WO2019034387A1 - Procédé pour favoriser la reminéralisation des dents - Google Patents

Procédé pour favoriser la reminéralisation des dents Download PDF

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Publication number
WO2019034387A1
WO2019034387A1 PCT/EP2018/070307 EP2018070307W WO2019034387A1 WO 2019034387 A1 WO2019034387 A1 WO 2019034387A1 EP 2018070307 W EP2018070307 W EP 2018070307W WO 2019034387 A1 WO2019034387 A1 WO 2019034387A1
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WIPO (PCT)
Prior art keywords
clay
fluoride
chloride
teeth
external surface
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PCT/EP2018/070307
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English (en)
Inventor
Sembian CHANDRASEKARAN
Meenakshi IYER
Neha TRIVEDI
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Unilever N.V.
Unilever Plc
Conopco, Inc., D/B/A Unilever
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Application filed by Unilever N.V., Unilever Plc, Conopco, Inc., D/B/A Unilever filed Critical Unilever N.V.
Priority to CN201880053225.XA priority Critical patent/CN110997071B/zh
Priority to EP18742826.3A priority patent/EP3668605A1/fr
Publication of WO2019034387A1 publication Critical patent/WO2019034387A1/fr

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0241—Containing particulates characterized by their shape and/or structure
    • A61K8/0254—Platelets; Flakes
    • A61K8/0258—Layered structure
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/20—Halogens; Compounds thereof
    • A61K8/21—Fluorides; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/26—Aluminium; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/4906—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with one nitrogen as the only hetero atom
    • A61K8/4926—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with one nitrogen as the only hetero atom having six membered rings
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/60—Particulates further characterized by their structure or composition
    • A61K2800/61—Surface treated
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/60—Particulates further characterized by their structure or composition
    • A61K2800/65—Characterized by the composition of the particulate/core
    • A61K2800/651—The particulate/core comprising inorganic material

Definitions

  • the present invention relates to oral care compositions for remineralisation of teeth.
  • Dental caries or cavities are fairly common and in a general sense they are known as tooth decay. Dental caries is caused by demineralisation of the enamel.
  • Fluoride ions partially fluoridate hydroxyapatite and simultaneously repair the lattice irregularities to improve the remineralisation process.
  • the effectiveness of fluoride depends upon the amount of fluoride ions available for deposition on the enamel. Therefore, it is desirable to increase or enhance the inherent anti caries action of fluorides so that the oral composition can do more remineralisation.
  • US4455293 B (Harvey et al., 1984) discloses a stable dentifrice formulation having a polishing agent comprising alkali metal aluminosilicate and a stabilising amount of mono-fluorophosphate ion.
  • compositions containing calcined kaolins have better rheological properties.
  • Compositions disclosed in this publication contain calcined kaolin, talc and titanium dioxide as primary ingredients.
  • the compositions also contain a source of fluoride.
  • US4064231 A (Kao Corp, 1977) discloses a dentifrice composition comprising a water- soluble fluoride and 0.3 to 13 wt% montmorillonite or hectorite having a specific composition leads to reduction of the water-soluble fluoride concentration in the dentifrice with the passage of time.
  • US4122163 A (Advanced Research & Technology Institute, 1978) discloses new and more effective dentifrice preparations containing calcined kaolin (a 1 :1 clay) for abrasion and a source of fluoride.
  • An example formulation contains Veegum® which is a 2:1 clay and trisodium citrate as the abrasive.
  • Fluorides tend to deactivate and be rendered unavailable by other ingredients in toothpaste, particularly the abrasives. Therefore, it is desirable that the performance of the source of fluoride ions, such as sodium monofluorophosphate, is improved to maximise the benefits.
  • a bipolar composite particle as disclosed hereinafter is able to increase or augment the efficacy of fluorides for more remineralisation of teeth.
  • bipolar composite material comprising:
  • a clay whose precursor is an asymmetric 1 :1 or 2:1 :1 clay particle comprising alternating tetrahedral and octahedral sheets terminating with a tetrahedral sheet at one external surface plane and an octahedral sheet at another;
  • an oral care composition further comprising at least one source of fluoride ions, for use in promoting remineralization of teeth.
  • a method of promoting remineralization of teeth by applying to said teeth an oral care composition comprising a bipolar composite material and further comprising at least one source of fluoride ions, wherein said material comprises: (i) a clay whose precursor is an asymmetric 1 :1 or 2:1 :1 clay particle, comprising alternating tetrahedral and octahedral sheets terminating with a tetrahedral sheet at one external surface plane and an octahedral sheet at another; and,
  • a bipolar composite material comprising:
  • a clay whose precursor is an asymmetric 1 :1 or 2:1 :1 clay particle comprising alternating tetrahedral and octahedral sheets terminating with a tetrahedral sheet at one external surface plane and an octahedral sheet at another;
  • composition for promoting remineralisation of teeth, where said composition further comprises at least one source of fluoride ions.
  • the invention disclosed in this application discloses a non-obvious solution to the problem, whilst still retaining the essential functional and consumer-relevant attributes of the oral care compositions.
  • the problem has been solved by identifying a new use of the antimicrobial particle.
  • the solution in the present invention lies in the inclusion of the bipolar composite material which acts as a carrier of the cationic antimicrobial agent.
  • the composite material is based on an inert material which does not affect important properties of the oral care
  • compositions In W014102032A1 , the Applicant has disclosed that the composite bipolar material is highly effective at controlling re-growth of bacteria, as well as at providing immediate control on the bacterial count.
  • median particle size (D50) of this material is 0.1 to 10 ⁇ , more preferably 0.4 to 1 ⁇ and most preferably 0.5 to 0.8 ⁇ . Without being bound by theory, it is believed that this makes more effective use of the antimicrobial agent, thereby providing opportunity for substantial reduction in dosage of the antibacterial agent. While conventional antibacterial agents need an optimised dosage of 0.2 to 0.5 wt%, the antibacterial agent, delivered in the form of the bipolar antibacterial material, is effective even at an (actual) dosage of 0.02 wt% of the oral care compostion, insofar as the antimicrobial effect is concerned.
  • Particle size distribution is also known as the median diameter or the medium value of the particle size distribution, it is the value of the particle diameter at 50 percent in the cumulative distribution. For example, if D50 is 5.8 ⁇ , then 50 % of the particles in the sample are larger than 5.8 ⁇ and 50 percent smaller than 5.8 ⁇ . D50 is usually used to represent the particle size of group of particles. The D50 is the size in microns that splits the distribution with half above and half below this diameter.
  • the precursor of the clay is an asymmetric 1 :1 clay particle.
  • Preferred 1 :1 clays include kaolinite and serpentine subgroups of minerals.
  • the species included within the kaolinite subgroup include but are not limited to kaolinite, dickite, halloysite and nacrite.
  • the species within the serpentine subgroup include but are not limited to chrysolite, lizardite, and amesite.
  • the precursor of the clay is an asymmetric 2:1 :1 clay particle.
  • Preferred 2:1 :1 clays include chlorite group of minerals.
  • the chlorite comprises tetrahedral-octahedral-tetrahedral sheets like 2:1 clays, with an extra weakly bound brucite like layer between tetrahedral layers.
  • the tetrahedral sheet preferably comprises coordinating tetrahedral cations of silicon.
  • the tetrahedral sheet may also include isomorphously substituted coordinating tetrahedral cations which are not silicon. Isomorphously substituted coordinating tetrahedral cations include, but are not limited to, cations of aluminum, iron or boron. It is preferred that the octahedral sheet has coordinating octahedral cations of aluminum.
  • the octahedral sheet may also comprise isomorphously substituted coordinating octahedral cations which are not aluminium.
  • Isomorphously substituted coordinating octahedral cations include cations of magnesium and iron.
  • the antimicrobial agent is attached to the coordinating cations on the exterior side of one of the external surface planes. Accordingly, the antimicrobial agent is attached to coordinating cations on the exterior side of the tetrahedral sheet. Alternatively, the antimicrobial molecule is attached to the coordinating cations on the exterior side of the octahedral sheet.
  • Coordinating cations on the exterior side of each of the tetrahedral and the octahedral surface sheets are attached to the antimicrobial agent, with the proviso that the antimicrobial agent attached to the coordinating cations on the exterior side of the tetrahedral surface sheet is not identical to the molecule attached to the coordinating cations on the exterior side of the octahedral surface sheet.
  • the antimicrobial agent is preferably attached to the coordinating cations on the external surface of the octahedral surface plane and is not preferably attached to coordination cations of non-exterior tetrahedral or octahedral plane or on the interior side of the surface sheets.
  • the ratio of the clay: antimicrobial agent is from 1 :0.001 to 1 :1 , more preferably from 1 :0.001 and 1 :0.1 parts by weight of the bipolar composite material.
  • the antibacterial agent is attached to coordinating cations on the external surface of the octahedral surface plane.
  • oral care compositions of the invention comprise 0.1 to 10 wt% of the bipolar antimicrobial material, more preferably 0.5 to 5 wt% material.
  • the quaternary ammonium compound is one or more of cetylpyridinium chloride (CPC), cetyltrimethylammonium chloride (CTAC), cetyltrimethylammonium bromide (CTAB), benzalkonium chloride (BKC), benzethonium chloride, cetrimide, quaternium, tetrabutyl ammonium bromide, undecylenamido propyltrimonium methosulphate, methylbenzethonium chloride, cetethyldimonium bromide,
  • cetromonium tosylate cocotrimonium chloride, dodecylbenzyltrimonium chloride, lauryl isoquinolium bromide, laurylpyridinium chloride, dequalinium chloride or domiphen bromide.
  • cetylpyridinium chloride CPC
  • the primary activity is linked to the cationic charge of its amine group.
  • cetylpyridinium chloride is attracted to and binds to negatively-charged protein moieties on the cell membrane or cell wall of the microorganism and to tooth surfaces which are also typically negatively charged.
  • precursor of the clay is a 1 :1 clay particle. Further preferably the precursor of the clay is kaolinite. It is particularly preferred that the antimicrobial quaternary ammonium compound is cetyl pyridinium chloride. It is further particularly preferred that when the precursor of the clay is kaolinite, the antimicrobial quaternary ammonium compound is cetyl pyridinium chloride.
  • the use in accordance with the invention is for non- therapeutic purpose. More particularly it is for cosmetic purpose.
  • teeth develop stains owing to prolonged use of such compositions comprising in particular, cetylpyridinium chloride, it is not a pathological state, but rather a bodily condition which is cosmetic or aesthetic in nature.
  • the oral care composition is a toothpaste.
  • the oral care composition is a mouthwash.
  • Other known forms include toothpowder, chewing gums and lozenges, strips and gels.
  • the toothpaste comprises at least one of calcium-based abrasive or silica- based abrasive.
  • Toothpastes are also known as dentifrices.
  • the term "dentifrice” generally denotes formulations which are used to clean the surfaces of the oral cavity.
  • the dentifrice is an oral composition that is not intentionally swallowed for purposes of systemic administration of therapeutic agents, but is applied to the oral cavity, used to treat the oral cavity and then expectorated.
  • the dentifrice is used in conjunction with a cleaning implement such as a toothbrush, usually by applying it to the bristles of the toothbrush and then brushing the accessible surfaces of the oral cavity.
  • the dentifrice is in the form of a paste or a gel (or a combination thereof).
  • An oral care composition according to the invention will usually contain a liquid continuous phase in an amount of from 40 to 99% by weight based on the total weight of the dentifrice.
  • a liquid continuous phase will typically comprise a mixture of water and polyhydric alcohol in various relative amounts, with the amount of water generally ranging from 10 to 45% by weight (based on the total weight of the dentifrice) and the amount of polyhydric alcohol generally ranging from 30 to 70% by weight (based on the total weight of the dentifrice).
  • Humectants are generally included in toothpastes for a soft, supple mouth feel.
  • Humectants also reduce the tendency of toothpastes to lose moisture.
  • Preferred toothpaste compositions contain 3.5 to 40 wt% humectants. Further preferred compositions have 10 to 40 wt%, more particularly 10 to 20 wt% humectants.
  • a particularly preferred humectant is sorbitol, generally available as 70% aqueous solution.
  • Other preferred humectants include glycerine, maltitol and xylitol.
  • More preferred toothpastes contain glycerine and sorbitol for a lubricated mouth feel, but their cumulative levels should not exceed the disclosed upper limit. Lower humectant content provides an effective way to reduce the cost of the product.
  • the oral care compositions of the invention comprise a source of fluoride.
  • the source of fluoride is stannous fluoride, sodium fluoride, potassium fluoride, sodium monofluorophosphate, sodium fluorosilicate, ammonium fluorosilicate, amine fluoride, ammonium fluoride, and combinations thereof.
  • the source of fluoride is a soluble fluoride salt that provides a source of fluoride ions. Any orally acceptable fluoride salt or combination of salts may be used. It is particularly preferred that the source is sodium monofluorophosphate.
  • the toothpaste composition in accordance with the present invention may include free fluoride ion in a range of 1 ,000 to 20,000 ppm by weight of the composition.
  • free fluoride ion concentration in a toothpaste composition for general consumer use would typically range from 1000 to 15000 ppm by weight of the composition.
  • Source of fluoride is preferably added to the composition of the disclosed invention at a level of about 0.01 wt% to 10 wt%, more preferably 0.03 to 5 wt%, still more preferably 0.1 to 2 wt% and most preferably from 0.15 to 1wt% of the composition.
  • the weight of the source of fluoride which is typically a fluoride salt, to provide the appropriate levels of the free fluoride ion will vary depending on the weight of the counter ion in the salt.
  • An oral care composition according to the invention will generally contain further ingredients to enhance performance and/or consumer acceptability such as abrasive cleaning agent, binder or thickening agent, and surfactant.
  • a dentifrice will usually comprise an abrasive cleaning agent in an amount of from 3 to 75% by weight based on the total weight of the dentifrice.
  • Suitable abrasive cleaning agents include silica xerogels, hydrogels and aerogels and precipitated particulate silicas; calcium carbonate, dicalcium phosphate, tricalcium phosphate, calcined alumina, sodium and potassium metaphosphate, sodium and potassium pyrophosphates, sodium trimetaphosphate, sodium hexametaphosphate, particulate hydroxyapatite and mixtures thereof.
  • abrasives examples include abrasive amorphous silica particles which have a weight mean particle size (d50) ranging from 3 to 15 microns.
  • Preferred abrasive amorphous silica particles for use in the composition of the invention have a weight mean particle size in the range 3 to 6 microns.
  • the abrasive amorphous silica particles employed are precipitated silica.
  • Suitable precipitated silicas for use as abrasive amorphous silica particles in the invention are commercially available and include those marketed by PQ Corporation under the trade names SORBOSIL® AC 43, AC77, AC35 and SORBOSIL® AC 33. Mixtures of any of the above described materials may also be used.
  • the level of abrasive amorphous silica particles generally ranges from 0.05 to 5%, preferably from 0.1 to 3%, more preferably from 0.2 to 0.8%, by total weight abrasive amorphous silica particles (as defined above) based on the total weight of the composition.
  • the compositions of the invention comprise calcium-based abrasive.
  • a particularly preferred abrasive is fine ground natural chalk (FGNC). It is obtained from limestone or marble.
  • FGNC may also be modified chemically or physically by coating during or after milling by heat treatment. Typical coating materials include magnesium stearate and oleate.
  • FGNC may also be modified during the milling process by using different milling techniques, for example, ball milling, air-classifier milling or spiral jet milling.
  • FGNC can be used as the sole calcium containing abrasive.
  • FGNC can also be used with other calcium containing abrasives to balance the abrasion.
  • Other preferred calcium containing abrasives include dicalcium phosphate (DCP), calcium pyrophosphate and precipitated calcium carbonate (PCC).
  • FGNC is 35 to 100 %, more preferably 75 to 100 % and especially from 95 to 100 % of the total abrasive. In such cases, the balance, most preferably, is PCC.
  • compositions of the invention preferably comprise a binder or thickening agent in an amount of from 0.5 to 10% by weight based on the total weight of the dentifrice.
  • Suitable binders or thickening agents include carboxyvinyl polymers (such as polyacrylic acids cross-linked with polyallyl sucrose or polyallyl
  • compositions of the invention preferably comprise a surfactant in an amount of from 0.2 to 10% by weight based on the total weight of the dentifrice.
  • Suitable surfactants include anionic surfactants, such as the sodium, magnesium, ammonium or ethanolamine salts of C8 to C18 alkyl sulphates (for example sodium lauryl sulphate), C8 to C18 alkyl sulphosuccinates (for example dioctyl sodium sulphosuccinate), C8 to C18 alkyl sulphoacetates (such as sodium lauryl sulphates), C8 to C18 alkyl sulphosuccinates (for example dioctyl sodium sulphosuccinate), C8 to C18 alkyl sulphoacetates (such as sodium lauryl anionic surfactants, such as the sodium, magnesium, ammonium or ethanolamine salts of C8 to C18 alkyl sulphates (for example sodium lauryl sulphate), C8 to C18 alkyl sulphosuccinates (for example dioctyl sodium sulphosuccinate), C8 to
  • sulphoacetate C8 to C18 alkyl sarcosinates (such as sodium lauryl sarcosinate), C8 to C18 alkyl phosphates (which can optionally comprise up to 10 ethylene oxide and/or propylene oxide units) and sulphated monoglycerides.
  • suitable surfactants include nonionic surfactants, such as optionally polyethoxylated fatty acid sorbitan esters, ethoxylated fatty acids, esters of polyethylene glycol, ethoxylates of fatty acid monoglycerides and diglycerides, and ethylene oxide/propylene oxide block polymers.
  • suitable surfactants include amphoteric surfactants, such as betaines or sulphobetaines. Mixtures of any of the above described materials may also be used.
  • oral care compositions of the invention include a smectite clay which is in addition to the clay present by way of the bipolar antimicrobial material.
  • Smectites constitute a group in the class of natural aluminosilicate minerals known as
  • Preferred smectite clay is selected from
  • montmorillonites bentonites, hectorites and derivatives thereof
  • purified aluminium magnesium silicates variant grades are commercially available as VEEGUM (R) from R. T. Vanderbilt Company
  • purified sodium magnesium silicates commercially available as LAPONITE (R) in various grades
  • organically modified smectites including tetra alkyl and/or trialkyl ammonium smectites organically modified montmorillonite clays
  • Aluminium magnesium silicate clays are particularly preferred.
  • An example is VEEGUM (R) HV. The clay tends to swell when exposed to water.
  • Preferred toothpaste compositions contain 0.2 to 3 wt percent clay. More preferred compositions include 0.5 to 1 wt percent clay.
  • compositions of the invention further preferably comprise a zinc salt, preferably zinc sulphate or zinc chloride, more preferably zinc sulphate heptahydrate.
  • a zinc salt preferably zinc sulphate or zinc chloride, more preferably zinc sulphate heptahydrate.
  • the level of zinc salt is from 0.05 to 1.0 wt% of the total composition more preferably from 0.1 to 0.5 wt%.
  • compositions of the invention may comprise a preservative, a preferred preservative is sodium benzoate.
  • the level of preservative is from 0.1 to 1 wt% of the total composition. It is preferred that pH of the composition at 20 °C is from 4 to 10, more preferably 7 to 9.
  • compositions of the invention may also comprise a deposition aid.
  • deposition aid in the context of this invention generally means a material which further aids deposition of whitening agents from the composition.
  • An example is polystyrene sulphonates.
  • Another example is Gantrez® polymers.
  • mouthwash generally denotes liquid formulations which are used to rinse the surfaces of the oral cavity and provide the user with a sensation of oral cleanliness and refreshment.
  • the mouthwash is an oral composition that is not intentionally swallowed for purposes of systemic administration of therapeutic agents, but is applied to the oral cavity, used to treat the oral cavity and then expectorated.
  • a mouthwash composition will usually contain an aqueous continuous phase.
  • the amount of water generally ranges from 70 to 99% by weight based on the total weight of the mouthwash.
  • a mouthwash composition according to the invention will generally contain further ingredients to enhance performance and/or consumer acceptability, such as the humectants and surfactants mentioned above for dentifrices.
  • the amount of humectant generally ranges from 5 to 20% by weight based on the total weight of the mouthwash and the amount of surfactant generally ranges from 0.1 to 5% by weight based on the total weight of the mouthwash.
  • compositions of the present invention (such as in particular dentifrices or
  • mouthwashes may also contain further optional ingredients customary in the art such as fluoride ion sources, anticalculus agents, buffers, flavouring agents, sweetening agents, colouring agents, opacifying agents, preservatives, antisensitivity agents and antimicrobial agents.
  • fluoride ion sources such as fluoride ion sources, anticalculus agents, buffers, flavouring agents, sweetening agents, colouring agents, opacifying agents, preservatives, antisensitivity agents and antimicrobial agents.
  • composition in the context of this invention typically involves application of the composition to the oral cavity, for a recommended time, before being expectorated.
  • the preferred time application time being from 10 to 60 seconds.
  • the bipolar composite material contained kaolinite and cetyl pyridinuim chloride in an amount which made the final amount of CPC to 0.045 wt% by weight of the total toothpaste composition. D50 of the material was 0.5 ⁇ .
  • the material was made in accordance with Example 1 of US2012/0177712 A1 (Unilever).
  • CPC cetyl pyridinium chloride
  • the toothpaste composition (inventive) of Table 1 was subject to a test to determine its efficacy towards remineralisation of teeth.
  • a marketed chalk-based toothpaste containing fluoride and arginine was also subjected to the same test.
  • Enamel specimens obtained from human permanent teeth were used as the hard tissue test substrate.
  • the teeth were sorted and cleaned. Selection of the tooth for further processing was based on the quality of the enamel and whether the particular tooth surface had sufficient size to obtain a large enough specimen to meet the study requirements. Tooth sections with white spots, cracks and other defects were rejected.
  • the tooth sections were cut into 3 x 3 mm specimens using a low-speed saw.
  • the teeth were stored in thymol during the sample preparation process.
  • the 3 x 3 mm specimens were ground and polished to create flat surfaces to facilitate surface micro hardness testing using a polishing unit.
  • the bottom side of the specimens was ground flat to a uniform thickness with 500-grit silicone carbide grinding paper.
  • the topside of the specimen was ground using 1200-grit paper until most of the tooth surface was flattened.
  • the specimens were serially polished using 4000-grit paper followed by 1 mm diamond polishing suspension. Specimens had at least 0.3 mm of enamel thickness.
  • the specimens were sonicated in de-ionized water between each grinding/polishing step. As a final cleaning step, the polished specimens were sonicated in 2 % microliquid.
  • the specimens were assessed with a magnification of 10X. To be accepted for the study the specimens were required to: not have any obvious cracks or other flaws in the enamel surface; b) have an evenly polished, high gloss enamel surface; c) have no contamination on the top surface from sticky wax or any other material.
  • Each specimen was mounted on an acrylic plate using wax. The sides of each specimen were covered with a varnish so that only the enamel surface was exposed. On the enamel surface, a sound reference area of approximately 3 mm x 1 mm was created on the specimens using acid-resistant, clear nail varnish.
  • the extent of fluorescence loss in the lesions was determined using QLF. All specimens were air-dried for at least 30 minutes before QLF measurements were performed using the QLF-D Biluminator 2 (Inspektor Research, the Netherlands). The clear nail varnish used to protect the sound enamel reference area was not removed, renewed or otherwise altered prior to basline QLF measurements (figure). Acquired QLF images were analyzed using the dedicated QLF Analysis software. AFbase values were recorded and at a threshold level of 5%, i.e. a minimum of 5% fluorescence loss between sound (i.e. the sound enamel area covered by nail varnish) and uncovered demineralized enamel (i.e. the experimental window). The distance between the camera and the surface of the specimen was kept constant throughout the experiment to facilitate repeat measurements.
  • Treatment Phase Saliva Collection A 50:50 (7.5 ml human + 7.5 ml mineral mix) mixture of pooled, human saliva and a mineral solution (2.20 g/L Gastric Mucin, 0.381 g/L NaCI, 0.213 g/L CaCI2-2H20, 0.738 g/L KH2P04, 1.1 14 g/L KCI) was used as the remineralization medium in all treatment regimens. Wax-stimulated saliva was collected from at least five individuals, pooled and refrigerated until use. Saliva samples were then warmed to room temperature and thoroughly mixed prior to distribution into 30 ml treatment beakers. Fresh saliva/mineral mix was used each day (changed during the acid challenge period).
  • the cyclic treatment regimen consisted of a 4 hours/day acid challenge in the lesion forming solution and four, one-minute treatment periods.
  • Each group was prepared by adding 5 g of the toothpaste to 10 ml of fresh saliva in a beaker with a magnetic stirrer. A fresh treatment for each subgroup was prepared just prior to each treatment. All treatments were stirred at 350 rpm. After the treatments, the specimens were rinsed with running deionized water. All specimens were then placed back into saliva. The remaining time (-20 hours) the specimens were in the saliva mixture, remineralization system. The regimen was repeated for 20 days. The treatment schedule for this experiment is given in the table below: On the first day, this treatment was not given; the test began with one hour in saliva to permit pellicle development prior to any treatments.
  • the fluoride content of each enamel specimen was determined using the microdrill technique to a depth of 100 ⁇ .
  • the diameter of the drill hole was determined.
  • the enamel powder from the drill hole was collected, dissolved (20 ⁇ of HCI0 4 , 40 ⁇ Citrate/EDTA Buffer and 40 ⁇ Dl water) and analyzed for fluoride by comparison to a similarly prepared standard curve. Fluoride data was calculated as ⁇ g F/cm3: ⁇ g F X dilution factor - volume of drilling).
  • compositions of Table 3 were compared against each other. Only the Composition 1 was inside the invention. The observations are also summarised in Table 3. Demineralisation
  • the toothpaste slurry was prepared by mixing one part of toothpaste composition with three parts of deionised water having 10 UI/mL alkaline phosphatase.
  • the acidic buffer was prepared by mixing 50 mmol/L acetic acid and 1.5 mmol/L KH2P04; pH5.0.
  • the neutral buffer was prepared by mixing 20 mmol/L HEPES and 1 .5 mmol/L KH2PO4; pH 7. This cycle was repeated 12 times.
  • Teeth sample was washed after each step to thoroughly rinse off the active agents from the previous steps. Efficacy was assessed by micro-hardness analysis of the teeth sample, before and after pH-cycling.
  • the teeth sample was demineralised for 10 days in a gel system prepared from equal parts of 8 percent methyl cellulose and lactic acid, at 37 degrees centigrade and a pH 4.6. After demineralisation. each teeth sample was indented in order to obtain the Hardness Knoop value of the teeth sample.
  • teeth sample were subjected to a pH-cycling regime as follows: First the teeth sample was immersed for 5 minutes in toothpaste slurry. The toothpaste slurry was prepared by mixing 1 part of toothpaste composition with 3 parts of deionised water having 10 UI/mL alkaline phosphatase. Next the teeth sample was immersed for 30 minutes in an acidic buffer. The acidic buffer was prepared by mixing 50 mmol/L acetic acid, 1.5 mmol/L calcium chloride dihydrate, 0.9 mmol/L potassium dihydrogen orthophosphate and 130 mmol/L potassium chloride, pH 5.0).

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  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
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  • Epidemiology (AREA)
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Abstract

Un matériau composite bipolaire comprenant : (i) une argile dont le précurseur est une particule d'argile 1:1 ou 2:1:1 asymétrique, comprenant des feuilles tétraédriques et octaédriques alternées se terminant avec une feuille tétraédrique sur un plan de surface externe et une feuille octaédrique sur l'autre; et, (ii) un composé d'ammonium quaternaire antimicrobien fixé à un cation de coordination sur l'un desdits plans de surface externe, dans une composition de soin bucco-dentaire, comprenant en outre au moins une source d'ions fluorure, destiné à être utilisé pour favoriser la reminéralisation des dents.
PCT/EP2018/070307 2017-08-17 2018-07-26 Procédé pour favoriser la reminéralisation des dents WO2019034387A1 (fr)

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WO2021078685A1 (fr) 2019-10-23 2021-04-29 Unilever Ip Holdings B.V. Procédé de réduction de l'hypersensibilité dentaire
WO2021104780A1 (fr) * 2019-11-28 2021-06-03 Unilever Ip Holdings B.V. Compositions antimicrobiennes comprenant de l'argile modifiée et des copolymères
WO2021259748A1 (fr) * 2020-06-24 2021-12-30 Unilever Ip Holdings B.V. Compositions comprenant du zinc et un agent antimicrobien
US11857655B2 (en) 2018-12-21 2024-01-02 Conopco. Inc. Antimicrobial compositions comprising modified clay and nonionic triblock copolymers

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US4455293A (en) 1981-11-19 1984-06-19 Colgate-Palmolive Company Stable dentifrice containing neutral siliceous polishing agent
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US4064231A (en) 1975-09-04 1977-12-20 Kao Soap Co., Ltd. Dentifrice composition
US4122163A (en) 1976-08-02 1978-10-24 Indiana University Foundation Dentifrice preparation comprising purified, calcined kaolin abrasives
US4455293A (en) 1981-11-19 1984-06-19 Colgate-Palmolive Company Stable dentifrice containing neutral siliceous polishing agent
EP0102695A2 (fr) 1982-06-28 1984-03-14 Indiana University Foundation Composition dentifrice comprenant des abrasifs du type kaolin calciné
WO2011036031A1 (fr) * 2009-09-24 2011-03-31 Unilever Nv Particule antimicrobienne et son procédé de préparation
US20120177712A1 (en) 2009-09-24 2012-07-12 Arpita Bhattacharya antimicrobial particle and a process for preparing the same
WO2014102032A1 (fr) 2012-12-27 2014-07-03 Unilever N.V. Composition de soin buccal comportant un adduit d'argile et un agent antibactérien
WO2017108368A1 (fr) * 2015-12-22 2017-06-29 Unilever N.V. Composition de dentifrice

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11857655B2 (en) 2018-12-21 2024-01-02 Conopco. Inc. Antimicrobial compositions comprising modified clay and nonionic triblock copolymers
WO2021078685A1 (fr) 2019-10-23 2021-04-29 Unilever Ip Holdings B.V. Procédé de réduction de l'hypersensibilité dentaire
WO2021104780A1 (fr) * 2019-11-28 2021-06-03 Unilever Ip Holdings B.V. Compositions antimicrobiennes comprenant de l'argile modifiée et des copolymères
CN114746063A (zh) * 2019-11-28 2022-07-12 联合利华知识产权控股有限公司 包含改性粘土和共聚物的抗微生物组合物
WO2021259748A1 (fr) * 2020-06-24 2021-12-30 Unilever Ip Holdings B.V. Compositions comprenant du zinc et un agent antimicrobien

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