US20100143423A1 - Oral care product - Google Patents

Oral care product Download PDF

Info

Publication number
US20100143423A1
US20100143423A1 US12/517,365 US51736507A US2010143423A1 US 20100143423 A1 US20100143423 A1 US 20100143423A1 US 51736507 A US51736507 A US 51736507A US 2010143423 A1 US2010143423 A1 US 2010143423A1
Authority
US
United States
Prior art keywords
composition
oral care
care product
teeth
product according
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Abandoned
Application number
US12/517,365
Other languages
English (en)
Inventor
Michael Francis Butler
Yan Deng
Mary Heppenstall-Butler
Andrew Joiner
Haiyan Li
Xiaoke Li
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Conopco Inc
Original Assignee
Conopco Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=39092967&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=US20100143423(A1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Conopco Inc filed Critical Conopco Inc
Assigned to CONOPCO, INC. D/B/A UNILEVER reassignment CONOPCO, INC. D/B/A UNILEVER ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BUTLER, MICHAEL FRANCIS, HEPPENSTALL-BUTLER, MARY, LI, HAIYAN, DENG, YAN, LI, XIAOKE, JOINER, ANDREW
Publication of US20100143423A1 publication Critical patent/US20100143423A1/en
Abandoned legal-status Critical Current

Links

Images

Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/24—Phosphorous; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00—Medicinal preparations containing inorganic active ingredients
    • A61K33/06—Aluminium, calcium or magnesium; Compounds thereof, e.g. clay
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00—Medicinal preparations containing inorganic active ingredients
    • A61K33/06—Aluminium, calcium or magnesium; Compounds thereof, e.g. clay
    • A61K33/08—Oxides; Hydroxides
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00—Medicinal preparations containing inorganic active ingredients
    • A61K33/06—Aluminium, calcium or magnesium; Compounds thereof, e.g. clay
    • A61K33/10—Carbonates; Bicarbonates
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00—Medicinal preparations containing inorganic active ingredients
    • A61K33/42—Phosphorus; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K45/00—Medicinal preparations containing active ingredients not provided for in groups A61K31/00 - A61K41/00
    • A61K45/06—Mixtures of active ingredients without chemical characterisation, e.g. antiphlogistics and cardiaca
    • 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
    • A61K8/25—Silicon; Compounds thereof
    • 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

Definitions

  • the present invention relates to an oral care product suitable for maintaining and/or enhancing the quality of teeth.
  • the product comprises compositions that react together to ultimately form hydroxyapatite on the teeth surface, a material that can lead to remineralisation and/or whitening of the teeth.
  • the hydroxyl ion is replaced by the fluoride ion and the resulting fluoroapatite composition is harder than the original hydroxyapatite composition and more resistant to the acidic attack.
  • ion replacement through fluoride treatment cannot achieve a complete restoration of the lost minerals.
  • the method is a preventive treatment and does not actively recover demineralised teeth to their original chemical and mechanical state.
  • the enamel layer of the tooth is naturally an opaque white or slightly off-white colour; however, this enamel layer can become stained or discoloured.
  • the enamel layer of the tooth is composed of hydroxyapatite mineral crystals that create a somewhat porous surface. It is believed that this porous nature of the enamel layer is what allows staining agents and discolouring substances to permeate the enamel and discolour the tooth.
  • a variety of products are currently used for teeth whitening. Such products often comprise a peroxide compound (alone or on combination with enzymes). Such products may be used in the form of strips. Such products generally have to be removed after a well defined time, the peroxide causing damage to the teeth and/or gums if left too long.
  • a particular problem with peroxide (and toothpastes comprising abrasive cleaners) is that it can roughen the surface of the teeth.
  • U.S. Pat. No. 5,605,675 discloses a process for remineralisation of dental enamel by application of a two-phase composition; one phase containing a water-soluble calcium compound and one phase containing a water soluble inorganic phosphate and a water-soluble fluorine compound.
  • U.S. Pat. No. 4,083,955 discloses a process for remineralisation of dental enamel by sequential application of two compositions, the first comprising calcium ions and second comprising phosphate ions, or vice versa.
  • WO 04/017929 discloses a preparation containing: an aqueous liquid part, a solid part comprising at least one silicate selected from tricalcium silicate and dicalcium silicate; calcium chloride and a water reducing agent, to be used to restore a mineralised substance, particularly in the dental field.
  • An object of the present invention is to provide a product which remineralises eroded teeth and/or whitens the teeth without the need for bleaching chemicals.
  • the present invention involves delivering an insoluble calcium salt to the surface of the teeth and converting this salt into hydroxyapatite in situ by the simultaneous or sequential application of a source of phosphate ions.
  • the insoluble calcium salt and the phosphates ions are delivered from independent compositions and their ability to interact prematurely is thereby minimised.
  • the in situ generation of hydroxyapatite results in remineralisation of the teeth, potentially reducing the likelihood of tooth decay and improving the appearance of the teeth, in particular their whiteness.
  • the teeth may also appear smoother and shinier as a result. Since many “whitening” treatments result in a roughening of the tooth surface, the ability to whiten and yet reduce surface roughness is a particular benefit of the present invention.
  • hydroxyapatite The in situ generation of hydroxyapatite is principally targeting at the enamel; however, it is also expected that any exposed dentin may also be beneficially affected in similar manner.
  • an oral care product comprising a first composition comprising an insoluble calcium salt that is not a calcium phosphate salt, a second independent composition comprising a source of phosphate ions, and a means for delivering each of the compositions to the surface of the teeth.
  • a method of remineralising and/or whitening the teeth comprising the steps of treating the teeth with a first composition comprising an insoluble calcium salt that is not a calcium phosphate salt and a second independent composition comprising a source of phosphate ions.
  • a product comprising a first composition comprising an insoluble calcium salt that is not a calcium phosphate salt in combination with a second independent composition comprising a source of phosphate ions for use as a medicament.
  • a first composition comprising an insoluble calcium salt that is not a calcium phosphate salt in combination with a second independent composition comprising a source of phosphate ions for the manufacture of an oral care product.
  • a second independent composition comprising a source of phosphate ions for the manufacture of an oral care product.
  • Such products may be used to improve tooth whiteness, reduce tooth decay, and/or reduce sensitivity.
  • the insoluble calcium salt used in the first composition may be any salt capable of delivery to the surface of the teeth when the composition is applied, other than a calcium phosphate.
  • calcium salts such as hydroxyapatite and fluoroapatite are not included as suitable salts.
  • the insoluble calcium salt is calcium silicate, present as the composite material calcium oxide-silica: CaO—SiO 2 .
  • the use of this insoluble calcium salt is preferred because of its excellent conversion to hydroxyapatite on the tooth surface.
  • the calcium silicate reacts with phosphate ions to form a calcium silicate-phosphate cement (CSPC) and that this material bonds strongly to the teeth and then gradually transforms into hydroxyapatite on the tooth surface. It is believed that the high affinity of the CSPC for the tooth surface underlies the superior remineralisation and whitening benefits obtained.
  • CSPC calcium silicate-phosphate cement
  • Ca:Si calcium silicate
  • the Ca:Si ratio is preferably from 1:5 to 2:1, more preferably from 1:3 to 1:1, and most preferably it is about 1:2.
  • the calcium silicate may comprise mono-calcium silicate, bi-calcium silicate, or tri-calcium silicate. Higher ratios of calcium to silicate are preferred because such ratios are believed to enhance active bonding to the tooth surface and subsequent transformation into hydroxyapatite; however, lower ratios are preferred for ease of obtaining the desired pH (vide infra).
  • ratios of calcium to silicon should be understood to be atom ratios.
  • the insoluble calcium salt is a “biomaterial”, by which is meant a material that is capable of bonding to human and/or animal tissue. It is especially preferred that the biomaterial is able to bond to tooth enamel and/or tooth dentin.
  • insoluble and soluble refer to a material's insolubility or solubility in water at temperatures typically found in the oral cavity. Insoluble calcium salts have a solubility of less than 0.01 mol/L.
  • the content of the insoluble calcium salt in the first composition is typically from 0.1 to 50%, particularly from 1 to 30%, and especially from 5 to 20% by weight.
  • the insoluble calcium salt may be in a crystalline or amorphous state; preferably it is in an amorphous state; more preferably it is in a mesoporous state, i.e. it is a material having pores with diameters from 1 to 50 microns.
  • Mesoporous calcium silicate is particularly preferred and is abbreviated as MCS in this specification.
  • MCS having an average pore size (diameter) of preferably from 0.4 to 4 nm, more preferably from 0.4 to 3.5 nm, and most preferably from 0.4 to 3 nm.
  • MCS having an average pore size (diameter) of preferably from 2 to 4 nm, more preferably from 2 to 3.5 nm, and most preferably from 2 to 3 nm.
  • MCS having an average pore size (diameter) of preferably from 1 to 2.7 nm and more preferably from 1.35 to 2.45 nm.
  • the pore size may be measured using any suitable method or means.
  • the pore size may be measured using BET nitrogen sorption or mercury porosimetry techniques (particularly BET nitrogen sorption techniques).
  • the first composition is substantially free of phosphate ions.
  • substantially free we mean that relative to the weight of the calcium ions, the amount of phosphate ions is less than 2.5%, particularly less than 1%, more particularly less than 0.1%, and especially less than 0.01% by weight. It is possible to prepare calcium oxide-silica containing less than 0.005% by weight of phosphate ions by using high purity starting materials, for example using calcium nitride supplied by China National Pharmaceutical Group Corporation (SINOPHARM), Beijing, which has a purity of greater than 99%.
  • the first composition is substantially free of fluoride ions.
  • substantially free we mean that relative to the weight of the calcium in the insoluble calcium salt, the amount of fluoride ions is less than 2.5%, particularly less than 1%, more particularly less than 0.1%, and especially less than 0.01% by weight.
  • the content of fluoride ions is preferably less than 0.1%, more preferably less than 0.01%, and most preferably less than 0.001% by weight.
  • Calcium silicate suitable for use in the present invention may be prepared by the methods described in our co-pending application PCT/EP2007/057556.
  • the pH of the first composition is preferably from 7 to 11, more preferably from 8 to 10.5, and most preferably from 9 to 10.
  • a preferred additional component in the first composition is an acidic buffering, such as citric acid.
  • an acidic buffering such as citric acid.
  • Such agents enable the composition to be formulated at the desired pH and are particularly desirably at higher Ca:Si ratios, for example 1:1 and greater and especially 2:1 and greater.
  • the second composition is added to the oral cavity together with the first composition. Whilst the saliva naturally present in the oral cavity provides a source of phosphate ions, this saliva should not be considered a second composition in accordance with the present invention. By adding the second composition together with the first composition, whether simultaneously or sequentially, superior remineralisation and/or whitening results.
  • the source of phosphate ions used in the first composition may be any source capable of delivering phosphate ions when the composition is applied to the teeth.
  • the source will be a water-soluble salt. Suitable water soluble salts include tri-sodium phosphate, di-sodium hydrogenphosphate, and sodium dihydrogenphosphate.
  • a preferred additional component in the second composition is a source of fluoride ions.
  • the source may be, for example, sodium fluoride, stannous fluoride, or sodium monofluorophosphate.
  • the level of fluoride ions present in the second composition is typically, from 10 mM to 100 mM, preferably from 25 mM to 75 mM, and more preferably from 40 mM to 60 mM.
  • the fluoride ions, particularly at the preferred concentrations, can aid the reaction between the insoluble calcium salt and the phosphate ions added from the second composition and present in the saliva.
  • the means for delivering each of the compositions to the surface of the teeth may be any means that allows both the insoluble calcium salt in the first composition and the phosphate in the second composition to be delivered to the teeth.
  • the delivery of the compositions may be sequential or simultaneous. In certain embodiments, for example dual phase toothpastes, the compositions are preferably delivered simultaneously.
  • the means of delivery may involve a dual tube having a first compartment for the first composition and a second, independent compartment for the second composition.
  • a dual tube typically has one of the compartments surrounding the other.
  • the dual tube allows for co-extrusion of the two compositions.
  • the means of delivery may involve a single tube having the first composition and second composition present as independent compositions within the same tube.
  • the compositions or phases are extruded from the tube as one, such extrusion being termed “contact extrusion”.
  • one the compositions may be present as stripes within the other composition.
  • one of the compositions is present as a sheath, surrounding the other composition in the core.
  • the first composition is present as a core composition and the second composition surrounds this as a sheath composition.
  • the quantity of water within each of the compositions is preferably less than 35%, more preferably less than 30%, and most preferably less than 25% by weight.
  • the first composition has less than 20% by weight of water and the second composition has less than 25% by weight of water. It has been found that minimising the quantities of water reduces premature interaction of the calcium salt and source of phosphate ions.
  • compositions may be applied to the teeth as a dual-phase toothpaste, such application involving mixing of the compositions (phases) and typically involving application using a toothbrush.
  • One or preferably both of the compositions may be applied to the teeth as a gel composition, the treatment involving mixing of the compositions on application and typically involving the mixed compositions being left on the teeth following application. Following such application, the mixed compositions are typically left on the teeth for from 10 minutes to 10 hours and more typically from 30 minutes to 8 hours.
  • the application may be carried daily.
  • the compositions may be applied from independently compartments of a dual compartment tube or from independent phases of a product contained within a single container which is typically a tube.
  • the means of delivery may involve a tape, in particular an adhesive tape, onto which one or preferably both of the compositions are applied, prior to the strip being placed in contact with the teeth.
  • a tape in particular an adhesive tape
  • the compositions can be held in close contact with tooth surface, facilitating a high concentration of calcium salt and/or source of phosphate ions close to the tooth surface. Much less of the composition(s) is/are lost into the saliva using this delivery means.
  • Gel compositions involve the use of a gel.
  • the first composition comprises a gel.
  • the gel typically comprises a polymeric matrix, and is more typically a hydrogel (vide infra). Excluding any water present, the polymeric matrix is typically present at from 1 to 25% by weight of the composition(s) of which it is a part.
  • a “gel” is a colloidal system in which a porous network of interconnected nano-particles spans the volume of a liquid medium.
  • gels are apparently solid, jelly-like materials. Both by weight and volume, gels are mostly liquid in composition and thus exhibit densities similar to liquids; however, they have the structural coherence of a solid.
  • the polymeric matrix material may be a hydrogel which, in the context of this invention, is an insoluble polymeric network containing an absorbed aqueous phase. Typically, the polymeric network is crosslinked. Typically, the content of other liquid components in the composition(s) comprising the hydrogel is not more than 10% by weight. Typically the content of water in the composition(s) comprising a hydrogel is from 80 to 99%.
  • Monomers used to prepare hydrogels may be selected from vinyl alcohol and acrylate, in particular sodium acrylate. Other monomers comprising an abundance of hydrophilic groups may also be used.
  • Preferred hydrogels comprise a polysaccharide, polyacrylamide, or polyacrylic acid.
  • Suitable polysaccharides may be storage polysaccharides, such as starch or glycogen, or structural polysaccharides, such as cellulose or chitin.
  • Suitable polysaccharides may include saccharide units selected from one or more of the following: isomaltose, glucose, fructose, galactose, xylose, mannose, sorbose, arabinose, rhamnose, fucose, maltose, sucrose, lactose, maltulose, ribose, lyxose, allose, altrose, gulose, idose, talose, trehalose, nigerose, kojibiose, and lactulose.
  • Preferred hydrogels comprise one or more polysaccharides selected from the group consisting of: tamarind gum, guar gum, locust bean gum, Tara, Fenugreek, Aloe, Chia, Flaxseed, Psyllium seed, quince seed, xanthan, gellan, welan, rhamsan, dextran, curdlan, pullulan, scleroglucan, schizophyllan, chitin, hydroxyalkyl cellulose, arabinan, de-branched arabinan, arabinoxylan, galactan, pectic galactan, galactomannan, glucomannan, lichenan, mannan, pachyman, rhamnogalacturonan, acacia gum, agar, alginates, carrageenan, chitosan, clavan, hyaluronic acid, heparin, inulin, cellodextrins, cellulose, and cellulose derivatives.
  • Particularly preferred hydrogels comprise polysaccharides selected from the group consisting of: sodium alginate, hydroxypropyl alginate, gum carrageenan, gum grabic, guar gum, karaya gum, chitosan, pectin, and starch.
  • hydrogel forming components are the Carbopol polymer, which are commercially available from Noveon.
  • compositions used in accordance with the invention may also comprise further ingredients which are common in the art, such as:
  • FIG. 1 Scanning electronic microscopy (SEM) image of human tooth enamel surface morphology of (a) before treatment and (b) after treatment for two weeks with MCS-gel in phosphate-containing saliva in an 8 hours/day cycling treatment.
  • SEM scanning electronic microscopy
  • FIG. 2 SEM image of cross section view of treated tooth. A thin layer in 5 micron thickness has been formed (right bright area) on the original tooth enamel (left area).
  • FIG. 3 Energy Dispersive X-ray (EDX) elemental analysis of Ca and P scanned (left to right) across the dark line indicated on the SEM cross-sectional image of FIG. 2 .
  • the “distances” indicated are distances in microns.
  • FIG. 4 Raman spectrum of tooth surface before and after MCS-gel treatment in the presence of a phosphate containing composition.
  • FIG. 5 a SEM image of a tooth surface prior to “etching” with phosphoric acid.
  • FIG. 5 b SEM image of a tooth surface after etching with phosphoric acid.
  • FIG. 6 a Raman spectrum of phosphoric acid etched tooth surface.
  • FIG. 6 b Raman spectrum of phosphoric acid etched tooth surface following treatment with MCS-gel composition and phosphate containing composition for one week.
  • compositions were prepared as described above with the sodium alginate present at 1 g, 1.5 g, and 3 g.
  • the viscosity of the resulting composition was found to be a function of the alginate level, being higher at the higher alginate levels.
  • Extracted human teeth were cleaned using 75% alcohol and brushed using toothpaste to remove surface bacteria and debris.
  • the composition designated 4 in Table 1 was uniformly painted onto the teeth at a level of 1.0 g per six teeth. The teeth were then immersed in human saliva at 37° C. After eight hours, the gel was washed off with tap water and the teeth re-immersed again in the saliva at 37° C. for the rest of day. This treatment was continued for two weeks.
  • the human saliva used was collected from many subjects. Its calcium concentration varied from 23 to 60 ppm and its phosphorus concentration (present as phosphate ions) varied from 124 to 154 ppm.
  • FIG. 1( a ) represents the appearance before treatment
  • FIG. 1( b ) represents the appearance after treatment. It can be seen that before treatment the surface is smooth and after treatment certain new crystalline structures have grown out from the original smooth surface. At a magnification of 10,000, tiny crystalline structures can be clearly seen, measuring about 100 nm.
  • FIG. 3 shows that the content of calcium and phosphorus in the newly formed hydroxyapatite is very similar to that in the original tooth enamel underneath.
  • FIG. 4 indicates that the chemical nature of the phosphate present in newly formed hydroxyapatite is essentially the same as that of the untreated teeth, strongly suggesting that only “natural” hydroxyapatite has been added to the teeth.
  • FIG. 5 a represents a tooth surface before etching
  • FIG. 5 b represents a tooth surface after etching.
  • Composition 5 MCS powder (0.5 g) added to water (10 g) and dispersed as described above, then sodium alginate (0.3 g) added with vigorous stirring. A uniform gel was formed after about ten minutes stirring.
  • FIG. 6 a is the Raman spectrum of a tooth surface before treatment
  • FIG. 6 b is the Raman spectrum of a tooth surface after treatment.
  • Table 2 indicates the position of the major peaks before and after treatment. There is a peak at 961.42 cm ⁇ 1 which corresponds to the major phosphate band.
  • the after treatment sample gave an essentially identical Raman spectrum to the before treatment sample, including the location of the phosphate band at 961.42 cm ⁇ 1 . This implies that the added material is identical to that originally present and is a somewhat surprising result.
  • the Raman bands V 1 , V 2 , V 3 , and V 4 are characteristic of the crystallinity/perfection of the apatite crystal lattice.
  • a product was prepared comprising two gel compositions: Gel I and Gel II. Details are given in Table 4.
  • An MSC powder as described above under “step I” was incorporated into Gel I by the method disclosed under “step I”.
  • Gel II was prepared by adding sodium alginate to a solution of phosphate buffer and sodium fluoride.
  • the product was applied by mixing equal weights of Gel I and Gel II and painting the mixture (total weight 2 g) onto six teeth using a cotton bud.
  • the treated teeth were immersed in human saliva (15 ml) for one hour, at 37° C., with gentle agitation. After this time, the teeth were rinsed and cleaned using a cotton bud to remove any remaining gel. They were then placed into fresh saliva for a further two hours. This process was performed twice a day for two weeks, giving a total of 28 treatments.
  • Example 6 as described above (i.e. a 1:1 by weight mixture of Gel I and Gel II) was applied to an adhesive plastic tape. Then the tape was then wrapped around each tooth and the wrapped teeth immersed in saliva for eight hours. The dosage applied was 2 g of the mixture of Gel I and Gel II per 6 teeth. After this time, the teeth were rinsed with water and then put into fresh saliva. This procedure was repeated for two weeks, including a tooth brushing each day to simulate real life usage.
  • Example 6 The effects of the above treatments with Example 6, with respect to tooth whitening, were investigated together with a “control” treatment involving tooth brushing (once a day) and treatment with saliva only.
  • the whitening effect was measured using a Minolta Chromameter CR-321 (3 mm aperture, 45/0) to quantitatively measure the L* and b* value of each tooth before and after treatment.
  • L* represents the overall light intensity that is reflected from the tested surface and b* represents the light contribution from the yellow-blue. Tooth whitening is indicated by an increase in reflected light intensity (L*) and a decrease in “yellowness” (b*).
  • L* reflected light intensity
  • b* yellow-blue
  • the results are shown in Table 5. Average colour changes after two weeks treatment are expressed as ⁇ L* and ⁇ b*. Good whitening effects were observed with both treatments according to the invention.
  • Example 7 gives superior “lightening” and “whitening” in comparison with the controls.
  • compositions detailed in Table 12 are intended for use in a 1:1 by weight ratio. These compositions are suitable for extrusion as independent compositions/phases from within the same compartment of the same tube, for example with the first composition forming a core and the second composition forming a surrounding sheath. The amount of water in the compositions of this Example is particularly low.
US12/517,365 2006-12-05 2007-11-23 Oral care product Abandoned US20100143423A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
CN2006003278 2006-12-05
CN2006/003278 2006-12-05
PCT/EP2007/062744 WO2008068149A1 (en) 2006-12-05 2007-11-23 Oral care product

Publications (1)

Publication Number Publication Date
US20100143423A1 true US20100143423A1 (en) 2010-06-10

Family

ID=39092967

Family Applications (3)

Application Number Title Priority Date Filing Date
US12/517,365 Abandoned US20100143423A1 (en) 2006-12-05 2007-11-23 Oral care product
US12/517,560 Expired - Fee Related US9149419B2 (en) 2006-12-05 2007-12-04 Oral care product
US12/517,562 Active 2028-01-25 US8257721B2 (en) 2006-12-05 2007-12-04 Oral care product

Family Applications After (2)

Application Number Title Priority Date Filing Date
US12/517,560 Expired - Fee Related US9149419B2 (en) 2006-12-05 2007-12-04 Oral care product
US12/517,562 Active 2028-01-25 US8257721B2 (en) 2006-12-05 2007-12-04 Oral care product

Country Status (11)

Country Link
US (3) US20100143423A1 (zh)
EP (3) EP2089040B1 (zh)
CN (3) CN101600443B (zh)
AT (2) ATE539759T1 (zh)
BR (3) BRPI0720183B1 (zh)
CL (1) CL2007003497A1 (zh)
DE (1) DE602007012463D1 (zh)
ES (2) ES2378282T3 (zh)
MX (1) MX2009006027A (zh)
PL (3) PL2089040T3 (zh)
WO (3) WO2008068149A1 (zh)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3214995A1 (en) * 2014-11-03 2017-09-13 Unilever PLC, a company registered in England and Wales under company no. 41424 of Modelling method

Families Citing this family (61)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9833386B2 (en) * 2006-03-30 2017-12-05 James D. Welch Method of, and system for smoothing teeth
ATE539759T1 (de) 2006-12-05 2012-01-15 Unilever Nv Mundpflegeprodukt
WO2010042754A2 (en) * 2008-10-08 2010-04-15 Medical College Of Georgia Research Institute, Inc. Methods and systems for mineralization of demineralized tissue
WO2010054494A2 (en) * 2008-11-14 2010-05-20 Profimed S.R.O. Biomimetic oral care composition
US20100189663A1 (en) * 2009-01-24 2010-07-29 Gallis Karl W Mouth rinse compositions including chemically modified silica or silicate materials for sustained delivery to tooth surfaces
US20100196514A1 (en) * 2009-02-02 2010-08-05 Chung Shan Medical University Calcium silicate-based composite cement and methods for the preparation
EP2413883A1 (en) * 2009-04-01 2012-02-08 Colgate-Palmolive Company Dentifrice compositions and methods for treating and preventing damage to tooth surfaces
WO2010148624A1 (en) * 2009-06-26 2010-12-29 Unilever Plc Dye polymers
WO2011109919A1 (en) 2010-03-09 2011-09-15 Unilever Plc Stable oral care compositions
US9877911B2 (en) 2010-06-23 2018-01-30 Conopco, Inc. Non-aqueous oral care compositions
WO2012031785A2 (en) 2010-09-10 2012-03-15 Unilever Plc Composite particle active and method for making the same
US20130171221A1 (en) * 2010-09-10 2013-07-04 Yan Deng Oral care compositions for benefiting teeth
US9717929B2 (en) * 2010-12-07 2017-08-01 Colgate-Palmolive Company Dentifrice compositions containing calcium silicate and a basic amino acid
US20130251772A1 (en) * 2010-12-07 2013-09-26 Colgate-Palmolive Company Dentifrice Compositions Containing Calcium Silicate
TWI461216B (zh) * 2010-12-09 2014-11-21 Univ Nat Taiwan 牙齒漂白催化劑及其應用
US20140079750A1 (en) * 2011-04-18 2014-03-20 Xiaoke Li Tooth remineralizing oral care compositions
CN103476385B (zh) * 2011-04-18 2015-12-09 荷兰联合利华有限公司 牙齿再矿化口腔护理组合物
GB201212222D0 (en) * 2012-07-10 2012-08-22 Univ Dundee Improved apparatus and method for mineralising biological materials
EP2906181B1 (en) * 2012-10-12 2017-12-06 Unilever N.V. Oral care composition
CN104703575B (zh) * 2012-10-12 2017-12-12 荷兰联合利华有限公司 口腔护理组合物
WO2015007503A1 (en) 2013-07-19 2015-01-22 Unilever Plc Remineralising oral care products
WO2015036277A1 (en) * 2013-09-10 2015-03-19 Unilever N.V. Oral care composition
CN105517530B (zh) * 2013-09-10 2019-08-27 荷兰联合利华有限公司 口腔护理组合物
EA033258B9 (ru) * 2013-09-10 2019-11-29 Unilever Nv Композиция для ухода за полостью рта
EP3151808B1 (en) * 2014-06-09 2018-10-17 Unilever PLC Oral care compositions
EP3166573A1 (en) * 2014-07-11 2017-05-17 Koninklijke Philips N.V. System for the administration of an oral care composition
BR112017016105B1 (pt) * 2015-02-16 2021-06-01 Unilever Ip Holdings B.V. Produto para cuidados orais, métodos para o branqueamento dos dentes e kit para o clareamento dos dentes
CN107223048B (zh) * 2015-02-16 2020-06-09 荷兰联合利华有限公司 口腔护理组合物
CN107635534B (zh) * 2015-05-13 2021-07-13 荷兰联合利华有限公司 口腔护理组合物
BR112017021611B1 (pt) * 2015-05-13 2021-04-27 Unilever Ip Holdings B.V. Composição para os cuidados orais, conjunto para os cuidados orais e uso de uma composição
CN104906137A (zh) * 2015-06-01 2015-09-16 张亚南 一种牙科手术后的恢复药剂及包含所述药剂的膏体剂
EP3302350B1 (en) * 2015-06-05 2022-07-20 Unilever IP Holdings B.V. Method of whitening teeth
US20180125625A1 (en) * 2015-06-05 2018-05-10 Conopco, Inc., D/B/A Unilever Oral care device
CN107743386A (zh) * 2015-06-05 2018-02-27 荷兰联合利华有限公司 口腔护理装置
EP3316851B1 (en) 2015-07-03 2019-09-11 Unilever NV Oral care composition comprising calcium silicate
GB201513040D0 (en) * 2015-07-23 2015-09-09 Ucl Business Plc Bone graft system
EP3349860B1 (en) 2015-10-08 2020-04-15 Colgate-Palmolive Company Oral care compositions
US10342646B2 (en) * 2015-10-17 2019-07-09 James D. Welch Method of, and system for smoothing teeth
EA036458B1 (ru) 2015-11-10 2020-11-12 Юнилевер Н.В. Композиция для ухода за полостью рта
BR112018072483B1 (pt) 2016-05-19 2021-11-16 Unilever Ip Holdings B.V. Composiqao para cuidados orais e uso da composiqao
EP3500232B1 (en) 2016-08-19 2020-06-10 Unilever N.V. Oral care composition
EA038664B1 (ru) * 2016-09-23 2021-09-30 ЮНИЛЕВЕР АйПи ХОЛДИНГС Б.В. Композиция для ухода за полостью рта
BR112019006087B1 (pt) 2016-10-18 2023-01-17 Unilever Ip Holdings B.V. Composição de cuidados bucais e uso de uma composição de cuidados bucais
EP3547989B1 (en) 2016-11-30 2022-10-05 Unilever Global IP Limited Oral care composition
BR112019010091B1 (pt) 2016-12-14 2022-09-13 Unilever Ip Holdings B.V. Composição de cuidados orais e uso da composição de cuidados orais
CN110545784B (zh) 2017-04-27 2022-10-25 联合利华知识产权控股有限公司 口腔护理组合物
EP3614994B1 (en) 2017-04-27 2021-10-13 Unilever Global IP Limited Oral care composition
WO2019007695A1 (en) 2017-07-07 2019-01-10 Unilever N.V. COMPOSITION FOR ORAL CARE
WO2019029917A1 (en) 2017-08-10 2019-02-14 Unilever N.V. COMPOSITION FOR ORAL CARE
EP3668478B1 (en) 2017-08-18 2022-04-13 Unilever Global IP Limited Oral care composition
WO2019034325A1 (en) 2017-08-18 2019-02-21 Unilever N.V. COMPOSITION FOR ORAL CARE
WO2019034348A1 (en) 2017-08-18 2019-02-21 Unilever N.V. COMPOSITION OF ORAL CARE
GB201721001D0 (en) 2017-12-15 2018-01-31 Glaxosmithkline Consumer Healthcare (Uk) Ip Ltd Novel Composition
PL3513777T3 (pl) 2018-01-22 2024-02-26 Ivoclar Vivadent Ag Sposób remineralizacji zębów
WO2020099068A1 (en) 2018-11-15 2020-05-22 Unilever N.V. Oral care composition
WO2020212159A1 (en) * 2019-04-17 2020-10-22 Unilever Plc Oral care product
AU2020426517A1 (en) 2020-01-29 2022-08-18 Rabbit Indústria E Comércio De Produtos De Higiene Pessoal Ltda Oral composition with synergistic association of organic and inorganic components for complete maintenance of oral health, method for obtaining same and uses
BR112022021230A2 (pt) 2020-05-21 2022-12-27 Unilever Ip Holdings B V Composição de cuidados orais, produto de cuidados orais, método de remineralização e/ou redução da hipersensibilidade dos dentes e uso de composição
EP4340949A1 (en) 2021-05-20 2024-03-27 Smile Makers, LLC Oral hygiene compositions and methods of use
CN117835953A (zh) * 2021-08-19 2024-04-05 联合利华知识产权控股有限公司 口腔护理组合物
WO2024046751A1 (en) 2022-08-31 2024-03-07 Unilever Ip Holdings B.V. Process for the manufacture of a non-aqueous composition

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4083955A (en) * 1975-04-02 1978-04-11 The Procter & Gamble Company Processes and compositions for remineralization of dental enamel
US5605675A (en) * 1995-06-06 1997-02-25 Enamelon Inc. Processes and compositions for remineralization and prevention of demineralization of dental enamel
US5858333A (en) * 1998-08-07 1999-01-12 Enamelon, Inc. Two-part oral products and methods of using same to remineralize teeth
US20020081555A1 (en) * 2000-11-13 2002-06-27 Wiesel Peter E. Systems for treating teeth
US6485708B1 (en) * 1999-05-13 2002-11-26 Church & Dwight Co. Inc. Products and methods for the remineralization and prevention of demineralization of teeth
US20030170185A1 (en) * 1998-04-24 2003-09-11 Sunstar Kabushiki Kaisha Oral composition
US20060102049A1 (en) * 2002-08-23 2006-05-18 Badreddine Bergaya Preparation for producing a material used to restore a mineralised substance, particularly in the dental field

Family Cites Families (44)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3929493A (en) 1974-04-09 1975-12-30 Lee Pharmaceuticals Dental base material
US4080440A (en) * 1974-12-13 1978-03-21 The Procter & Gamble Company Method for remineralizing tooth enamel
SE420596B (sv) * 1975-03-25 1981-10-19 Osaka Packing Formad kropp av amorf kiseldioxid, eventuellt innehallande kalciumkarbonat, sett att framstella en formad kropp av amorf kiseldioxid samt partikel av amorf kiseldioxid for framstellning av en formad kropp
US4038380A (en) 1976-05-17 1977-07-26 Colgate-Palmolive Company Calcium meta silicate as dental polishing agent
AU530013B2 (en) 1978-11-29 1983-06-30 Beecham Group Limited Alumina free oral composition
US4612053A (en) * 1983-10-06 1986-09-16 American Dental Association Health Foundation Combinations of sparingly soluble calcium phosphates in slurries and pastes as mineralizers and cements
US4725576A (en) 1983-12-29 1988-02-16 Research Foundation Of State University Of New York Fungicidal polypeptide compositions containing L-histidine and methods for use therefore
DE3430801A1 (de) * 1984-08-22 1986-03-06 Bayer Ag, 5090 Leverkusen Verwendung von poroesen fuellstoffen in polymerisierbaren massen, solche massen und deren verwendung zur herstellung von formkoerpern
JPH0531166A (ja) 1991-07-26 1993-02-09 Nippon Electric Glass Co Ltd 生体活性複合インプラント材
EP0639823B1 (en) 1993-03-08 2000-05-17 Nohmi Bosai Ltd. Fire alarm receiver and fire alarm system
DE4343103A1 (de) 1993-12-17 1995-06-22 Braun Ag Elektrische Zahnbürste
JP3528181B2 (ja) 1995-08-08 2004-05-17 エナメロン・インコーポレイテッド 歯の病変部の再石灰用の改善された製品および方法
SK102998A3 (en) 1996-01-29 1999-04-13 Univ Maryland Bioactive glass compositions and methods of treatment using bioactive glass
US5735942A (en) 1996-02-07 1998-04-07 Usbiomaterials Corporation Compositions containing bioactive glass and their use in treating tooth hypersensitivity
US6491900B2 (en) 1996-08-20 2002-12-10 American Dental Association Health Foundation Anti-carious candies and confections
US5833954A (en) * 1996-08-20 1998-11-10 American Dental Association Health Foundation Anti-carious chewing gums, candies, gels, toothpastes and dentifrices
US5804228A (en) 1996-08-21 1998-09-08 Caco Pacific Corporation Minimum vestige nozzle assembly for plastics injection molding
US5726138A (en) * 1996-08-26 1998-03-10 Lever Brothers Company, Division Of Conopco, Inc. Aqueous solution compositions comprising polymer hydrogel compositions
DE19847630A1 (de) 1998-10-15 2000-04-20 Basf Ag Siliciumdioxid mit Meso- und Mikroporen
US20020037258A1 (en) 1999-08-05 2002-03-28 Gregory P. Dodd Dental composition for the mineral occlusion of dentinal tubules in sensitive teeth
US6482395B1 (en) 1999-06-01 2002-11-19 Church & Dwight Co. Inc. Remineralizing-mineralizing oral products containing discrete cationic and anionic agglomerate components and method of use
CA2377402C (en) * 1999-06-14 2011-01-18 Imperial College Innovations Silver-containing, sol-gel derived bioglass compositions
IT1320188B1 (it) * 2000-04-26 2003-11-26 Perfetti Spa Gomma da masticare.
US7182937B2 (en) 2000-10-13 2007-02-27 Block Drug Company, Inc. Anhydrous dentrifice formulations for the delivery of incompatible ingredients
DE10063945A1 (de) 2000-12-20 2002-07-04 Henkel Kgaa Remineralisierende Dental-Klebefolie
JP2002322013A (ja) 2001-04-25 2002-11-08 Univ Nagoya 活性物質の前駆体、該前駆体を用いた活性物質、及びその活性物質の製造方法
ES2296684T3 (es) * 2001-05-17 2008-05-01 KETTENBACH GMBH & CO. KG Material de blanqueo dental quimicamente endurecible.
US20040241238A1 (en) 2001-05-25 2004-12-02 Pilar Sepulveda Foamed sol-gel and method of manufacturing the same
US6902806B2 (en) 2002-04-30 2005-06-07 National Institute Of Advanced Science And Technology Mesoporous silica having controlled-release on-off control function, production method thereof and method using same
TWI283657B (en) 2002-07-15 2007-07-11 Pentax Corp CaO-SiO2-based bioactive glass and sintered calcium phosphate glass using same
CN1569736A (zh) 2002-09-28 2005-01-26 中国科学院上海硅酸盐研究所 可降解多孔硅酸钙陶瓷生物活性材料的制备方法
US20040191187A1 (en) 2003-01-31 2004-09-30 Hong Luo Multivalent ion compatible carbomer formulations
HRP20030304A2 (en) 2003-04-17 2005-02-28 Bašić Robert Oral composition for stabilisation, (re)calcification and (re)mineralisation of tooth enamel and dentine
GB0315012D0 (en) 2003-06-27 2003-07-30 Leuven K U Res & Dev Zeotiles
US20060018966A1 (en) * 2003-07-22 2006-01-26 Lin Victor S Antimicrobial mesoporous silica nanoparticles
AU2004308400A1 (en) 2003-12-19 2005-07-14 Novamin Technology Inc. Compositions and methods for preventing or reducing plaque and/or gingivitis using a bioactive glass containing dentifrice
CN1253391C (zh) 2003-12-22 2006-04-26 复旦大学 纳米介孔以及介孔－大孔复合生物玻璃及其制备方法
US20060093562A1 (en) * 2004-11-04 2006-05-04 Kellar Kenneth E Use of sodium decyl sulfate in toothpaste
US20060115437A1 (en) 2004-11-26 2006-06-01 Robert Hayman Dental whitening compositions
WO2006099748A1 (en) 2005-03-25 2006-09-28 Innovative Bioceramix, Inc. Hydraulic cement compositions and methods of making and using the same
CN1739482A (zh) 2005-08-26 2006-03-01 广州市华之特奥因特种材料科技有限公司 一种光触媒美白牙膏及其制备方法
CN1785862A (zh) 2005-10-27 2006-06-14 中国科学院上海硅酸盐研究所 一种钙硅基有序介孔生物活性玻璃及其制备方法和应用
WO2008017203A1 (en) * 2006-08-01 2008-02-14 Unilever Plc Biomaterials, their preparation and use
ATE539759T1 (de) 2006-12-05 2012-01-15 Unilever Nv Mundpflegeprodukt

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4083955A (en) * 1975-04-02 1978-04-11 The Procter & Gamble Company Processes and compositions for remineralization of dental enamel
US5605675A (en) * 1995-06-06 1997-02-25 Enamelon Inc. Processes and compositions for remineralization and prevention of demineralization of dental enamel
US20030170185A1 (en) * 1998-04-24 2003-09-11 Sunstar Kabushiki Kaisha Oral composition
US5858333A (en) * 1998-08-07 1999-01-12 Enamelon, Inc. Two-part oral products and methods of using same to remineralize teeth
US6485708B1 (en) * 1999-05-13 2002-11-26 Church & Dwight Co. Inc. Products and methods for the remineralization and prevention of demineralization of teeth
US20020081555A1 (en) * 2000-11-13 2002-06-27 Wiesel Peter E. Systems for treating teeth
US20060102049A1 (en) * 2002-08-23 2006-05-18 Badreddine Bergaya Preparation for producing a material used to restore a mineralised substance, particularly in the dental field

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Martinez et al., Bioactivity of Ca0-SiO2 binary glass systems, Chemical Materials, 2000, 12, pp. 3080-3088. *
Saravanapavan et al., Mesoporous calcium silicate glasses. I. Synthesis, J. of Non-Crystal. Solids, 2003, 318, pp. 1-13. *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3214995A1 (en) * 2014-11-03 2017-09-13 Unilever PLC, a company registered in England and Wales under company no. 41424 of Modelling method
US20170332962A1 (en) * 2014-11-03 2017-11-23 Conopco, Inc., D/B/A Unilever Modelling method
EP3622887A1 (en) * 2014-11-03 2020-03-18 Unilever PLC Modelling system

Also Published As

Publication number Publication date
ATE497771T1 (de) 2011-02-15
BRPI0717922B1 (pt) 2017-03-14
BRPI0717906A2 (pt) 2013-11-05
EP2089039B1 (en) 2013-03-13
US8257721B2 (en) 2012-09-04
CN101600443B (zh) 2014-08-13
PL2089038T3 (pl) 2011-07-29
BRPI0720183A2 (pt) 2013-12-24
US20100136067A1 (en) 2010-06-03
ES2378282T3 (es) 2012-04-10
BRPI0717922A2 (pt) 2013-10-22
WO2008068149A1 (en) 2008-06-12
CN101600444A (zh) 2009-12-09
CN101600442A (zh) 2009-12-09
EP2089040A1 (en) 2009-08-19
BRPI0717906B1 (pt) 2015-12-08
US9149419B2 (en) 2015-10-06
CN101600444B (zh) 2014-09-17
MX2009006027A (es) 2009-06-16
DE602007012463D1 (de) 2011-03-24
EP2089040B1 (en) 2012-01-04
EP2089038B1 (en) 2011-02-09
ATE539759T1 (de) 2012-01-15
WO2008068247A1 (en) 2008-06-12
CN101600443A (zh) 2009-12-09
BRPI0720183B1 (pt) 2019-03-26
PL2089039T3 (pl) 2013-08-30
PL2089040T3 (pl) 2012-06-29
CN101600442B (zh) 2015-01-14
EP2089039A1 (en) 2009-08-19
CL2007003497A1 (es) 2008-08-01
US20100150974A1 (en) 2010-06-17
ES2357991T3 (es) 2011-05-04
BRPI0717922B8 (pt) 2017-05-30
WO2008068248A1 (en) 2008-06-12
EP2089038A1 (en) 2009-08-19

Similar Documents

Publication Publication Date Title
EP2089040B1 (en) Oral care product
US20130171221A1 (en) Oral care compositions for benefiting teeth
US20140079750A1 (en) Tooth remineralizing oral care compositions
CN111093604B (zh) 口腔护理组合物
CN110997072B (zh) 口腔护理组合物
CN110545784B (zh) 口腔护理组合物
EP3547989B1 (en) Oral care composition
EP3668478B1 (en) Oral care composition
WO2020099068A1 (en) Oral care composition
CN110573131B (zh) 口腔护理组合物
WO2021047971A1 (en) Method for remineralizing and/or reducing sensitivity of teeth
EA042242B1 (ru) Композиция для ухода за полостью рта

Legal Events

Date Code Title Description
AS Assignment

Owner name: CONOPCO, INC. D/B/A UNILEVER,NEW JERSEY

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:BUTLER, MICHAEL FRANCIS;DENG, YAN;HEPPENSTALL-BUTLER, MARY;AND OTHERS;SIGNING DATES FROM 20090528 TO 20100118;REEL/FRAME:024067/0127

STCB Information on status: application discontinuation

Free format text: ABANDONED -- FAILURE TO RESPOND TO AN OFFICE ACTION