WO2022106186A1 - Composition de soin buccal pour des avantages de blanchiment - Google Patents

Composition de soin buccal pour des avantages de blanchiment Download PDF

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Publication number
WO2022106186A1
WO2022106186A1 PCT/EP2021/080324 EP2021080324W WO2022106186A1 WO 2022106186 A1 WO2022106186 A1 WO 2022106186A1 EP 2021080324 W EP2021080324 W EP 2021080324W WO 2022106186 A1 WO2022106186 A1 WO 2022106186A1
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WO
WIPO (PCT)
Prior art keywords
composition
calcium
citrate
range
sheet
Prior art date
Application number
PCT/EP2021/080324
Other languages
English (en)
Inventor
Somnath Das
Satyajit Samadder
Original Assignee
Unilever Ip Holdings B.V.
Unilever Global Ip Limited
Conopco, Inc., D/B/A Unilever
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
Application filed by Unilever Ip Holdings B.V., Unilever Global Ip Limited, Conopco, Inc., D/B/A Unilever filed Critical Unilever Ip Holdings B.V.
Publication of WO2022106186A1 publication Critical patent/WO2022106186A1/fr

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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
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36—Carboxylic acids; Salts or anhydrides thereof
    • A61K8/365—Hydroxycarboxylic acids; Ketocarboxylic acids
    • 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
    • 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 composition for providing whitening benefits to teeth.
  • WO2012/143220 discloses an oral care composition for whitening and remineralizing teeth comprising a phosphate source and re-generation source calcium salt having a particle size of five microns or less so that in-situ hydroxyapatite may be generated upon use.
  • the calcium salt therein are calcium carbonate, calcium silicate, calcium sulfate, calcium phosphate, calcium gluconate, calcium oxide, calcium lactate, calcium hydroxide, calcium carboxymethyl cellulose, calcium alginate, calcium salts of citric acid.
  • EP3222326 discloses a calcium source having a water solubility less than 0.1 moles per litre at room temperature in combination with a phosphate source for use in preventing calculus.
  • the calcium source discloses therein are calcium gluconate, calcium oxide, calcium lactate, calcium carbonate, calcium hydroxide, calcium sulphate, calcium carboxymethyl cellulose, calcium alginate, calcium salts of citric acid, calcium silicate or a mixture thereof.
  • US 5219602 A discloses aqueous dispersion of calcium citrate salt compositions adaptable for use in food compositions, particularly as opacifiers, whitening agents, texture modifiers and partial fat substitutes.
  • US 5275806 A discloses topical sun-protection composition which comprise effective amounts of the reaction product of a calcium compound such as calcium hydroxide, calcium oxide, or calcium carbonate, with citric acid, the reaction product exhibiting a calcium :citrate molar ratio of 2.5:2 to 2.95:2.
  • the present invention relates a tooth whitening composition
  • a tooth whitening composition comprising:
  • composition (b) an orally acceptable vehicle, wherein said composition is an oral care composition.
  • composition of the invention wherein the sheet like crystals of calcium citrate are prepared using a process comprising the steps of:
  • Oral care composition for the purposes of the present invention means a paste, powder, liquid, gum, serum or other preparation for cleaning the teeth or other surfaces in the oral cavity.
  • Toothpaste for the purpose of the present invention means a paste or gel dentifrice for use with a toothbrush. Especially preferred are tooth pastes suitable for cleaning teeth by brushing for about one minutes, preferably two minutes. “Mouth wash” for the purpose of the present invention means liquid dentifrice for use in rinsing the mouth. Especially preferred are mouth washes suitable for rinsing the mouth by swishing and/or gargling for about half a minute before expectorating.
  • the present invention relates to a tooth whitening composition
  • a tooth whitening composition comprising calcium salt of citric acid which has a specific plate I sheet like morphology; and an orally acceptable base.
  • Calcium salt of citric acid has the molecular formula Ca 3 (cit) 2 . xH 2 O where (cit) is a citrate group; and x has a value from 0 to 4
  • Sheet like crystals of calcium citrate for use in the oral care composition of the invention has an average length in the range of 0.5 to 4 micrometer; average width in the range of 0.5 to 4 micrometer and average thickness in the range of 30 to 100 nanometers.
  • the average length of the sheet like crystals of calcium citrate is preferably in the range of 2 to 3 micrometer.
  • the average width of the sheet like crystals of calcium citrate is preferably in the range of 2 to 3 micrometer.
  • the average thickness of the sheet like crystals of calcium citrate is preferably in the range of 60 to 80 nanometers.
  • the sheet like crystals may be preferably configured during the process of its preparations such that they comprise two to five layers of the sheet like crystals stacked upon each other.
  • the present inventors believe that when sheet-like crystals of calcium citrate are included in a toothpaste used for brushing teeth, the material deposited due to its unique morphology delivers enhanced whitening while minimizing abrasion of the tooth surface.
  • the composition of the invention comprises an orally acceptable base.
  • the orally acceptable base preferably comprises an abrasive, a surfactant, a volatile alcohol, a humectant or combinations thereof. More preferred orally acceptable bases include an abrasive, a humectant or mixtures thereof.
  • the orally acceptable base preferably is included in as much as 99.8%, more preferably at as much as 96% by weight of the composition.
  • the orally acceptable base is included in at least 80% more preferably at least 90%, by weight of the composition.
  • the oral care composition of the present invention may be delivered in the form of an ointment, a gel, a dentifrice or a mouthwash.
  • Dentifrices include forms like toothpaste and toothpowder.
  • a composition is most preferably presented in the form of a toothpaste, a toothpowder or a mouthwash.
  • Oral care composition of the present invention preferably comprises an abrasive.
  • the abrasive may preferably be calcium carbonate or silica.
  • Gels usually contain silica, whereas opaque creams generally contain calcium-based abrasives, especially chalk (calcium carbonate).
  • opaque toothpastes the compositions have 5 to 60 wt% calcium-based abrasive. In more preferred compositions it is 30 to 60 wt% and furthermore preferably from 35 to 55 wt%.
  • Optimal compositions have 40 to 55 wt% calcium-based abrasive.
  • a preferred abrasive is fine ground natural chalk (FGNC), which is a form of chalk. It is obtained from limestone or marble.
  • FGNC may also be modified chemically or physically by coating during milling or after milling by heat treatment. Typical coating materials include magnesium stearate or oleate.
  • the morphology of 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 may be used as the sole calcium-based abrasive. However, FGNC may also be used with the other calcium-based abrasives for some balance of abrasion. Usually, the particle size of chalk is from 1 to 60 pm, and preferred sizes range from 1 to 15 pm.
  • DCP dicalcium phosphate
  • PCC precipitated calcium carbonate
  • abrasives may also be used depending upon the intended degree of abrasion. These include synthetic abrasive polishing agents such as amorphous precipitated silica and silica gels. It is preferred that gel compositions of the invention comprises silica as the abrasive. Abrasive silica for incorporation in the composition of the invention is preferably one with a low refractive index.
  • the low refractive index silicas, used as abrasives in the present invention are preferably silicas with an apparent refractive index (Rl) in the range of 1.41 to 1.47, preferably 1 .435 to 1 .445 , preferably having a weight mean particle size of between 5 and 15 mm, a BET (nitrogen) surface area of between 10 and 100 m 2 /g and an oil absorption of about 70 - 150 cm 3 /100 g, but abrasive silicas with a lower apparent refractive index may also be used .
  • Typical examples of suitable low refractive index abrasive silicas e.g. having an Rl of between 1.435 and 1.445.
  • the amount of these silicas in the composition of the present invention generally ranges from 5-60% by weight, usually 5-20% by weight of the composition.
  • abrasive agents include magnesium carbonate, sodium metaphosphate, potassium metaphosphate, zirconium silicate, potassium metaphosphate, magnesium orthophosphate, tricalcium phosphate, magnesium orthophosphate, trimagnesium phosphate, aluminum silicate, zirconium silicate and perlite.
  • Suitable humectants are preferably used in the oral care composition of the present invention.
  • Preferred humectant for inclusion in the present invention is a polyhydric alcohol (also referred to as polyol).
  • Preferred ones include, for example, glycerin, sorbitol, propylene glycol, dipropylene glycol, diglycerol, triacetin, mineral oil, polyethylene glycol (preferably, PEG-400), alkane diols like butane diol and hexanediol, ethanol, pentylene glycol, or a mixture thereof.
  • Glycerin, polyethylene glycol, sorbitol or mixtures thereof are the preferred humectants, most preferred ones being glycerol (also known as glycerine) and sorbitol.
  • the humectant may be present in the range of from 10 to 90% by weight of oral care compositions. More preferably, the humectant makes up from 25 to 80%, and most preferably, from 45 to 70% by weight of the composition, based on total weight of the composition and including all ranges subsumed therein.
  • an oral care composition comprises a surfactant.
  • the composition comprises at least 0.01% surfactant by weight of the composition, more preferably at least 0.1% and most preferably from 0.5 to 7%.
  • 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 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.
  • anionic surfactants such as the sodium, magnesium, am
  • the surfactant comprises or is an anionic surfactant.
  • the preferred surfactants are sodium lauryl sulphate and/or sodium dodecylbenzene sulfonate. Most preferably the surfactant is sodium lauryl sulphate.
  • Other 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.
  • Other suitable surfactants include amphoteric surfactants, such as betaines or sulphobetaines. Mixtures of any of the above described materials may also be used.
  • Most preferred surfactants are an alkali metal alkyl sulphate or a betaine.
  • the composition comprises a thickener.
  • Thickeners that may be used in this invention include, sodium carboxymethyl cellulose (SCMC), hydroxyl ethyl cellulose, methyl cellulose, ethyl cellulose, gum tragacanth, gum arabic, gum karaya, xanthan gum, sodium alginate, carrageenan gum, guar gum, Irish moss, starch, modified starch, silica based thickeners including silica aerogels, magnesium aluminum silicate (e.g., Veegum), Carbomers (cross-linked acrylates) and mixtures thereof.
  • SCMC sodium carboxymethyl cellulose
  • hydroxyl ethyl cellulose hydroxyl ethyl cellulose
  • methyl cellulose methyl cellulose
  • ethyl cellulose gum tragacanth
  • gum arabic gum karaya
  • xanthan gum sodium alginate
  • carrageenan gum guar gum
  • Irish moss Irish mos
  • thickening silica, sodium carboxymethyl cellulose and/or a Carbomer is/are preferred thickeners for use in the composition of the invention.
  • Thickening silica is especially preferred to be used in gel toothpastes.
  • Gel toothpastes generally contain upto 8.5 wt% thickening silica whereas opaque toothpastes typically contain 3 to 4 wt% thickening silica.
  • Thickener when present, preferably makes up from 0.01 to about 10%, more preferably from 0.1 to 9%, and most preferably, from 1.5 to 8% by weight of the composition.
  • Water may preferably be included in 5 to 95%, in particular 10 to 75%, and especially at from 10 to 60%, further-more preferably 10 to 45% by total weight of the composition.
  • the oral care composition of this invention is a toothpaste or gel
  • the same typically has a viscosity from about 30,000 to 180,000 centipoise, and preferably, from 60,000 to 170,000 centipoise, and most preferably, from 65,000 to 165,000 centipoise.
  • the oral care composition of the present invention may contain a variety of other ingredients which are common in the art to enhance physical properties and performance. These ingredients include antimicrobial, anti-caries agents, plaque buffers, fluoride sources, vitamins, plant extracts, desensitizing agents, anti-calculus agents, biomolecules, flavors, proteinaceous materials, preservatives, opacifying agents, coloring agents, pH-adjusting agents, sweetening agents, particulate abrasive materials, polymeric compounds, buffers and salts to buffer the pH and ionic strength of the compositions, and mixtures thereof. Such ingredients typically and collectively make-up less than 20% by weight of the composition, and preferably, from 0.0 to 15% by weight, and most preferably, from 0.01 to 12% by weight of the composition, including all ranges subsumed therein.
  • the reaction to prepare the sheet like crystals of calcium citrate for inclusion in the composition of the invention comprises the steps of (a) mixing a calcium salt with a water-soluble ionic citrate in an aqueous solution of a polyhydric alcohol for extended period of time to generate a precipitate; (b) filtering the precipitate and drying it to prepare the sheet like crystals of calcium citrate.
  • the preferred calcium salt for use in the above reaction are calcium chloride, calcium nitrate, or calcium acetate.
  • the preferred water-soluble ionic citrates for use in the above reaction are sodium citrate, potassium citrate, or ammonium citrate; most preferred being alkali metal citrates like sodium citrate or potassium citrate.
  • the preferred polyhydric alcohol for use in the reaction to prepare the calcium citrate of the invention are ethylene glycol, propylene glycol, glycerol, polyethylene glycol or polypropylene glycol, more preferably propylene glycol, glycerol, or polyethylene glycol.
  • the reaction to prepare the precipitate is generally carried out for 1 to 24 hours preferablylO to 16 hours.
  • the calcium citrate which is used in the present invention is therefore most preferably prepared using a process comprising the following steps: a) first mixing a water-soluble calcium salt with a water-soluble ionic citrate.
  • the preferred mole ratio of calcium ion to citrate ion is in the range of 2:1 to 1 :1 most preferably in a 3:2 molar ratio in an aqueous solution of polyhydric alcohol.
  • the polyhydric alcohol in the reaction mixture is preferably in the range of 5 to 20 wt% most preferably about 10 wt%, with respect to total reaction batch size.
  • the reaction is carried out for an extended period of time preferably at room temperature (about 25 °C), to generate a precipitate; b) the filtering the precipitate and c) drying it to prepare the calcium citrate.
  • a non-therapeutic method of whitening teeth comprising the steps of (i) applying the composition of the present invention on to a tooth surface for at least one minute; and (ii) rinsing the surface to be substantially free of the composition.
  • the method is preferably non-therapeutic i.e., for achieving cosmetic benefits.
  • Examples A-D, 1-3 Whitening provided by various samples within and outside the invention: The following samples were analyzed for whitening benefits using various samples.
  • Example - A Tea-stained hydroxyapatite (HAP) disk.
  • Step 1 Take 2 gm of tea leaves in a beaker.
  • Step 2 Add 100 ml boiling distilled water to the beaker and wait for two minutes.
  • Step 3 Filter the solution using a filter paper after two minutes, into a petri dish.
  • Step 4 Immerse pristine HAP disks into the solution (-100 ml volume, while the tea was still warm) for 5 minutes and then reverse the sides and let it sit for another 5 minutes.
  • Step 5 Dip rinse each disk in Milli Q water twice.
  • Step 6 Leave it in air for drying for 20-30 minutes, with the circular disk standing on its edge and both sides exposed to air.
  • Step 1 Drop 10OpI of test sample on the stained full disk.
  • Step 2 Spread the sample as evenly as possible across the disk.
  • Step 3 Let it dry in the air for 20 minutes.
  • Step 4 Keep it in the oven at 40°C for 10 minutes to dry and measure the L*a*b* values.
  • Example B Titania STV 455 at 1 wt%.
  • Example C Calcium citrate synthesized using conventional process (used at 1 wt%).
  • Example D Commercially available calcium citrate (used at 1 wt%).
  • Example 1 Calcium citrate synthesized using process of the invention with glycerol as the crystal habit modifier (used at 1 wt%).
  • Example 2 Calcium citrate synthesized using process of the invention with propylene glycol as the crystal habit modifier (used at 1 wt%).
  • Example 3 Calcium citrate synthesized using process of the invention with polyethylene glycol (68k) as the crystal habit modifier (used at 1 wt%).
  • the calcium citrate for Example C was prepared using the following procedure:
  • the calcium citrate for Examples 1-3 was prepared using the following procedure:
  • Powder sample was taken on a conducting carbon tape and then gold coated for 60 s under vacuum, SEM was analysed using Hitachi S4700 SEM machine at 10kV external voltage and 100 torr vacuum and different magnifications at 12 mm working distance.
  • L* presented here is the average of at least five measurements taken on the circular surface of 0.5 cm diameter in the SCI and SCE modes with small aperture.
  • Example 1 gives enhanced whitening on HAP discs as compared to conventional calcium citrate as well as conventional material like titanium dioxide (Examples A -D).
  • Example E-G and 4-6 Whitening obtained with different concentration of calcium citrate Experiments similar that in Table 1 were conducted except that a different concentration was used (0.5 wt%) instead of 1.0 wt%. The whiteness obtained is summarized in Table 2 below:

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  • Life Sciences & Earth Sciences (AREA)
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Abstract

L'invention concerne une composition de blanchiment des dents comprenant : (a) des cristaux de type feuille de citrate de calcium ayant une longueur moyenne dans la plage de 0,5 à 4 micromètres; une largeur moyenne dans la plage de 0,5 à 4 micromètres et une épaisseur moyenne dans la plage de 30 à 100 nanomètres ; et (b) un véhicule acceptable par voie orale, ladite composition étant une composition de soin buccal.
PCT/EP2021/080324 2020-11-19 2021-11-02 Composition de soin buccal pour des avantages de blanchiment WO2022106186A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
IN202021050497 2020-11-19
IN202021050497 2020-11-19
EP21150071.5 2021-01-04
EP21150071 2021-01-04

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WO2022106186A1 true WO2022106186A1 (fr) 2022-05-27

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2216816A (en) * 1938-06-13 1940-10-08 Pepsodent Co Dentifrice
US5219602A (en) 1991-12-20 1993-06-15 Kraft General Foods, Inc. Aqueous calcium citrate compositions
US5275806A (en) 1992-09-16 1994-01-04 Kraft General Foods, Inc. Topical compositions for protection against ultraviolet radiation
US20080050407A1 (en) * 2006-02-03 2008-02-28 Haas Michael S Oral care products comprising buffer systems for improved mineralization/remineralization benefits
WO2012143220A1 (fr) 2011-04-18 2012-10-26 Unilever Nv Compositions de soins bucco-dentaires permettant la reminéralisation des dents
EP3222326A1 (fr) 2016-03-23 2017-09-27 Unilever PLC Composition de dentifrice

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2216816A (en) * 1938-06-13 1940-10-08 Pepsodent Co Dentifrice
US5219602A (en) 1991-12-20 1993-06-15 Kraft General Foods, Inc. Aqueous calcium citrate compositions
US5275806A (en) 1992-09-16 1994-01-04 Kraft General Foods, Inc. Topical compositions for protection against ultraviolet radiation
US20080050407A1 (en) * 2006-02-03 2008-02-28 Haas Michael S Oral care products comprising buffer systems for improved mineralization/remineralization benefits
WO2012143220A1 (fr) 2011-04-18 2012-10-26 Unilever Nv Compositions de soins bucco-dentaires permettant la reminéralisation des dents
EP3222326A1 (fr) 2016-03-23 2017-09-27 Unilever PLC Composition de dentifrice

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
JUNFENG LI ET AL: "Preparation and properties of calcium citrate nanosheets for bone graft substitute", BIOENGINEERED, vol. 7, no. 5, 2 September 2016 (2016-09-02), US, pages 376 - 381, XP055658884, ISSN: 2165-5979, DOI: 10.1080/21655979.2016.1226656 *
LI JUN FENG ET AL: "Facile Self-Assembly Synthesis of Hierarchical 3D Flowerlike Calcium Citrate Microspheres", vol. 45, 1 January 2017 (2017-01-01), CH, pages 185 - 192, XP055814072, ISSN: 1662-5250, Retrieved from the Internet <URL:http://dx.doi.org/10.4028/www.scientific.net/JNanoR.45.185> DOI: 10.4028/www.scientific.net/JNanoR.45.185 *
SILVIA PABISCH ET AL: "Effect of interparticle interactions on size determination of zirconia and silica based systems A comparison of SAXS, DLS, BET, XRD and TEM", CHEMICAL PHYSICS LETTERS, ELSEVIER BV, NL, vol. 521, 18 November 2011 (2011-11-18), pages 91 - 97, XP028356279, ISSN: 0009-2614, [retrieved on 20111125], DOI: 10.1016/J.CPLETT.2011.11.049 *

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