水系口腔用組成物用基材及び重曹と共に酸性成分として乳酸アルミニウムが配合され、苦みやえぐみが改善した非水系口腔用組成物が提案され、更に配合し得る歯石沈着防止成分の例示にピロリン酸ナトリウム、ポリリン酸ナトリウムが記載されている。特許文献5(特開2004-26816号公報)には、固形剤型の口腔用組成物に乳酸アルミニウム、ピロリン酸ナトリウム、ポリリン酸ナトリウム等を配合し得ることが開示されている。 On the other hand, it is known that a condensed phosphate can be blended with an aluminum lactate in an oral composition, and Patent Document 3 (Japanese Patent Laid-Open No. 7-165550) discloses that it is effective in preventing and treating dentinal hypersensitivity. As an oral composition, an oral band (Example 7) containing aluminum lactate and sodium pyrophosphate is described. Patent Document 4 (Japanese Patent Application Laid-Open No. 2002-302429) proposes a non-aqueous oral composition in which aluminum lactate is blended as an acidic component together with a non-aqueous oral composition base material and baking soda to improve bitterness and itchiness. Furthermore, sodium pyrophosphate and sodium polyphosphate are described as examples of the calculus deposition preventing component that can be further blended. Patent Document 5 (Japanese Patent Application Laid-Open No. 2004-26816) discloses that aluminum lactate, sodium pyrophosphate, sodium polyphosphate, and the like can be blended in a solid dosage form oral composition.
特開平10-231237号公報Japanese Patent Laid-Open No. 10-231237 特開2013-119520号公報JP 2013-119520 A 特開平7-165550号公報JP 7-165550 A 特開2002-302429号公報JP 2002-302429 A 特開2004-26816号公報JP 2004-26816 A
 しかしながら、乳酸アルミニウムを配合した口腔用組成物のpH低下の抑制については十分とは言い難く改善の余地があるものであり、pH低下をより有効に抑制する技術の開発が望まれた。 However, the suppression of the pH drop of the oral composition containing aluminum lactate is not sufficient and there is room for improvement, and the development of a technique for more effectively suppressing the pH drop has been desired.
 本発明は、上記事情に鑑みなされたもので、高い象牙細管封鎖効果を奏すると共にpH低下抑制効果が優れ、経時においてpH低下が抑えられ、また、金属味が抑えられ使用感も良好な乳酸アルミニウム含有の歯磨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. Aluminum lactate exhibits a high dentinal tubule sealing effect and is excellent in pH lowering suppression effect, suppressed pH decrease over time, and suppressed metallic taste and good usability. It aims at providing the dentifrice composition containing.
 本発明者は、上記目的を達成するため鋭意検討を行った結果、(A)乳酸アルミニウムを0.01~5質量%含有する歯磨組成物に、(B)縮合リン酸塩を0.01~5質量%と、(C)α-オレフィンスルホン酸塩を0.1~3質量%とを配合することによって、高い象牙細管封鎖効果を奏すると共にpH低下抑制効果が優れ、経時においてpH低下が抑制され、また、金属味が抑えられて使用感も改善し、知覚過敏抑制に好適に使用できることを知見し、本発明をなすに至った。 As a result of intensive studies to achieve the above object, the present inventor has found (A) a dentifrice composition containing 0.01 to 5% by mass of aluminum lactate and (B) 0.01 to 5% of condensed phosphate. By blending 5% by mass and 0.1 to 3% by mass of (C) α-olefin sulfonate, it exhibits a high dentinal tubule-sealing effect and is excellent in pH reduction inhibiting effect. In addition, the metal taste was suppressed, the usability was improved, and it was found that it can be suitably used to suppress hypersensitivity, and the present invention has been made.
 即ち、後述の比較例に示すように、乳酸アルミニウムを配合した歯磨剤組成物は、ピロリン酸塩及びα-オレフィンスルホン酸塩を含まないと、アニオン性界面活性剤のラウリル硫酸ナトリウムが含まれていても、経時においてpH低下が生じてpHが変動し、金属味が発現して味も悪く(比較例7)、また、ピロリン酸塩及びα-オレフィンスルホン酸塩が配合されていてもいずれかの量が不適切であると、pHが低下してしまうか、あるいは金属味やオイル感が発現して使用感が悪くなる(比較例3~6)。これに対して、後述の実施例に示すように、(A)乳酸アルミニウムに(B)縮合リン酸塩、(C)α-オレフィンスルホン酸塩を適切量で組み合わせて歯磨組成物に配合すると、(B)、(C)成分の組み合わせが特異的に作用し、乳酸アルミニウムによる象牙細管封鎖効果が優れると共に50℃で1ヶ月保存してもpH変化量が1.0に満たない優れたpH低下抑制効果を奏し、pHが経時で安定化し、酸性に傾くのも防止することができ、また、金属味を抑え、オイル感の発現も防止し、味の良い良好な使用感を与えることもできる。
 なおこの場合、(B)成分量が多すぎると(A)成分由来の金属味がより強く発現し、また、(C)成分量が多すぎるとオイル感が強く生じてしまうという問題が生じるが、(B)、(C)成分を適切に組み合わせることによって、これら問題も全て解消し、上記格別な作用効果を付与できる。
That is, as shown in a comparative example described later, a dentifrice composition containing aluminum lactate does not contain pyrophosphate and α-olefin sulfonate, and does not contain anionic surfactant sodium lauryl sulfate. However, the pH decreases over time, the pH fluctuates, the metal taste appears and the taste is poor (Comparative Example 7), and either pyrophosphate and α-olefin sulfonate are blended. If the amount is inadequate, the pH will drop, or a metallic taste or oily feeling will appear and the feeling of use will worsen (Comparative Examples 3 to 6). On the other hand, as shown in the examples described later, when (A) aluminum lactate and (B) condensed phosphate and (C) α-olefin sulfonate are combined in an appropriate amount and blended into the dentifrice composition, The combination of the components (B) and (C) acts specifically, and the dentinal tubule sealing effect of aluminum lactate is excellent, and the pH change is less than 1.0 even when stored at 50 ° C. for 1 month. It has a suppressive effect, pH can be stabilized over time, and it can be prevented from being acidic, and it can also suppress the metallic taste, prevent the appearance of oiliness, and give a good feeling of good taste. .
In this case, if the amount of the component (B) is too large, the metal taste derived from the component (A) is more strongly expressed, and if the amount of the component (C) is too large, a feeling of oil is strongly generated. By appropriately combining the components (B) and (C), all of these problems can be solved and the above-mentioned special effects can be imparted.
 従って、本発明は、下記の歯磨組成物及び歯磨組成物におけるpH低下と金属味の発現を抑制する方法を提供する。
〔1〕
 (A)乳酸アルミニウムを0.01~5質量%と、(B)縮合リン酸塩を0.01~5質量%と、(C)α-オレフィンスルホン酸塩を0.1~3質量%とを配合したことを特徴とする歯磨組成物。
〔2〕
 (B)成分の縮合リン酸塩が、ピロリン酸塩又はトリポリリン酸塩である〔1〕に記載の歯磨組成物。
〔3〕
 (C)α-オレフィンスルホン酸塩が、炭素数が14~16のα-オレフィンスルホン酸塩である〔1〕又は〔2〕に記載の歯磨組成物。
〔4〕
 (B)/(A)が質量比として0.005~50、かつ(C)/(A)が質量比として0.05~100である〔1〕~〔3〕のいずれかに記載の歯磨組成物。
〔5〕
 更に、(D)硝酸カリウムを0.1~7質量%配合した〔1〕~〔4〕のいずれかに記載の歯磨組成物。
〔6〕
 25℃におけるpHが5以上である〔1〕~〔5〕のいずれかに記載の歯磨組成物。
〔7〕
 練歯磨剤に調製された〔1〕~〔6〕のいずれかに記載の歯磨組成物。
〔8〕
 (A)乳酸アルミニウムを0.01~5質量%含有する歯磨組成物に、(B)縮合リン酸塩を0.01~5質量%と、(C)α-オレフィンスルホン酸塩を0.1~3質量%とを配合し、前記歯磨組成物におけるpH低下と金属味の発現を抑制する方法。
〔9〕
 (B)/(A)が質量比として0.005~50、かつ(C)/(A)が質量比として0.05~100である、〔8〕に記載の歯磨組成物におけるpH低下と金属味の発現を抑制する方法。
〔10〕
 更に、(D)硝酸カリウムを0.1~7質量%配合する〔8〕又は〔9〕に記載の歯磨組成物におけるpH低下と金属味の発現を抑制する方法。
〔11〕
 歯磨組成物が、25℃におけるpHが5以上である〔8〕~〔10〕のいずれかに記載の歯磨組成物におけるpH低下と金属味の発現を抑制する方法。
〔12〕
 練歯磨剤に調製する〔8〕~〔11〕のいずれかに記載の歯磨組成物におけるpH低下と金属味の発現を抑制する方法。
Accordingly, the present invention provides the following dentifrice composition and a method for suppressing the decrease in pH and expression of metallic taste in the dentifrice composition.
[1]
(A) 0.01-5% by mass of aluminum lactate, (B) 0.01-5% by mass of condensed phosphate, and (C) 0.1-3% by mass of α-olefin sulfonate. A dentifrice composition characterized by comprising
[2]
The dentifrice composition according to [1], wherein the condensed phosphate of component (B) is pyrophosphate or tripolyphosphate.
[3]
(C) The dentifrice composition according to [1] or [2], wherein the α-olefin sulfonate is an α-olefin sulfonate having 14 to 16 carbon atoms.
[4]
The toothbrush according to any one of [1] to [3], wherein (B) / (A) is from 0.005 to 50 in terms of mass ratio, and (C) / (A) is in the range of from 0.05 to 100 Composition.
[5]
The dentifrice composition according to any one of [1] to [4], further comprising (D) 0.1 to 7% by mass of potassium nitrate.
[6]
The dentifrice composition according to any one of [1] to [5], wherein the pH at 25 ° C is 5 or more.
[7]
The dentifrice composition according to any one of [1] to [6], which is prepared as a toothpaste.
[8]
(A) A dentifrice composition containing 0.01-5% by mass of aluminum lactate, (B) 0.01-5% by mass of condensed phosphate, and (C) 0.1% of α-olefin sulfonate. A method for suppressing the decrease in pH and the appearance of metallic taste in the dentifrice composition by blending ˜3 mass%.
[9]
(B) / (A) has a mass ratio of 0.005 to 50, and (C) / (A) has a mass ratio of 0.05 to 100, and the pH reduction in the dentifrice composition according to [8] A method for suppressing the expression of metallic taste.
[10]
(D) A method for suppressing a decrease in pH and expression of metallic taste in the dentifrice composition according to [8] or [9], wherein 0.1 to 7% by mass of potassium nitrate is blended.
[11]
The method for suppressing a decrease in pH and expression of metallic taste in a dentifrice composition according to any one of [8] to [10], wherein the dentifrice composition has a pH of 5 or more at 25 ° C.
[12]
A method for suppressing a decrease in pH and expression of a metallic taste in the dentifrice composition according to any one of [8] to [11] prepared in a toothpaste.
 本発明によれば、高い象牙細管封鎖効果を奏すると共にpH低下抑制効果が優れ、経時においてpH低下が抑えられ、また、金属味が抑えられオイル感も抑制され良好な使用感を与える、知覚過敏抑制用として好適な乳酸アルミニウム含有の歯磨組成物を提供できる。 According to the present invention, there is a high dentinal tubule sealing effect and an excellent pH lowering suppressing effect, the pH lowering is suppressed over time, the metallic taste is suppressed, the oily feeling is also suppressed, and a good feeling of use is given. A dentifrice composition containing aluminum lactate suitable for suppression can be provided.
 以下、本発明について更に詳述する。本発明の歯磨組成物は、(A)乳酸アルミニウム、(B)縮合リン酸塩、(C)α-オレフィンスルホン酸塩を含有する。 Hereinafter, the present invention will be described in further detail. The dentifrice composition of the present invention contains (A) aluminum lactate, (B) condensed phosphate, and (C) α-olefin sulfonate.
 (A)乳酸アルミニウムは、乳酸と金属アルミニウムの反応生成物であり、化学式C915AlO9で表され、白色で無臭の粉末である。歯牙への作用として、象牙細管を狭窄又は閉塞する象牙細管封鎖効果が知られており、象牙細管の露出により生じる象牙質知覚過敏症の軽減効果を有する。乳酸アルミニウムは市販のものを使用し得る。
 (A)成分の乳酸アルミニウムの配合量は、組成物全体の0.01~5%(質量%、以下、同様。)であり、好ましくは0.1~3%、より好ましくは1~2%である。0.01%以上配合すると、十分な象牙細管封鎖効果を付与することができる。多く配合し過ぎないほうが、十分にpH低下を抑制し、使用感を改善するには好適であり、5%を超えるとpH低下傾向が非常に強くなり、また、金属味が強く発現してしまう。
(A) Aluminum lactate is a reaction product of lactic acid and metallic aluminum, is represented by the chemical formula C 9 H 15 AlO 9 , and is a white, odorless powder. As an effect on the teeth, a dentinal tubule sealing effect that narrows or occludes the dentinal tubule is known, and has an effect of reducing dentinal hypersensitivity caused by exposure of the dentinal tubule. Commercially available aluminum lactate can be used.
The blending amount of the component (A) aluminum lactate is 0.01 to 5% (mass%, hereinafter the same) of the whole composition, preferably 0.1 to 3%, more preferably 1 to 2%. It is. When 0.01% or more is blended, a sufficient dentinal tubule sealing effect can be imparted. If too much is added, it is preferable to sufficiently suppress the pH drop and improve the feeling of use. If it exceeds 5%, the tendency to drop the pH becomes very strong, and the metallic taste is strongly expressed. .
 本発明では、(B)縮合リン酸塩と(C)α-オレフィンスルホン酸塩とを組み合わせて配合することによって、高い象牙細管封鎖効果を奏すると共に優れたpH低下抑制効果を与え、使用感も改善する。(B)成分を欠くとpHの低下が抑制できず、(C)成分を欠くと金属味が抑制されず使用感が劣る。 In the present invention, the combination of (B) condensed phosphate and (C) α-olefin sulfonate gives a high dentinal tubule sealing effect and an excellent pH reduction inhibiting effect, and also provides a feeling of use. Improve. If the component (B) is absent, the pH drop cannot be suppressed, and if the component (C) is absent, the metallic taste is not suppressed and the usability is poor.
 (B)縮合リン酸塩としては、下記一般式(1)又は(2)で示される直鎖状又は環状の縮合リン酸塩を使用し得る。
 Mn+2n3n+1   (1)
 (MPO3m    (2)
(式中、MはNa又はKを示し、nは2以上の整数、mは3以上の整数である。)
 上記一般式(1)で示される直鎖状のポリリン酸塩としては、n=2のピロリン酸ナトリウムやピロリン酸カリウム、n=3のトリポリリン酸ナトリウムやトリポリリン酸カリウム、n=4のテトラポリリン酸ナトリウムやテトラポリリン酸カリウム、高重合度のメタリン酸ナトリウムやメタリン酸カリウムなどが挙げられる。
 上記一般式(2)で示される環状のポリリン酸塩としては、m=3のトリメタリン酸ナトリウムやトリメタリン酸カリウム、m=4のテトラメタリン酸ナトリウムやテトラメタリン酸カリウム、m=6のヘキサメタリン酸ナトリウムやヘキサメタリン酸カリウムなどが挙げられる。
 これら縮合リン酸塩は1種を単独で又は2種以上を混合して使用し得るが、中でも直鎖状の水溶性縮合リン酸塩が好ましく、特にピロリン酸塩、トリポリリン酸塩、とりわけピロリン酸塩がより好ましく、ナトリウム塩であることが更に好ましい。
 具体的には市販品を使用でき、例えばピロリン酸ナトリウム(太平化学産業(株)製、東北化学(株)製)、ピロリン酸カリウム(太平化学産業(株)製、東亞合成化学(株)製)、トリポリリン酸ナトリウム(太平化学産業(株)製、セントラル硝子(株)製、日本ビルダー(株)製)などを使用し得る。
(B) As the condensed phosphate, a linear or cyclic condensed phosphate represented by the following general formula (1) or (2) may be used.
M n + 2 P n O 3n + 1 (1)
(MPO 3 ) m (2)
(In the formula, M represents Na or K, n is an integer of 2 or more, and m is an integer of 3 or more.)
The linear polyphosphate represented by the general formula (1) includes n = 2 sodium pyrophosphate and potassium pyrophosphate, n = 3 sodium tripolyphosphate and potassium tripolyphosphate, and n = 4 tetrapolyphosphoric acid. Examples include sodium and potassium tetrapolyphosphate, sodium metaphosphate having high polymerization degree, and potassium metaphosphate.
Examples of the cyclic polyphosphate represented by the general formula (2) include m = 3 sodium trimetaphosphate and potassium trimetaphosphate, m = 4 sodium tetrametaphosphate and potassium tetrametaphosphate, and m = 6 sodium hexametaphosphate. And potassium hexametaphosphate.
These condensed phosphates can be used singly or in combination of two or more, and among them, linear water-soluble condensed phosphates are preferable, and pyrophosphates, tripolyphosphates, especially pyrophosphoric acid are particularly preferable. A salt is more preferable, and a sodium salt is still more preferable.
Specifically, commercially available products can be used, for example, sodium pyrophosphate (manufactured by Taihei Chemical Sangyo Co., Ltd., Tohoku Chemical Co., Ltd.), potassium pyrophosphate (manufactured by Taihei Chemical Sangyo Co., Ltd., Toagosei Co., Ltd.) ), Sodium tripolyphosphate (manufactured by Taihei Chemical Sangyo Co., Ltd., Central Glass Co., Ltd., Nippon Builder Co., Ltd.) and the like can be used.
 (B)成分の縮合リン酸塩の配合量は、組成物全体の0.01~5%であり、好ましくは0.1~1%、より好ましくは0.3~0.5%である。配合量が0.01%以上であると、満足なpH低下抑制効果を付与できる。多く配合し過ぎないほうが使用感の改善には好適であり、5%を超えると金属味が強く発現し、使用感が低下する。 The blending amount of the (B) component condensed phosphate is 0.01 to 5%, preferably 0.1 to 1%, more preferably 0.3 to 0.5% of the entire composition. If the blending amount is 0.01% or more, a satisfactory pH reduction suppressing effect can be imparted. If too much is added, it is suitable for improving the feeling of use, and if it exceeds 5%, the metallic taste is strongly developed and the feeling of use is lowered.
 (C)α-オレフィンスルホン酸塩としては、炭素数が14~16のα-オレフィンスルホン酸のナトリウム塩、カリウム塩等のアルカリ金属塩を用いることができ、炭素数14のα-オレフィンスルホン酸塩、特にナトリウム塩(一般名;テトラデセンスルホン酸ナトリウム)が好ましい。
 これらα-オレフィンスルホン酸塩は、市販品を使用することができる。具体的には、テトラデセンスルホン酸ナトリウム(α-オレフィン(C14)スルホン酸ナトリウム、ライオン・スペシャリティ・ケミカルズ(株)製、「KリポランPJ-400CJ」)などを使用し得る。
 なお、α-オレフィンスルホン酸塩は、副生物としてヒドロキシアルキルスルホン酸塩を含むことがあり、その割合は特に限定されるものではないが通常20%以下であるが、このようなα-オレフィンスルホン酸塩を本発明では用いることができる。
(C) As the α-olefin sulfonate, an alkali metal salt such as a sodium salt or potassium salt of an α-olefin sulfonic acid having 14 to 16 carbon atoms can be used, and an α-olefin sulfonic acid having 14 carbon atoms can be used. Salts, particularly sodium salts (generic name; sodium tetradecenesulfonate) are preferred.
As these α-olefin sulfonates, commercially available products can be used. Specifically, sodium tetradecene sulfonate (α-olefin (C14) sodium sulfonate, manufactured by Lion Specialty Chemicals Co., Ltd., “K Lipolane PJ-400CJ”) and the like can be used.
The α-olefin sulfonate may contain a hydroxyalkyl sulfonate as a by-product, and the ratio is not particularly limited, but is usually 20% or less. Acid salts can be used in the present invention.
 (C)成分のα-オレフィンスルホン酸塩の配合量は、組成物全体の0.1~3%であり、好ましくは0.5~2%、より好ましくは0.7~1.5%である。上記配合量の範囲内であると、使用感を改善できる。配合量が0.1%に満たないと金属味を抑制することができず、3%を超えるとオイル感が強く発現し、味が悪くなって使用感が劣る。 The blending amount of the component (C) α-olefin sulfonate is 0.1 to 3% of the total composition, preferably 0.5 to 2%, more preferably 0.7 to 1.5%. is there. A feeling in use can be improved as it exists in the range of the said compounding quantity. If the blending amount is less than 0.1%, the metal taste cannot be suppressed, and if it exceeds 3%, an oily feeling is strongly expressed, the taste is poor and the feeling of use is inferior.
 なお、アニオン性界面活性剤であってもラウリル硫酸ナトリウム等のアルキル硫酸塩を(B)縮合リン酸塩と組み合わせて配合しても、(A)乳酸アルミニウムによる使用感の低下が改善せず、本発明の目的は達成されない。 In addition, even if it is an anionic surfactant or an alkyl sulfate such as sodium lauryl sulfate is combined with (B) the condensed phosphate, (A) the decrease in feeling of use due to aluminum lactate is not improved, The object of the present invention is not achieved.
 本発明では、(A)成分に(B)、(C)成分を適切割合で組み合わせると、pH低下の抑制効果がより向上し、使用感もより改善できる。
 この場合、(A)成分の配合量に対する(B)成分の配合量を示す(B)/(A)が質量比として0.005~50とすることができるが、0.005~5が好ましく、より好ましくは0.1~3である。また、(A)成分の配合量に対する(C)成分の配合量を示す(C)/(A)が質量比として0.05~100とすることができるが、0.05~3が好ましく、より好ましくは0.3~1である。
 (B)/(A)、及び/又は(C)/(A)が上記比率の範囲内であると、本発明の効果がより優れる。
In the present invention, when the components (B) and (C) are combined in an appropriate ratio with the component (A), the effect of suppressing the decrease in pH is further improved and the feeling in use can be further improved.
In this case, (B) / (A) indicating the blending amount of the component (B) with respect to the blending amount of the component (A) can be 0.005 to 50 as the mass ratio, preferably 0.005 to 5 More preferably, it is 0.1-3. Further, (C) / (A) indicating the blending amount of the component (C) with respect to the blending amount of the component (A) can be 0.05 to 100 as a mass ratio, preferably 0.05 to 3, More preferably, it is 0.3 to 1.
The effect of this invention is more excellent in (B) / (A) and / or (C) / (A) being in the range of the said ratio.
 更に、本発明では、(D)硝酸カリウムを配合することができる。硝酸カリウムは、知覚過敏による痛みを緩和し、知覚過敏抑制成分として有効である。
 (D)成分の硝酸カリウムの配合量は、組成物全体の0.1~7%が好ましく、より好ましくは0.5~5%である。この範囲内で添加することが、知覚過敏抑制効果の増強に好適である。また、本発明のpH低下抑制効果、金属味の発現の抑制においても好適である。
Furthermore, in this invention, (D) potassium nitrate can be mix | blended. Potassium nitrate relieves pain caused by hypersensitivity and is effective as a hypersensitivity inhibitor.
The blending amount of component (D) potassium nitrate is preferably 0.1 to 7%, more preferably 0.5 to 5% of the total composition. Addition within this range is suitable for enhancing the effect of suppressing hypersensitivity. Moreover, it is suitable also in the suppression effect of pH fall of this invention, and suppression of expression of a metallic taste.
 本発明の歯磨組成物は、25℃におけるpHを5以上、特に5~10、より好ましくは6~8とすることが好ましく、このようなpHになるように調整することが好ましい。pH5以上であると、十分な象牙細管封鎖効果が発揮され、使用にも適するものとなる。
 なお、pHを調整する場合、pH調整剤を添加してもよく、例えば水酸化ナトリウム等のアルカリ金属の水酸化物、炭酸水素塩、炭酸塩などを添加することもできる。
The dentifrice composition of the present invention preferably has a pH at 25 ° C. of 5 or more, particularly 5 to 10, more preferably 6 to 8, and is preferably adjusted to such a pH. When the pH is 5 or more, a sufficient dentinal tubule sealing effect is exhibited, and it is suitable for use.
In addition, when adjusting pH, you may add a pH adjuster, for example, hydroxide of alkali metals, such as sodium hydroxide, hydrogencarbonate, carbonate, etc. can also be added.
 本発明の歯磨組成物は、練歯磨、液状歯磨、潤製歯磨など、特に練歯磨として好適に調製される。また、上記成分に加えて、その他の公知成分を本発明の効果を妨げない範囲で必要に応じて配合できる。例えば、練歯磨剤では、研磨剤、粘結剤、粘稠剤、界面活性剤、更に必要により甘味剤、着色剤、防腐剤、香料、有効成分などを配合できる。なお、液体媒体として水を配合し、通常の方法で調製することができる。 The dentifrice composition of the present invention is suitably prepared as a toothpaste, such as a toothpaste, a liquid toothpaste, and a toothpaste. Moreover, in addition to the said component, another well-known component can be mix | blended as needed in the range which does not prevent the effect of this invention. For example, in a toothpaste, an abrasive, a binder, a thickener, a surfactant, and a sweetener, a colorant, a preservative, a fragrance, an active ingredient, and the like can be blended as necessary. In addition, water can be mix | blended as a liquid medium and it can prepare by a normal method.
 研磨剤としては、沈降性シリカ、アルミノシリケート、ジルコノシリケート等のシリカ系研磨剤、リン酸カルシウム系化合物、炭酸カルシウム、水酸化アルミニウム、合成樹脂系研磨剤などが挙げられる。研磨剤の配合量は、通常、練歯磨では10~50%、液状歯磨では0~30%である。 Examples of the abrasive include silica-based abrasives such as precipitated silica, aluminosilicate, zirconosilicate, calcium phosphate-based compounds, calcium carbonate, aluminum hydroxide, and synthetic resin-based abrasives. The blending amount of the abrasive is usually 10 to 50% for toothpaste and 0 to 30% for liquid toothpaste.
 粘結剤としては、カラギーナン、キサンタンガム等のガム類、カルボキシメチルセルロースナトリウム等のセルロース誘導体などの有機粘結剤、ゲル化性シリカ、ゲル化性アルミニウムシリカ等の無機粘結剤が挙げられる。粘結剤の配合量は、通常、0.1~10%であり、練歯磨では0.1~5%、液状歯磨では0~5%が好ましい。 Examples of the binder include gums such as carrageenan and xanthan gum, organic binders such as cellulose derivatives such as carboxymethylcellulose sodium, and inorganic binders such as gelling silica and gelling aluminum silica. The amount of the binder is usually 0.1 to 10%, preferably 0.1 to 5% for toothpaste and 0 to 5% for liquid toothpaste.
 粘稠剤としては、ソルビット、キシリット、プロピレングリコール等の糖アルコール、多価アルコールが挙げられる。粘稠剤の配合量は、通常、5~50%であり、特に20~45%が好ましい。 Examples of the thickener include sugar alcohols such as sorbit, xylit, and propylene glycol, and polyhydric alcohols. The blending amount of the thickener is usually 5 to 50%, particularly preferably 20 to 45%.
 界面活性剤としては、アニオン性界面活性剤、ノニオン性界面活性剤、カチオン性界面活性剤、両性界面活性剤を配合することができる。
 アニオン性界面活性剤としては、ラウリル硫酸ナトリウム等のアルキル硫酸塩などが挙げられる。ノニオン性界面活性剤としては、エチレンオキサイドの平均付加モル数が5~60のポリオキシエチレン硬化ヒマシ油等のポリオキシエチレン脂肪酸エステル、糖脂肪酸エステル、糖アルコール脂肪酸エステル、ポリグリセリン脂肪酸エステル、ポリオキシエチレン高級アルコールエーテル等が挙げられる。
 カチオン性界面活性剤としては、アルキルアンモニウム型等が挙げられ、両性界面活性剤としては、ベタイン型、イミダゾリン型が挙げられる。
 界面活性剤の配合量は、形態、使用目的等に応じ調整でき、例えば、練歯磨では0~10%、液状歯磨では0~5%である。
As the surfactant, an anionic surfactant, a nonionic surfactant, a cationic surfactant, and an amphoteric surfactant can be blended.
Examples of the anionic surfactant include alkyl sulfates such as sodium lauryl sulfate. Nonionic surfactants include polyoxyethylene fatty acid esters such as polyoxyethylene hydrogenated castor oil having an average addition mole number of ethylene oxide of 5 to 60, sugar fatty acid esters, sugar alcohol fatty acid esters, polyglycerin fatty acid esters, polyoxy Examples include ethylene higher alcohol ethers.
Examples of cationic surfactants include alkylammonium types, and examples of amphoteric surfactants include betaine types and imidazoline types.
The blending amount of the surfactant can be adjusted according to the form, purpose of use, and the like, for example, 0 to 10% for toothpaste and 0 to 5% for liquid toothpaste.
 甘味剤としては、サッカリンナトリウム等が挙げられ、着色剤としては、青色1号、黄色4号、二酸化チタン等が挙げられる。防腐剤としては、メチルパラベン、エチルパラベン等のパラオキシ安息香酸エステル、安息香酸又はその塩などが挙げられる。 Examples of sweeteners include sodium saccharin and the like, and examples of colorants include blue No. 1, yellow No. 4, and titanium dioxide. Examples of the preservative include paraoxybenzoic acid esters such as methyl paraben and ethyl paraben, 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、アニス油、ユーカリ油、ウィンターグリーン油、カシア油、クローブ油、タイム油、セージ油、レモン油、オレンジ油、ハッカ油、カルダモン油、コリアンダー油、マンダリン油、ライム油、ラベンダー油、ローズマリー油、ローレル油、カモミル油、キャラウェイ油、マジョラム油、ベイ油、レモングラス油、オリガナム油、パインニードル油、ネロリ油、ローズ油、ジャスミン油、グレープフルーツ油、スウィーティー油、柚油、イリスコンクリート、アブソリュートペパーミント、アブソリュートローズ、オレンジフラワー等の天然香料や、これら天然香料の加工処理(前溜部カット、後溜部カット、分留、液液抽出、エッセンス化、粉末香料化等)した香料、及び、メントール、カルボン、アネトール、シネオール、サリチル酸メチル、シンナミックアルデヒド、オイゲノール、3-l-メントキシプロパン-1,2-ジオール、チモール、リナロール、リナリールアセテート、リモネン、メントン、メンチルアセテート、N-置換-パラメンタン-3-カルボキサミド、ピネン、オクチルアルデヒド、シトラール、プレゴン、カルビールアセテート、アニスアルデヒド、エチルアセテート、エチルブチレート、アリルシクロヘキサンプロピオネート、メチルアンスラニレート、エチルメチルフェニルグリシデート、バニリン、ウンデカラクトン、ヘキサナール、ブタノール、イソアミルアルコール、ヘキセノール、ジメチルサルファイド、シクロテン、フルフラール、トリメチルピラジン、エチルラクテート、エチルチオアセテート等の単品香料、更に、ストロベリーフレーバー、アップルフレーバー、バナナフレーバー、パイナップルフレーバー、グレープフレーバー、マンゴーフレーバー、バターフレーバー、ミルクフレーバー、フルーツミックスフレーバー、トロピカルフルーツフレーバー等の調合香料等、口腔用組成物に用いられる公知の香料素材を組み合わせて使用することができるが、実施例記載の香料に限定されるものではない。
 また、配合量も特に限定されないが、上記の香料素材は、製剤組成中に0.000001~1%使用するのが好ましい。上記香料素材を使用した賦香用香料としては、製剤組成中に0.1~2%使用するのが好ましい。
Perfumes include peppermint oil, spearmint oil, anise oil, eucalyptus oil, winter green oil, cassia oil, clove oil, thyme oil, sage oil, lemon oil, orange oil, peppermint oil, cardamom oil, coriander oil, mandarin oil, Lime oil, lavender oil, rosemary oil, laurel oil, camomil oil, caraway oil, marjoram oil, bay oil, lemongrass oil, origanum oil, pine needle oil, neroli oil, rose oil, jasmine oil, grapefruit oil, sweetie Natural fragrances such as oil, bran oil, Iris concrete, absolute peppermint, absolute rose, orange flower, and processing of these natural fragrances (front reservoir cut, rear reservoir cut, fractional distillation, liquid-liquid extraction, essence, powder Perfumed, menthol, moss Bonn, Anethole, Cineol, Methyl salicylate, Synamic aldehyde, Eugenol, 3-l-Mentoxypropane-1,2-diol, Thymol, Linalol, Linarel acetate, Limonene, Menthone, Menthyl acetate, N-Substituted paramenthane 3-carboxamide, pinene, octylaldehyde, citral, pulegone, carbyl acetate, anisaldehyde, ethyl acetate, ethyl butyrate, allylcyclohexane propionate, methyl anthranilate, ethyl methyl phenyl glycidate, vanillin, undecalactone, Hexanal, butanol, isoamyl alcohol, hexenol, dimethyl sulfide, cycloten, furfural, trimethylpyrazine, ethyl lactate, ethyl thiol For oral compositions such as single flavors such as acetate, and other flavors such as strawberry flavor, apple flavor, banana flavor, pineapple flavor, grape flavor, mango flavor, butter flavor, milk flavor, fruit mix flavor, tropical fruit flavor, etc. Although it can be used combining the well-known fragrance | flavor raw material used, it is not limited to the fragrance | flavor of an Example description.
Further, the blending amount is not particularly limited, but the above fragrance material is preferably used at 0.000001 to 1% in the preparation composition. The flavoring fragrance using the fragrance material is preferably used in an amount of 0.1 to 2% in the preparation composition.
 有効成分としては、歯磨組成物に通常配合される公知のもの、例えば殺菌剤、抗炎症剤、酵素、フッ化物、植物抽出物、歯石防止剤、歯垢防止剤などを配合できる。例えば、イソプロピルメチルフェノール等の非イオン性殺菌剤、カチオン性殺菌剤、トラネキサム酸、イプシロンアミノカプロン酸、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化物などが挙げられる。なお、上記有効成分は、本発明の効果を妨げない範囲で有効量配合することができる。 As the active ingredient, known ingredients that are usually blended in dentifrice compositions, such as bactericides, anti-inflammatory agents, enzymes, fluorides, plant extracts, tartar inhibitors, dental plaque inhibitors, and the like can be blended. For example, nonionic fungicides such as isopropylmethylphenol, cationic fungicides, tranexamic acid, epsilon aminocaproic acid, anti-inflammatory agents such as allantoin, enzymes such as dextranase, sodium fluoride, sodium monofluorophosphate, etc. Fluoride etc. are mentioned. In addition, the said active ingredient can be mix | blended in an effective amount in 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。 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.
 [実施例、比較例]
 表1~3に示す組成の歯磨組成物(練歯磨)を常法によって調製し、下記方法で評価した。結果を表1~3に併記した。
 なお、歯磨組成物は、25℃におけるpHが7.0になるように調整した。
[Examples and Comparative Examples]
Dentifrice compositions (toothpaste) having the compositions shown in Tables 1 to 3 were prepared by a conventional method and evaluated by the following methods. The results are shown in Tables 1 to 3.
In addition, the dentifrice composition was adjusted so that pH in 25 degreeC might be set to 7.0.
<評価方法>
(1)象牙細管封鎖効果の評価方法
 Pashleyらの方法(J.Dent.Res.57,187-193,1987)に準じ、象牙細管の液の通過性を計測し、各歯磨組成物による象牙細管の封鎖の程度を評価した。
 ヒトの歯根から象牙質ブロックを切り出し、耐水研磨紙#2000で研磨を行って標本を作製し、サンプルとした。歯磨組成物3gと1mM相当のCaCl2及び3mM相当のKH2PO4を含むpH7.0の人工唾液6gとを混合して3倍希釈液とし、遠心分離して得た上澄を処置液とした。なお、3倍希釈は、歯磨き時に歯磨組成物が唾液によって希釈されることを想定したことによる。この処置液にサンプルを1分間浸漬し、蒸留水で濯いだ後、上記人工唾液中に37℃で12時間浸漬した。同様の操作を1日2回行い、この一連の操作を合計5日間繰り返した。最終日サンプルを蒸留水でよく濯ぎ、乾燥後、サンプルを固定し一定圧下で生理食塩水を流し、サンプルを通過する単位時間当たりの生理食塩水の量を測定して、処置液で処置前の通過量に対する、通過性抑制率を算出した(下記式)。評価はn=3で行い、その平均値を採用した。
 通過性抑制率(%)=
 ((処置前の液の通過量-処置後の液の通過量)/(処置前の液の通過量))×100
   通過量:10分間に通過する生理食塩水量(μL)
<Evaluation method>
(1) Evaluation method of dentinal tubule sealing effect According to the method of Pashley et al. (J. Dent. Res. 57, 187-193, 1987), the permeability of dentinal tubule fluid was measured, and dentinal tubules by each dentifrice composition The degree of blockade of was evaluated.
A dentin block was cut out from a human tooth root and polished with water-resistant abrasive paper # 2000 to prepare a sample, which was used as a sample. 3 g of dentifrice composition and 6 g of artificial saliva of pH 7.0 containing 1 mM of CaCl 2 and 3 mM of KH 2 PO 4 were mixed to make a 3-fold dilution, and the supernatant obtained by centrifugation was treated with the treatment liquid. did. The 3-fold dilution is based on the assumption that the dentifrice composition is diluted with saliva when brushing. The sample was immersed in this treatment solution for 1 minute, rinsed with distilled water, and then immersed in the artificial saliva at 37 ° C. for 12 hours. The same operation was performed twice a day, and this series of operations was repeated for a total of 5 days. Rinse the sample thoroughly with distilled water on the last day, and after drying, fix the sample, flush saline under constant pressure, measure the amount of saline per unit time passing through the sample, and treat with the treatment solution before treatment The permeability suppression rate with respect to the passage amount was calculated (the following formula). Evaluation was performed at n = 3, and the average value was adopted.
Passability suppression rate (%) =
((Amount of fluid before treatment -Amount of fluid after treatment) / (Amount of fluid before treatment)) × 100
Passage volume: Saline volume (μL) passing in 10 minutes
 得られた通過性抑制率の平均値から、下記の評価基準によって象牙細管封鎖の程度を判断し、象牙細管封鎖効果を評価した。
 象牙細管封鎖効果の評価基準;
  ◎:通過性抑制率が90%以上である
  ○:通過性抑制率が80%以上90%未満である
  △:通過性抑制率が60%以上80%未満である
  ×:通過性抑制率が60%未満である
The degree of dentinal tubule sealing was judged from the average value of the obtained permeability inhibition rate according to the following evaluation criteria, and the dentinal tubule sealing effect was evaluated.
Evaluation criteria for ivory tubule sealing effect;
A: The permeability inhibition rate is 90% or more. O: The permeability inhibition rate is 80% or more and less than 90%. Δ: The permeability inhibition rate is 60% or more and less than 80%. X: The permeability inhibition rate is 60. Less than%
(2)pH低下抑制効果の評価方法
 歯磨組成物の製造直後の25℃におけるpHを予め測定しておき、歯磨組成物をラミネートチューブに50g充填し、50℃で1ヶ月間保存した後のpHを測定した(25℃における値)。
 下記式からpH変化量を算出し、下記の評価基準によりpH低下の抑制効果を判定した。
 pH変化量=
 (調製直後の歯磨組成物のpH)-(50℃で1ヶ月間保存後の歯磨組成物のpH)
 pH低下の抑制効果の評価基準;
  ◎:pH変化量が0.5未満
  ○:pH変化量が0.5以上1.0未満
  △:pH変化量が1.0以上1.5未満
  ×:pH変化量が1.5以上
(2) Evaluation method of pH reduction inhibitory effect The pH after measuring the pH at 25 ° C. immediately after production of the dentifrice composition, filling the dentifrice composition in a laminate tube 50 g, and storing at 50 ° C. for 1 month. Was measured (value at 25 ° C.).
The amount of change in pH was calculated from the following formula, and the effect of suppressing the decrease in pH was determined according to the following evaluation criteria.
pH change =
(PH of dentifrice composition immediately after preparation) − (pH of dentifrice composition after storage at 50 ° C. for 1 month)
Evaluation criteria for inhibitory effect on pH decrease;
◎: pH change amount is less than 0.5 ○: pH change amount is 0.5 or more and less than 1.0 △: pH change amount is 1.0 or more and less than 1.5 ×: pH change amount is 1.5 or more
(3)使用感の評価方法
 (3-1)金属味のなさ
 歯磨組成物約1gを歯ブラシに取り、3分間歯磨きを行った際の金属味を、被験者10人が下記の評点基準により判定した。
 金属味のなさの評点基準;
  5点:全く感じない
  4点:やや感じる
  3点:感じる
  2点:強く感じる
  1点:非常に強く感じる
 10人の平均値を求め、下記の評価基準により金属味のなさを判定した。
 金属味のなさの評価基準;
  ◎:10人の平均点が4.0点以上
  ○:10人の平均点が3.0点以上4.0点未満
  △:10人の平均点が2.0点以上3.0点未満
  ×:10人の平均点が2.0点未満
(3) Evaluation method of use feeling (3-1) No metallic taste Ten subjects examined the metallic taste when taking about 1 g of a dentifrice composition on a toothbrush and brushing for 3 minutes according to the following rating criteria. .
Rating criteria for lack of metal taste;
5 points: I do not feel at all 4 points: I feel a little 3 points: I feel 2 points: I feel strongly 1 point: I feel very strong The average value of 10 people was determined, and the lack of metallic taste was determined according to the following evaluation criteria.
Evaluation criteria for lack of metal taste;
◎: Average score of 10 people is 4.0 points or more ○: Average score of 10 people is 3.0 points or more and less than 4.0 points △: Average score of 10 people is 2.0 points or more and less than 3.0 points × : Average score of 10 people is less than 2.0
 (3-2)オイル感のなさ
 歯磨組成物約1gを歯ブラシに取り、3分間歯磨きを行った際のオイル感を、被験者10人が下記の評点基準により判定した。
 オイル感のなさの評点基準;
  5点:全く感じない
  4点:やや感じる
  3点:感じる
  2点:強く感じる
  1点:非常に強く感じる
 10人の平均値を求め、下記の評価基準によりオイル感のなさを判定した。
 オイル感のなさの評価基準;
  ◎:10人の平均点が4.0点以上
  ○:10人の平均点が3.0点以上4.0点未満
  △:10人の平均点が2.0点以上3.0点未満
  ×:10人の平均点が2.0点未満
(3-2) No Oil Feeling About 10 g of the dentifrice composition was put on a toothbrush, and 10 subjects determined the oil feeling when brushing for 3 minutes according to the following rating criteria.
Grade criteria for lack of oil;
5 points: Not felt at all 4 points: Feels slightly 3 points: Feels 2 points: Feels strongly 1 point: Feels very strongly 10 averages were obtained and the lack of oil feeling was judged according to the following evaluation criteria.
Evaluation criteria for lack of oil feeling;
◎: Average score of 10 people is 4.0 points or more ○: Average score of 10 people is 3.0 points or more and less than 4.0 points △: Average score of 10 people is 2.0 points or more and less than 3.0 points × : Average score of 10 people is less than 2.0
 使用原料の詳細を下記に示す。
(A)乳酸アルミニウム;(株)武蔵野化学研究所製
(B)ピロリン酸ナトリウム;太平化学産業(株)製
(B)トリポリリン酸ナトリウム;太平化学産業(株)製
(C)α-オレフィンスルホン酸ナトリウム;ライオン・スペシャリティ・ケミカルズ(株)製
(D)硝酸カリウム;大塚化学(株)製
Details of the raw materials used are shown below.
(A) Aluminum lactate; Musashino Chemical Laboratory Co., Ltd. (B) Sodium pyrophosphate; Taihei Chemical Industrial Co., Ltd. (B) Sodium tripolyphosphate; Taihei Chemical Industrial Co., Ltd. (C) α-olefin sulfonic acid Sodium: Lion Specialty Chemicals Co., Ltd. (D) Potassium nitrate; Otsuka Chemical Co., Ltd.
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000003
Figure JPOXMLDOC01-appb-T000003
 以下、処方例を示す。なお、使用原料は上記と同様であり、製剤の25℃におけるpHは5~10の範囲内である。 The following are examples of prescriptions. The raw materials used are the same as described above, and the pH of the preparation at 25 ° C. is in the range of 5-10.
[処方例1]歯磨剤
(A)乳酸アルミニウム            2
(B)ピロリン酸ナトリウム          0.5
(C)α-オレフィンスルホン酸ナトリウム   1
(D)硝酸カリウム              5
フッ化ナトリウム               0.33
無水ケイ酸                 18
ラウリル硫酸ナトリウム            1.0
70%ソルビット液             25
プロピレングリコール             3
キサンタンガム                0.8
サッカリンナトリウム             0.2
香料                     1.2
水                     バランス 
計                    100.0%
[Formulation Example 1] Dentifrice (A) Aluminum lactate 2
(B) Sodium pyrophosphate 0.5
(C) Sodium α-olefin sulfonate 1
(D) Potassium nitrate 5
Sodium fluoride 0.33
Silicic anhydride 18
Sodium lauryl sulfate 1.0
70% sorbit solution 25
Propylene glycol 3
Xanthan gum 0.8
Saccharin sodium 0.2
Fragrance 1.2
Water balance
Total 100.0%
[処方例2]歯磨剤
(A)乳酸アルミニウム            1.5
(B)ピロリン酸ナトリウム          1
(C)α-オレフィンスルホン酸ナトリウム   1
(D)硝酸カリウム              5
モノフルオロリン酸ナトリウム         1.1
無水ケイ酸                 20
ラウリル硫酸ナトリウム            1.5
70%ソルビット液             30
プロピレングリコール             3
キサンタンガム                0.8
サッカリンナトリウム             0.3
香料                     1.4
水                     バランス 
計                    100.0%
[Prescription Example 2] Dentifrice (A) Aluminum lactate 1.5
(B) Sodium pyrophosphate 1
(C) Sodium α-olefin sulfonate 1
(D) Potassium nitrate 5
Sodium monofluorophosphate 1.1
Silicic anhydride 20
Sodium lauryl sulfate 1.5
70% sorbite solution 30
Propylene glycol 3
Xanthan gum 0.8
Saccharin sodium 0.3
Fragrance 1.4
Water balance
Total 100.0%

Claims (12)

  1.  (A)乳酸アルミニウムを0.01~5質量%と、(B)縮合リン酸塩を0.01~5質量%と、(C)α-オレフィンスルホン酸塩を0.1~3質量%とを配合したことを特徴とする歯磨組成物。 (A) 0.01-5% by mass of aluminum lactate, (B) 0.01-5% by mass of condensed phosphate, and (C) 0.1-3% by mass of α-olefin sulfonate. A dentifrice composition characterized by comprising
  2.  (B)成分の縮合リン酸塩が、ピロリン酸塩又はトリポリリン酸塩である請求項1記載の歯磨組成物。 The dentifrice composition according to claim 1, wherein the condensed phosphate of component (B) is pyrophosphate or tripolyphosphate.
  3.  (C)α-オレフィンスルホン酸塩が、炭素数14~16のα-オレフィンスルホン酸塩である請求項1又は2記載の歯磨組成物。 The dentifrice composition according to claim 1 or 2, wherein the (C) α-olefin sulfonate is an α-olefin sulfonate having 14 to 16 carbon atoms.
  4.  (B)/(A)が質量比として0.005~50、かつ(C)/(A)が質量比として0.05~100である請求項1~3のいずれか1項記載の歯磨組成物。 The dentifrice composition according to any one of claims 1 to 3, wherein (B) / (A) has a mass ratio of 0.005 to 50, and (C) / (A) has a mass ratio of 0.05 to 100. object.
  5.  更に、(D)硝酸カリウムを0.1~7質量%配合した請求項1~4のいずれか1項記載の歯磨組成物。 The dentifrice composition according to any one of claims 1 to 4, further comprising (D) 0.1 to 7% by mass of potassium nitrate.
  6.  25℃におけるpHが5以上である請求項1~5のいずれか1項記載の歯磨組成物。 The dentifrice composition according to any one of claims 1 to 5, wherein the pH at 25 ° C is 5 or more.
  7.  練歯磨剤に調製された請求項1~6のいずれか1項記載の歯磨組成物。 The dentifrice composition according to any one of claims 1 to 6, which is prepared as a toothpaste.
  8.  (A)乳酸アルミニウムを0.01~5質量%含有する歯磨組成物に、(B)縮合リン酸塩を0.01~5質量%と、(C)α-オレフィンスルホン酸塩を0.1~3質量%とを配合し、前記歯磨組成物におけるpH低下と金属味の発現を抑制する方法。 (A) A dentifrice composition containing 0.01-5% by mass of aluminum lactate, (B) 0.01-5% by mass of condensed phosphate, and (C) 0.1% of α-olefin sulfonate. A method for suppressing the decrease in pH and the appearance of metallic taste in the dentifrice composition by blending ˜3 mass%.
  9.  (B)/(A)が質量比として0.005~50、かつ(C)/(A)が質量比として0.05~100である請求項8記載の歯磨組成物におけるpH低下と金属味の発現を抑制する方法。 9. The pH reduction and metallic taste of the dentifrice composition according to claim 8, wherein (B) / (A) is 0.005 to 50 in terms of mass ratio and (C) / (A) is in the range of 0.05 to 100. To suppress the expression of.
  10.  更に、(D)硝酸カリウムを0.1~7質量%配合する請求項8又は9記載の歯磨組成物におけるpH低下と金属味の発現を抑制する方法。 Furthermore, (D) The method for suppressing a decrease in pH and expression of metallic taste in a dentifrice composition according to claim 8 or 9, wherein 0.1 to 7% by mass of potassium nitrate is blended.
  11.  歯磨組成物が、25℃におけるpHが5以上である請求項8~10のいずれか1項記載の歯磨組成物におけるpH低下と金属味の発現を抑制する方法。 11. The method for suppressing pH reduction and expression of metallic taste in a dentifrice composition according to any one of claims 8 to 10, wherein the dentifrice composition has a pH of 5 or more at 25 ° C.
  12.  練歯磨剤に調製する、請求項8~11のいずれか1項記載の歯磨組成物におけるpH低下と金属味の発現を抑制する方法。 A method for suppressing a decrease in pH and expression of a metallic taste in a dentifrice composition according to any one of claims 8 to 11, which is prepared as a toothpaste.
PCT/JP2016/051874 2015-01-26 2016-01-22 Dentifrice composition WO2016121650A1 (en)

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JP7031253B2 (en) * 2017-11-29 2022-03-08 ライオン株式会社 Toothpaste composition
JP7264620B2 (en) * 2017-12-27 2023-04-25 花王株式会社 oral composition
JP7388126B2 (en) * 2018-11-01 2023-11-29 ライオン株式会社 Oral composition

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