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WO2015176867A1 - Toothpaste tube and composition - Google Patents

Toothpaste tube and composition Download PDF

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Publication number
WO2015176867A1
WO2015176867A1 PCT/EP2015/057620 EP2015057620W WO2015176867A1 WO 2015176867 A1 WO2015176867 A1 WO 2015176867A1 EP 2015057620 W EP2015057620 W EP 2015057620W WO 2015176867 A1 WO2015176867 A1 WO 2015176867A1
Authority
WO
WIPO (PCT)
Prior art keywords
tube
calcium
composition
composition according
phosphate
Prior art date
Application number
PCT/EP2015/057620
Other languages
French (fr)
Inventor
Cinzia Brignoli
Manuela MUCCIO
Original Assignee
Unilever Plc
Unilever N.V.
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 Plc, Unilever N.V., Conopco, Inc., D/B/A Unilever filed Critical Unilever Plc
Publication of WO2015176867A1 publication Critical patent/WO2015176867A1/en

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B1/00—Layered products having a non-planar shape
    • B32B1/08—Tubular products
    • 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
    • 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
    • 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
    • A61K8/34—Alcohols
    • A61K8/345—Alcohols containing more than one hydroxy group
    • 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
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8141—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • A61K8/8147—Homopolymers or copolymers of acids; Metal or ammonium salts thereof, e.g. crotonic acid, (meth)acrylic acid; Compositions of derivatives of such polymers
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B32B15/085—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising polyolefins
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
    • 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
    • A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/87—Application Devices; Containers; Packaging
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2439/00—Containers; Receptacles
    • B32B2439/40—Closed containers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2597/00—Tubular articles, e.g. hoses, pipes

Definitions

  • the present invention relates to toothpaste tubes and compositions.
  • tubes having properties such that the correct dosage of toothpaste is dispensed.
  • Toothpastes have different viscosities and flow rates.
  • the present invention relates to a toothpaste tube that is adapted to the viscosity of the toothpaste, thus giving the benefit that when the tube is squeezed the correct amount of toothpaste is dosed. During storage temperature fluctuations can cause the viscosity of toothpaste to increase, the present invention mitigates this effect.
  • the present invention relates to a flexible, gas impermeable laminate tube and toothpaste composition therein, i) the tube comprises a laminate, the laminate comprising an inner polymer layer, a gas impermeable barrier layer, and an outer polymer layer, wherein the outer polymer layer comprising a thermoplastic polyolefine and polypropylene layer; ii) the toothpaste composition comprising: a. a water insoluble and/or slightly soluble calcium source; b. a phosphate source; c. thickener; and d. carrier humectants; and in which the toothpaste composition has a viscosity from 50,000 to 200,000 centipoise at a temperature of 20° C.
  • the toothpaste composition has a viscosity from 50,000 to 200,000 centipoise at a temperature of 20° C.
  • the present invention comprises a toothpaste tube.
  • the tube having a top end, a bottom end and a flexible wall made of a laminate.
  • the wall at the bottom end of the tube is crimped to form a seal
  • the top end of the tube has a shoulder sealed to and approximately perpendicular to the wall, the shoulder preferably being made of a material which is more rigid than the wall.
  • the shoulder preferably comprises or provides a support for a nozzle.
  • the nozzle preferably having a cap, such that the container may be sealed.
  • the tube comprises a laminate, the laminate comprising an inner polymer layer, a gas impermeable barrier layer, and an outer polymer layer, wherein the outer polymer layer comprising a polyolefine and polypropylene layer.
  • the laminate of the tube comprises: a. an inner layer of non-reactive resin film; this layer is preferably polyethylene, polypropylene or mixtures thereof, b. barrier layer of aluminium foil, c. outer polymer layer comprising polyolefine layer and a polypropylene layer.
  • the outer layer laminate of the tube further comprises a linear low density polyethylene polypropylene or mixtures thereof.
  • a tie layer is preferably present between the polymeric layers and the barrier layer.
  • the toothpaste composition according to the invention comprises: a) a water insoluble and/or slightly soluble calcium source; b) a phosphate source; c) thickener; and d) carrier humectants; and
  • the toothpaste composition has a viscosity from 50,000 to 200,000 centipoise. It should be noted that in the context of the present invention all viscosities are measured at a temperature of 20° C with a Brookfield Viscometer, Spindle No. 4.
  • the viscosity at 20° C is from 60,000 to 180,000 centipoise, and most preferably, from 65,000 to 165,000 centipoise.
  • Soluble and insoluble calcium source refers to the solubility of the calcium source in water.
  • Soluble means a source that dissolves in water to give a solution with a concentration of at least 0.1 moles per litre at room temperature.
  • Insoluble means a source that dissolves in water to give a solution with a concentration of less than 0.001 moles per litre at room temperature.
  • Slightly soluble therefore, is defined to mean a source that dissolves in water to give a solution with a concentration of greater than 0.001 moles per litre at room temperature and less than 0.1 moles per litre at room temperature.
  • Substantially free of, as used herein, means less than 1.5%, and preferably, less than 1.0%, and most preferably, from 0.0 to 0.75% by weight, based on total weight of the oral care composition, including all ranges subsumed therein.
  • Single- phase composition means a one phase composition having both calcium and phosphate sources therein and prior to dispensing or unpackaging and use.
  • Anhydrous, as used herein, means substantially free of water.
  • Generated calcium and phosphate comprising compound means a compound with calcium and phosphate like calcium phosphate and hydroxyapatite that is formed within the monophase product from distinct compounds comprising calcium and phosphate. Toothpaste compositions relates to pastes and gel compositions, preferably pastes.
  • the calcium source suitable for use in this invention is limited only to the extent that the same may be used in an oral cavity.
  • the calcium source employed is insoluble or slightly soluble in water, but most preferably, insoluble in water.
  • Illustrative examples of the types of calcium source that may be used in this invention include, for example, calcium phosphate (i.e., added), calcium gluconate, calcium oxide, calcium lactate, calcium carbonate, calcium hydroxide, calcium sulfate, calcium carboxymethyl cellulose, calcium alginate, calcium salts of citric acid, calcium silicate, mixtures thereof or the like.
  • the calcium source is calcium silicate.
  • the calcium silicate used is (CaSi0 3 ) whereby the same is made commercially available under the name Microcal ET by Ineos Silicas, Ltd.
  • the calcium source is insoluble calcium silicate, present as the composite material calcium oxide-silica (CaO-Si0 2 ) as described in commonly-owned application Publication No. 2008/0151 17.
  • the ratio of calcium to silicon may be from 1 :10 to 3:1.
  • the Ca:Si ratio is preferably from 1 :5 to 2:1 , and more preferably, from 1 :3 to 2:1 , and most preferably, from about 1 :2 to 2:1 .
  • the calcium silicate may comprise mono-calcium silicate, bi-calcium silicate, or tri-calcium silicate whereby ratios of calcium to silicon (Ca:Si) should be understood to be atom ratios.
  • the calcium source employed in this invention may be in a crystalline or amorphous state, and preferably, the same is in an amorphous state.
  • the calcium source is in a mesoporous state, i.e. the source is a material having pores with diameters from 1 nm to 50 microns.
  • Mesoporous calcium silicate (MCS) is often preferred.
  • MCS Mesoporous calcium silicate
  • the MCS which may be used in this invention can be made by combining a calcium salt, a silica precursor like silicate and a structure-directing agent to yield a solid suitable for calcinating. A more detailed description of the process that may be conducted to make the MCS suitable for use in this invention is described in the aforementioned commonly- owned application, Publication No.
  • the amount of calcium source in the composition of this invention is typically from 0.1 to 50%, and preferably, from 1 to 30%, and most preferably, from 5 to 20% by weight of the oral care composition based on total weight of the oral care composition and including all ranges subsumed therein.
  • composition is a single phase composition.
  • the phosphate source that may be used in this invention is limited only to the extent that the same may be used in a composition suitable for use in an oral cavity.
  • Illustrative examples of the types of phosphate source suitable for use in this invention include monosodium phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, sodium pyrophosphate, tetrasodium pyrophosphate, sodium tripolyphosphate, sodium hexametaphosphate, potassium dihydrogenphosphate, trisodium phosphate, tripotassium phosphate, mixtures thereof or the like.
  • the phosphate source is preferably one which is water soluble.
  • the phosphate source makes up from 0.5 to 15%, and preferably, from 2 to 12%, and most preferably, from 4 to 9% by weight of the oral care composition, based on total weight of the oral care composition and including all ranges subsumed therein.
  • the phosphate source used is one which results in an oral care composition having a pH from 5.5 to 8, preferably from 6 to 7.5, and most preferably, about neutral.
  • the phosphate source used is trisodium phosphate and monosodium dihydrogen phosphate at a trisodium phosphate to monosodium dihydrogen phosphate weight ratio of 1 :4 to 4:1 , preferably 1 :3 to 3:1 , and most preferably, from 1 :2 to 2:1 , including all ratios subsumed therein.
  • compositions described herein may comprise ingredients which are common in the art, such as: ⁇ antimicrobial agents, e.g. Triclosan, chlorhexidine, copper-, zinc- and stannous salts such as zinc citrate, zinc sulphate, zinc glycinate, sodium zinc citrate and stannous pyrophosphate, sanguinarine extract, metronidazole, quaternary ammonium compounds, such as cetylpyridinium chloride; bis-guanides, such as chlorhexidine digluconate, hexetidine, octenidine, alexidine; and halogenated bisphenolic compounds such as 2,2' methylenebis-(4-chloro-6-bromophenol);
  • ⁇ antimicrobial agents e.g. Triclosan, chlorhexidine, copper-, zinc- and stannous salts such as zinc citrate, zinc sulphate, zinc glycinate, sodium zinc citrate and stannous pyrophosphate, sanguinarine extract, met
  • anti-inflammatory agents such as ibuprofen, flurbiprofen, aspirin, indomethacin, etc.
  • anti-caries agents such as sodium trimetaphosphate and casein;
  • plaque buffers such as urea, calcium lactate, calcium glycerophosphate and strontium polyacrylates
  • vitamins such as Vitamins A, C and E;
  • desensitizing agents e.g. potassium citrate, potassium chloride, potassium tartrate, potassium bicarbonate, potassium oxalate, and potassium nitrate;
  • anti-calculus agents e.g. alkali-metal pyrophosphates, hypophosphite-containing polymers, organic phosphonates and phosphocitrates, etc.;
  • biomolecules e.g. bacteriocins, antibodies, enzymes, etc.
  • flavors e.g., peppermint and spearmint oils
  • proteinaceous materials such as collagen
  • coloring agents like FD&C blue, yellow and/or red dyes/colorants
  • surfactants such as anionic, nonionic, cationic and zwitterionic or amphoteric surfactants (e.g., sodium lauryl sulfate, sodium dodecylbenzene sulfonate);
  • particulate abrasive materials such as abrasive silicas, aluminas, calcium carbonates, zirconium silicate, polymethylmethacrylate, dicalciumphosphates, calcium pyrophosphates, hydroxyapatites, trimetaphosphates, insoluble
  • hexametaphosphates as well as agglomerated particulate abrasive materials
  • fluoride sources like sodium fluoride, stannous fluoride, sodium
  • polymeric compounds which can enhance the delivery of active ingredients such as antimicrobial agents can also be included.
  • examples of such polymers are copolymers of polyvinylmethylether with maleic anhydride and other similar delivery enhancing polymers, e.g., those described in DE-A03,942,643; ⁇ buffers and salts to buffer the pH and ionic strength of the oral care compositions; and
  • bleaching agents such as peroxy compound, e.g., potassium peroxydiphosphate, effervescing systems such as sodium bicarbonate/citric acid systems, colour change systems, and the like.
  • Such ingredients common in the art typically and collectively make-up less than 20% by weight of the oral care composition, and preferably, from 0.0 to 15% by weight, and most preferably, from about 0.01 to about 12% by weight of the oral care composition, including all ranges subsumed therein.
  • Thickener may also be used in this invention and is limited only to the extent that the same may be added to a composition suitable for use in an oral cavity.
  • Illustrative examples of the types of thickeners that may be used in this invention include, sodium carboxymethyl cellulose, hydroxyl ethyl cellulose, methyl cellulose, ethyl cellulose, gum tragacanth, gum Arabic, gum karaya, sodium alginate, carrageenan, guar, xanthan gum, Irish moss, starch, modified starch, silica based thickeners including silica aerogels, magnesium aluminum silicate (i.e., Veegum) Carbomers (cross-linked acrylates) and mixtures thereof.
  • silica based thickeners including silica aerogels, magnesium aluminum silicate (i.e., Veegum) Carbomers (cross-linked acrylates) and mixtures thereof.
  • sodium carboxymethyl cellulose and/or Carbomers are preferred.
  • Carbomer those having a molecular weight of at least 700,000 are desired, and preferably, those having a molecular weight of at least 1 ,200,000, and most preferably, those having a molecular weight of at least about 2,500,000 are desired. Mixtures of Carbomers may also be used herein.
  • the Carbomer is Carbopol ® 980. It has been described as a high molecular weight and cross-linked polyacrylic acid and identified via CAS number 9063-87-0. The same is available commercially from Lubrizol Advanced Materials, Inc.
  • Thickener typically makes up from 0.01 to about 10%, and preferably, from 0.1 to 8%, and most preferably, from 1.5 to 6% by weight of the oral care composition, based on total weight of the oral care composition and including all ranges subsumed therein.
  • Suitable carrier humectants are preferably used in the oral care composition of the present invention and they 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.
  • the carrier humectants should, in any case, be substantially free of water, and preferably, anhydrous. The same, for example, can be used in solid form, whereby glycerin is the preferred carrier humectant.
  • the carrier humectant is used to take the balance of the compositions up to 100%, and the same may be present in the range of from 10 to 90% by weight of the oral care composition.
  • the carrier humectant makes up from 25 to 80%, and most preferably, from 45 to 70% by weight of the oral care composition, based on total weight of the oral care composition and including all ranges subsumed therein.
  • the compositions of this invention are prepared by conventional methods of making oral care formulations. Such methods include mixing the ingredients under moderate shear and atmospheric pressure.
  • the compositions are used in the oral cavity, and preferably, are of the form that may be brushed onto teeth with a toothbrush.
  • the stable oral care compositions of this invention result in remineralisation of teeth (i.e., new hydroxyapatite formation) and teeth whitening.
  • use (for a period of about two weeks to one month) of the stable oral care composition of the present invention will result in a new hydroxyapatite layer on teeth that is from 0.5 to 20 microns, and preferably, from 0.75 to 5 microns, including all ranges subsumed therein.
  • Oral care compositions were prepared by mixing (in weight percent) the following ingredients under moderate shear until a homogeneous composition was obtained.
  • composition was stored in a second tube (Example A) not according to the invention, (tube originally used for Signal _ Italy 2014).
  • the storage data is as follows: Temperature Example A Example 1
  • formulations stored in the tubes of the invention are more stable in storage and thus easier to squeeze from the tube than the identical formulation stored in a more conventional tube.
  • the tube according to the invention has a soft feel, thus providing the correct level of pressure by the consumer and the correct dosing of the toothpaste.

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Epidemiology (AREA)
  • Birds (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
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  • Oral & Maxillofacial Surgery (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Cosmetics (AREA)

Abstract

A flexible, gas impermeable laminate tube and toothpaste composition therein, i) the tube comprises a laminate, the laminate comprising an inner polymer layer, gas impermeable barrier layer, and an outer polymer layer, wherein the outer polymer layer comprises a polyolefine and polypropylene layer; ii) the toothpaste composition comprising: a. a water insoluble and/or slightly soluble calcium source; b. a phosphate source; c. thickener; and d. carrier humectants; and in which the toothpaste composition has a viscosity from 50,000 to 200,000 centipoise at a temperature of 20° C.

Description

TOOTHPASTE TUBE AND COMPOSITION
The present invention relates to toothpaste tubes and compositions. In particular, tubes having properties such that the correct dosage of toothpaste is dispensed.
Toothpastes have different viscosities and flow rates. The present invention relates to a toothpaste tube that is adapted to the viscosity of the toothpaste, thus giving the benefit that when the tube is squeezed the correct amount of toothpaste is dosed. During storage temperature fluctuations can cause the viscosity of toothpaste to increase, the present invention mitigates this effect.
Description of the Invention
The present invention relates to a flexible, gas impermeable laminate tube and toothpaste composition therein, i) the tube comprises a laminate, the laminate comprising an inner polymer layer, a gas impermeable barrier layer, and an outer polymer layer, wherein the outer polymer layer comprising a thermoplastic polyolefine and polypropylene layer; ii) the toothpaste composition comprising: a. a water insoluble and/or slightly soluble calcium source; b. a phosphate source; c. thickener; and d. carrier humectants; and in which the toothpaste composition has a viscosity from 50,000 to 200,000 centipoise at a temperature of 20° C. Detailed Description of the Invention
Toothpaste Tube
The present invention comprises a toothpaste tube. The tube having a top end, a bottom end and a flexible wall made of a laminate.
Preferably the wall at the bottom end of the tube is crimped to form a seal, and preferably the top end of the tube has a shoulder sealed to and approximately perpendicular to the wall, the shoulder preferably being made of a material which is more rigid than the wall. The shoulder preferably comprises or provides a support for a nozzle. The nozzle preferably having a cap, such that the container may be sealed.
The tube comprises a laminate, the laminate comprising an inner polymer layer, a gas impermeable barrier layer, and an outer polymer layer, wherein the outer polymer layer comprising a polyolefine and polypropylene layer.
Preferably the laminate of the tube comprises: a. an inner layer of non-reactive resin film; this layer is preferably polyethylene, polypropylene or mixtures thereof, b. barrier layer of aluminium foil, c. outer polymer layer comprising polyolefine layer and a polypropylene layer.
Preferably the outer layer laminate of the tube further comprises a linear low density polyethylene polypropylene or mixtures thereof.
A tie layer is preferably present between the polymeric layers and the barrier layer.
Composition
The toothpaste composition according to the invention comprises: a) a water insoluble and/or slightly soluble calcium source; b) a phosphate source; c) thickener; and d) carrier humectants; and
The toothpaste composition has a viscosity from 50,000 to 200,000 centipoise. It should be noted that in the context of the present invention all viscosities are measured at a temperature of 20° C with a Brookfield Viscometer, Spindle No. 4.
Preferably the viscosity at 20° C is from 60,000 to 180,000 centipoise, and most preferably, from 65,000 to 165,000 centipoise.
Soluble and insoluble calcium source, as used herein, refers to the solubility of the calcium source in water. Soluble means a source that dissolves in water to give a solution with a concentration of at least 0.1 moles per litre at room temperature. Insoluble means a source that dissolves in water to give a solution with a concentration of less than 0.001 moles per litre at room temperature. Slightly soluble, therefore, is defined to mean a source that dissolves in water to give a solution with a concentration of greater than 0.001 moles per litre at room temperature and less than 0.1 moles per litre at room temperature. Substantially free of, as used herein, means less than 1.5%, and preferably, less than 1.0%, and most preferably, from 0.0 to 0.75% by weight, based on total weight of the oral care composition, including all ranges subsumed therein. Single- phase composition means a one phase composition having both calcium and phosphate sources therein and prior to dispensing or unpackaging and use. Anhydrous, as used herein, means substantially free of water. Generated calcium and phosphate comprising compound means a compound with calcium and phosphate like calcium phosphate and hydroxyapatite that is formed within the monophase product from distinct compounds comprising calcium and phosphate. Toothpaste compositions relates to pastes and gel compositions, preferably pastes. The calcium source suitable for use in this invention is limited only to the extent that the same may be used in an oral cavity. In a preferred embodiment, the calcium source employed is insoluble or slightly soluble in water, but most preferably, insoluble in water. Illustrative examples of the types of calcium source that may be used in this invention include, for example, calcium phosphate (i.e., added), calcium gluconate, calcium oxide, calcium lactate, calcium carbonate, calcium hydroxide, calcium sulfate, calcium carboxymethyl cellulose, calcium alginate, calcium salts of citric acid, calcium silicate, mixtures thereof or the like. In a preferred embodiment the calcium source is calcium silicate. In a more preferred embodiment, the calcium silicate used is (CaSi03) whereby the same is made commercially available under the name Microcal ET by Ineos Silicas, Ltd.
In yet another preferred embodiment, the calcium source is insoluble calcium silicate, present as the composite material calcium oxide-silica (CaO-Si02) as described in commonly-owned application Publication No. 2008/0151 17.
When a calcium silicate composite material is employed, the ratio of calcium to silicon (Ca:Si) may be from 1 :10 to 3:1. The Ca:Si ratio is preferably from 1 :5 to 2:1 , and more preferably, from 1 :3 to 2:1 , and most preferably, from about 1 :2 to 2:1 . The calcium silicate may comprise mono-calcium silicate, bi-calcium silicate, or tri-calcium silicate whereby ratios of calcium to silicon (Ca:Si) should be understood to be atom ratios.
The calcium source employed in this invention may be in a crystalline or amorphous state, and preferably, the same is in an amorphous state. In an often preferred embodiment, the calcium source is in a mesoporous state, i.e. the source is a material having pores with diameters from 1 nm to 50 microns. Mesoporous calcium silicate (MCS) is often preferred. The MCS which may be used in this invention can be made by combining a calcium salt, a silica precursor like silicate and a structure-directing agent to yield a solid suitable for calcinating. A more detailed description of the process that may be conducted to make the MCS suitable for use in this invention is described in the aforementioned commonly- owned application, Publication No. WO 2008/0151 17. The amount of calcium source in the composition of this invention is typically from 0.1 to 50%, and preferably, from 1 to 30%, and most preferably, from 5 to 20% by weight of the oral care composition based on total weight of the oral care composition and including all ranges subsumed therein.
Preferably the composition is a single phase composition.
The phosphate source that may be used in this invention is limited only to the extent that the same may be used in a composition suitable for use in an oral cavity. Illustrative examples of the types of phosphate source suitable for use in this invention include monosodium phosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, sodium pyrophosphate, tetrasodium pyrophosphate, sodium tripolyphosphate, sodium hexametaphosphate, potassium dihydrogenphosphate, trisodium phosphate, tripotassium phosphate, mixtures thereof or the like. The phosphate source is preferably one which is water soluble.
Typically, the phosphate source makes up from 0.5 to 15%, and preferably, from 2 to 12%, and most preferably, from 4 to 9% by weight of the oral care composition, based on total weight of the oral care composition and including all ranges subsumed therein. In a preferred embodiment, the phosphate source used is one which results in an oral care composition having a pH from 5.5 to 8, preferably from 6 to 7.5, and most preferably, about neutral. In a most preferred embodiment, the phosphate source used is trisodium phosphate and monosodium dihydrogen phosphate at a trisodium phosphate to monosodium dihydrogen phosphate weight ratio of 1 :4 to 4:1 , preferably 1 :3 to 3:1 , and most preferably, from 1 :2 to 2:1 , including all ratios subsumed therein.
The oral care compositions described herein may comprise ingredients which are common in the art, such as: ■ antimicrobial agents, e.g. Triclosan, chlorhexidine, copper-, zinc- and stannous salts such as zinc citrate, zinc sulphate, zinc glycinate, sodium zinc citrate and stannous pyrophosphate, sanguinarine extract, metronidazole, quaternary ammonium compounds, such as cetylpyridinium chloride; bis-guanides, such as chlorhexidine digluconate, hexetidine, octenidine, alexidine; and halogenated bisphenolic compounds such as 2,2' methylenebis-(4-chloro-6-bromophenol);
anti-inflammatory agents such as ibuprofen, flurbiprofen, aspirin, indomethacin, etc. anti-caries agents such as sodium trimetaphosphate and casein;
plaque buffers such as urea, calcium lactate, calcium glycerophosphate and strontium polyacrylates;
vitamins such as Vitamins A, C and E;
plant extracts;
desensitizing agents, e.g. potassium citrate, potassium chloride, potassium tartrate, potassium bicarbonate, potassium oxalate, and potassium nitrate;
anti-calculus agents, e.g. alkali-metal pyrophosphates, hypophosphite-containing polymers, organic phosphonates and phosphocitrates, etc.;
biomolecules, e.g. bacteriocins, antibodies, enzymes, etc.
flavors, e.g., peppermint and spearmint oils;
proteinaceous materials such as collagen;
preservatives;
opacifying agents;
coloring agents like FD&C blue, yellow and/or red dyes/colorants;
pH-adjusting agents;
sweetening agents;
surfactants, such as anionic, nonionic, cationic and zwitterionic or amphoteric surfactants (e.g., sodium lauryl sulfate, sodium dodecylbenzene sulfonate);
particulate abrasive materials such as abrasive silicas, aluminas, calcium carbonates, zirconium silicate, polymethylmethacrylate, dicalciumphosphates, calcium pyrophosphates, hydroxyapatites, trimetaphosphates, insoluble
hexametaphosphates as well as agglomerated particulate abrasive materials;
fluoride sources like sodium fluoride, stannous fluoride, sodium
monofluorophosphate, zinc ammonium fluoride, tin ammonium fluoride, calcium fluoride, cobalt ammonium fluoride or mixtures thereof;
polymeric compounds which can enhance the delivery of active ingredients such as antimicrobial agents can also be included. Examples of such polymers are copolymers of polyvinylmethylether with maleic anhydride and other similar delivery enhancing polymers, e.g., those described in DE-A03,942,643; ■ buffers and salts to buffer the pH and ionic strength of the oral care compositions; and
■ other optional ingredients that may be included are, e.g., bleaching agents such as peroxy compound, e.g., potassium peroxydiphosphate, effervescing systems such as sodium bicarbonate/citric acid systems, colour change systems, and the like.
Such ingredients common in the art typically and collectively make-up less than 20% by weight of the oral care composition, and preferably, from 0.0 to 15% by weight, and most preferably, from about 0.01 to about 12% by weight of the oral care composition, including all ranges subsumed therein.
Thickener may also be used in this invention and is limited only to the extent that the same may be added to a composition suitable for use in an oral cavity. Illustrative examples of the types of thickeners that may be used in this invention include, sodium carboxymethyl cellulose, hydroxyl ethyl cellulose, methyl cellulose, ethyl cellulose, gum tragacanth, gum Arabic, gum karaya, sodium alginate, carrageenan, guar, xanthan gum, Irish moss, starch, modified starch, silica based thickeners including silica aerogels, magnesium aluminum silicate (i.e., Veegum) Carbomers (cross-linked acrylates) and mixtures thereof.
Typically, sodium carboxymethyl cellulose and/or Carbomers are preferred. When a Carbomer is employed, those having a molecular weight of at least 700,000 are desired, and preferably, those having a molecular weight of at least 1 ,200,000, and most preferably, those having a molecular weight of at least about 2,500,000 are desired. Mixtures of Carbomers may also be used herein.
In an especially preferred embodiment, the Carbomer is Carbopol® 980. It has been described as a high molecular weight and cross-linked polyacrylic acid and identified via CAS number 9063-87-0. The same is available commercially from Lubrizol Advanced Materials, Inc.
Thickener typically makes up from 0.01 to about 10%, and preferably, from 0.1 to 8%, and most preferably, from 1.5 to 6% by weight of the oral care composition, based on total weight of the oral care composition and including all ranges subsumed therein. Suitable carrier humectants are preferably used in the oral care composition of the present invention and they 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. The carrier humectants should, in any case, be substantially free of water, and preferably, anhydrous. The same, for example, can be used in solid form, whereby glycerin is the preferred carrier humectant.
The carrier humectant is used to take the balance of the compositions up to 100%, and the same may be present in the range of from 10 to 90% by weight of the oral care composition. Preferably, the carrier humectant makes up from 25 to 80%, and most preferably, from 45 to 70% by weight of the oral care composition, based on total weight of the oral care composition and including all ranges subsumed therein. The compositions of this invention are prepared by conventional methods of making oral care formulations. Such methods include mixing the ingredients under moderate shear and atmospheric pressure. The compositions are used in the oral cavity, and preferably, are of the form that may be brushed onto teeth with a toothbrush. Unexpectedly, the stable oral care compositions of this invention result in remineralisation of teeth (i.e., new hydroxyapatite formation) and teeth whitening. Typically, use (for a period of about two weeks to one month) of the stable oral care composition of the present invention will result in a new hydroxyapatite layer on teeth that is from 0.5 to 20 microns, and preferably, from 0.75 to 5 microns, including all ranges subsumed therein. The invention will now be demonstrated by the following non-limiting Examples:
Examples Oral care compositions (monophase) were prepared by mixing (in weight percent) the following ingredients under moderate shear until a homogeneous composition was obtained.
Figure imgf000010_0001
The toothpastes described above were placed in a tube made according to the invention (Example 1 ) from the following laminate:
· External Layer low density polyethylene/polypropylene
• Aluminium foil
• Internal Layer polyethylene
For comparison the composition was stored in a second tube (Example A) not according to the invention, (tube originally used for Signal _ Italy 2014).
The storage data is as follows: Temperature Example A Example 1
5°C 1 1600ο 108000
25°C 160000 188000
40°C 400000 328000
50°C Out of limits 7500000
It can thus be seen that formulations stored in the tubes of the invention are more stable in storage and thus easier to squeeze from the tube than the identical formulation stored in a more conventional tube.
It should be further noted that the tube according to the invention has a soft feel, thus providing the correct level of pressure by the consumer and the correct dosing of the toothpaste.

Claims

A flexible, gas impermeable laminate tube and toothpaste composition therein, i) the tube comprises a laminate, the laminate comprising an inner polymer layer, a gas impermeable barrier layer, and an outer polymer layer, wherein the outer polymer layer comprises a polyolefine and polypropylene layer; ii) the toothpaste composition comprising: a. a water insoluble and/or slightly soluble calcium source; b. a phosphate source; c. thickener; and d. carrier humectants; and in which the toothpaste composition has a viscosity from 50,000 to 180,000 centipoise at a temperature of 20° C.
A tube and composition according to claim 1 , in which the laminate of the tube comprises the following layers: a. an inner layer of non-reactive resin film; b. a barrier layer of aluminium foil, c. an outer polymer layer comprising a polyolefine and polypropylene layer.
A tube and composition according to claim 1 or claim 2, in which the inner layer of the laminate of the tube comprises an inner polylethylene layer.
4. A tube and composition according to any preceding claim in which the outer layer of the laminate of the tube comprises a low density polyethylene/polypropylene layer.
5. A tube and composition according to any preceding claim in which the composition is substantially free of water.
6. A tube and composition according to any preceding claim in which the phosphate source of the composition is water soluble.
7. A tube and composition according to any preceding claim in which the calcium
source of the composition comprises 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.
8. A tube and composition according to any of the preceding claim 8 in which the
calcium source is calcium silicate.
9. A tube and composition according to claim 9 in which the calcium silicate is one having a of Ca:Si ratio of 1 :10 to 3:1 .
10. A tube and composition according to any of the preceding claims wherein the
calcium source makes up from 0.1 to 50% by weight of the composition.
1 1 . A tube and composition according to any of the preceding claims wherein the
phosphate source of the composition is monosodium phosphate, sodium
dihydrogen phosphate, disodium hydrogen phosphate, sodium pyrophosphate, tetrasodium pyrophosphate, sodium tripolyphosphate, sodium hexametaphosphate, potassium dihydrogenphosphate, trisodium phosphate, tripotassium phosphate or a mixture thereof.
12. A composition according to claim 12 wherein the phosphate source is trisodium phosphate, disodium hydrogen phosphate, monosodium dihydrogen phosphate or a mixture thereof.
13. A tube and composition according to any preceding claim in which the thickener of the composition is carboxymethyl cellulose, Carbomer or a mixture thereof.
A tube and composition according to any of the preceding claims wherein the carrier humectants of the composition is s 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.
The composition according to any of the preceding claims in which the composition has a pH from 5.5 to 8.
16. The composition according to any preceding claim which is a single phase
composition.
PCT/EP2015/057620 2014-05-19 2015-04-08 Toothpaste tube and composition WO2015176867A1 (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018033427A1 (en) * 2016-08-19 2018-02-22 Unilever N.V. Oral care composition
EA038664B1 (en) * 2016-09-23 2021-09-30 ЮНИЛЕВЕР АйПи ХОЛДИНГС Б.В. Oral care composition
WO2022184874A1 (en) * 2021-03-05 2022-09-09 Unilever Ip Holdings B.V. Oral care composition

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003066320A2 (en) * 2002-02-04 2003-08-14 Colgate-Palmolive Company Container wall post-forming
WO2011109919A1 (en) * 2010-03-09 2011-09-15 Unilever Plc Stable oral care compositions
WO2012122898A1 (en) * 2011-03-11 2012-09-20 Colgate-Palmolive Company Packaging and materials for making same

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003066320A2 (en) * 2002-02-04 2003-08-14 Colgate-Palmolive Company Container wall post-forming
WO2011109919A1 (en) * 2010-03-09 2011-09-15 Unilever Plc Stable oral care compositions
WO2012122898A1 (en) * 2011-03-11 2012-09-20 Colgate-Palmolive Company Packaging and materials for making same

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018033427A1 (en) * 2016-08-19 2018-02-22 Unilever N.V. Oral care composition
EA038664B1 (en) * 2016-09-23 2021-09-30 ЮНИЛЕВЕР АйПи ХОЛДИНГС Б.В. Oral care composition
WO2022184874A1 (en) * 2021-03-05 2022-09-09 Unilever Ip Holdings B.V. Oral care composition

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