CN106456462A - Dentifrice compositions with improved fluoride stability - Google Patents
Dentifrice compositions with improved fluoride stability Download PDFInfo
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- CN106456462A CN106456462A CN201580024067.1A CN201580024067A CN106456462A CN 106456462 A CN106456462 A CN 106456462A CN 201580024067 A CN201580024067 A CN 201580024067A CN 106456462 A CN106456462 A CN 106456462A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
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- 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
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- 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
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- 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
- A61K8/73—Polysaccharides
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- 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
- A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
- A61K2800/28—Rubbing or scrubbing compositions; Peeling or abrasive compositions; Containing exfoliants
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/48—Thickener, Thickening system
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Abstract
The invention discloses dentifrice compositions with improved fluoride stability. Soluble fluoride ion stability is increased in certain dentifrice formulations with the use of carrageenan, particularly under alkaline pH conditions.
Description
Technical field
The present invention relates to having the dentifrice composition of fluoride sources.
Background technology
Dentifrice composition is known for tooth and oral health care.For many markets and consumer, water content
High (for example>45 weight %) and carbonate content is high (for example>25 weight %) preparation substrate be high performance-price ratio.Report
Lead, linear sulphated polysaccharide (such as carrageenan) is used in dentifrice composition as thickener.However, said preparation substrate has
When there is fluorine ion stability problem, when there is high temperature and/or long distribution time, such as in some developing countries market, institute
Problem of stating generally is aggravated.The beneficial effect of fluorine ion and its correlation is key for user's experience and product acceptability
's.Need to provide the dentifrice formulations of the fluorine ion stability with improvement.
Content of the invention
The present invention is based partially on following wonderful observation：Soluble fluoride ion stability is in the water using carrageenan
Increased in content height and the high dentifrice formulations of carbonate content.Additionally, this fluorine ion stability effect is more than pH 8,
Further enhance under the conditions of the preferably greater than pH of pH 8.0.In addition, in carrageenan, seemingly fluorine ion is steady for λ-carrageenan
The optimal one kind of qualitative performance.
Therefore, it is an advantage of the invention that the stability of soluble fluoride ion over time.Accelerating (such as 60 DEG C of high temperature
Lower 6 weeks) and long-range circumstances condition (1 year at such as 30 DEG C) under observe described advantage.
One aspect of the present invention provides dentifrice composition, and described dentifrice composition comprises：A () presses the weight of described composition
The water of gauge 45% to 75%, preferably 50% to 60% water；(b) by weight of the composition 25% to 50%, preferably
27% to 47%, preferably 27% to 37% calcic abrasive material is it is preferable that wherein said calcic abrasive material is calcium carbonate；C () presses described
The weight meter 0.0025% to 2% of composition, preferably 0.5% to 1.5% fluoride sources are it is preferable that wherein said fluorine ion
Source is sodium monofluorophosphate；(d) by weight of the composition 0.01%% to 7%, preferably 0.1% to 6% straight chain sulfuric acid
Change polysaccharide it is preferable that wherein said linear sulphated polysaccharide is carrageenan；(e) more than 8.0, preferably greater than 8.5, more excellent
Choosing is equal to or more than the pH of pH 9.
Another aspect of the present invention provides a kind of dentifrice composition, and described dentifrice composition comprises：A () presses described combination
The weight meter 45% to 75% of thing, preferably 50% to 60% water；B () by weight of the composition 25% to 50% is excellent
Select 27% to 47%, preferably 27% to 37% calcic abrasive material is it is preferable that wherein said calcic abrasive material includes calcium carbonate；C () presses
The weight meter 0.0025% to 2% of described composition, preferably 0.5% to 1.5% fluoride sources are it is preferable that described fluorine ion
Source comprises sodium monofluorophosphate；(d) by weight of the composition 0.01%% to 7%, preferably 0.1% to 6% λ-angle
Fork dish glue.
Another aspect of the present invention provides a kind of process adamantine method, and methods described includes using aforementioned claim
The step of described oral care composition brushing teeth.
Although specification is finally particularly pointed out by claims and is distinctly claimed the present invention, it is believed that this
Bright the present invention will be more fully understood by following explanation.
Brief description
Fig. 1 describes the dentifrice formulations of embodiment 1-15, and wherein embodiment 1,12,13,14 and 15 is control formulation.
Specific embodiment
Definition
As used herein, term " Oral carriers " refers to suitable carrier or composition, and it can be used for forming the present invention's
The composition and/or composition of the present invention is applied to by oral cavity in safe and efficient mode.
As used herein, term " include (comprising) " means to add step in addition to those specifically referring to and becomes
Point.This term covers term " consist of " and " substantially by ... form ".The composition of the present invention can comprise, by simultaneously base
By invention as described herein basis and notable condition and any additional or optional becoming as herein described in basis
Divide, component, step or restrictive condition form.
As used herein, term " effective dose " refers to that compound or the amount of composition be enough to facilitate positive beneficial effect,
Oral health beneficial effect, and/or sufficiently low amount to be to avoid serious side effect, that is, in the reasonable determination range of technical staff
The rational effective hazard ratio of interior offer.In one embodiment, " effective dose " refers to by weight of the composition at least
0.01%, or at least 0.1% material.
As used herein, except as otherwise noted, term " tooth powder " refer to for clean oral surfaces paste, gel, powder
End, tablet or liquid preparation.As used herein, term " tooth " refers to nature tooth and artificial teeth or artificial tooth.
Unless otherwise indicated, all percentages, number and ratio are based on the gross weight meter of the present composition.Unless it is another
Indicate outward, all these weight being related to ingredients listed are based on activity substance content meter, and therefore do not include may be included in can
Solvent in commercially available material or accessory substance.Herein, term " percentage by weight " is represented by " weight % ".Unless it is another
Indicate outward, as used herein, all molecular weight are weight average molecular weight, and it is gram/mol to represent.
As used herein, when in for claim, article " one " and " a kind of " are understood to mean one kind or many
Plant claimed or according to claims materials.
As used herein, term "comprising", " inclusion ", " containing " be meant that nonrestrictive, you can add do not affect
Other steps of result and other parts.Terms above cover term " by ... form " and " substantially by ... form ".
As used herein, word " preferred ", " preferably " and their variant refer to can provide in certain circumstances
Embodiment of the present invention of specific beneficial effect.However, other embodiments are alternatively under identical or other environment
Preferably.Additionally, it is disabled that the statement of one or more preferred embodiments is not offered as other embodiments, and not
It is intended to exclude other embodiments from the scope of the present invention.
Water
Herein, the composition of the present invention comprises by weight of the composition 45% to 75% water.In a reality
Apply in scheme, described composition comprises by weight of the composition 40% to 70%, or 45% to 65%, or 40% to
60%, or 50% to 70%, or 50% to 60%, or 45% to 55%, or 55% to 65%, or 50% to 60%, or about
55%, or the water of combinations thereof.Can add water in described preparation, and/or water can enter institute because comprising other compositions
State in composition.Preferably, described water is USP water.
Calcic abrasive material
The composition of the present invention comprises the calcic abrasive material of 25 weight % to 50 weight %, and wherein said calcic abrasive material is selected from carbon
Sour calcium, Dicalcium Phosphate, tricalcium phosphate, tricalcium orthophosphate, calcium metaphosphate, calcium polyphosphate, calcium voelckerite, sodium carbonate and they
Combination.In preferred embodiments, described composition comprises by weight of the composition 25% to 60%, more preferably
25% to 50%, even more preferably 25% to 40%, even more preferably still 26% to 39%, or 27% to 47%, or 27% to
37%, or 30% to 35%, or 30% to 34%, or the calcic abrasive material of combinations thereof.
In another preferred composition, described composition comprises the calcic abrasive material of percentage by weight illustrated above, its
Described in calcic abrasive material be calcium carbonate, and wherein said calcium carbonate has：2 microns to 7 microns, preferably 3 microns to 6 microns,
More preferably 3.4 microns to 5.8 microns of D50 particle size range；Or 8 microns to 15 microns, preferably 9 microns to 14 microns, more preferably
9.2 microns to 13.5 microns of D90；Or be less than 28 microns, preferably 1 micron to less than 27 microns, more preferably less than 26 microns or 1
Micron is to the D98 scope less than 26 microns.It is highly preferred that described calcium carbonate has the particle size range of above-mentioned D50 and D90 scope；
Even more preferably in the range of above-mentioned D50, D90 and D98.Astoundingly it is believed that having these above-mentioned particle size distribution
Calcium carbonate can increase fluorine ion stability beneficial effect.Fluorine ion stability can measure as described herein；And general as in
Measure described in state national standard method GB8372-2008.
In particle size distribution measurement, term " D50 " refers to mass median diameter, and it is considered as average grain by mass
Degree.I.e. D50 is the size in units of micron, described size by be distributed into higher than this half of diameter by mass and
Half less than this diameter by mass.Term D90 similarly refers to the size in units of micron, and described size separates low
In by mass the 90% of D90 distribution.And similarly, term D98 refers to the size in units of micron, described a size of
Distribution less than by mass the 98% of D98.
Using laser diffraction particle size measuring instrument, (such as Bettersize BT9300H, derives from DanDong Better
Instrument, China), measure the granularity of calcium carbonate (as raw material).In general, laser scattering technology passes through to measure
Particle is by working from the light of particle diffraction during laser beam.Particle scattered light at a certain angle, this and their size positive correlations.
Therefore, Bettersize BT9300H calculates size distribution using the light scattering mode being associated with sample.According to ISO
13320-1-1999 method.In brief, by pre-dispersed for calcium carbonate raw material (" DI- water ") in deionized water.Then by one
The calcium carbonate serosity determining volume is transferred in sampling unit, and described sampling unit is filled with DI- water as dispersion soln.Calcium carbonate
Particle passes through to recycle and ultrasonic dispersed, obtains granularity simultaneously and measures.
In one embodiment, described calcic abrasive material is calcium carbonate.In preferred embodiments, described calcic abrasive material
Selected from the natural whiting of fine gtinding, the calcium carbonate grinding, winnofil and combinations thereof.Preferred at one
In embodiment, described calcic abrasive material be selected from fine gtinding natural whiting, grind calcium carbonate and combinations thereof (
In the above-mentioned weight percentage ranges of calcic abrasive material；And there is above-mentioned D50, D90 and D98 measure).
The natural whiting (FGNC) of fine gtinding is one of the more preferably calcic abrasive material that can be used in the present invention.It obtains
From lime stone or marble.FGNC also heat treatment can carry out chemically or physically modification after applying during grinding or grinding.Allusion quotation
The coating material of type includes magnesium stearate or magnesium oleate.The form of FGNC can be ground by using different during process of lapping
Technology such as ball milling, air current classifying grind or spiral spray is ground and to be changed.One example of natural whiting is described in WO 03/
In 030850, it has 1 to 15 μm of median particle and 0.5 to 3m2The BET surface area of/g.Natural whiting can have 325 to
800 mesh, or the granularity selected from 325,400,600,800 mesh or their combinations；Or, described granularity is 0.1 to 30 micron, or
0.1 to 20 micron, or 5 to 20 microns.
In one embodiment, the present composition is free or substantially free of silicate.
PEG
The composition of the present invention can comprise polyethylene glycol (PEG), and it has the Different Weight percentage accounting for described composition
And various average molecular weight range.In one aspect of the invention, described composition has by weight of the composition
0.1% to 15%, preferably 0.2% to 12%, more preferably 0.3% to 10%, even more preferably from 0.5% to 7%, or 1% to 5%,
Or 1% to 4%, or 1% to 2%, or 2% to 3%, or 4% to 5%, or the PEG of combinations thereof.Another in the present invention
Individual aspect, PEG is to have 100 dalton to 1600 dalton, preferably 200 to 1000, or 400 to 800, or 500 to 700 dongle
, or the PEG of the average molecular weight range of combinations thereof.PEG is by oxirane and the ethylene glycol with below general formula
The addition reaction of equivalent and the water-soluble linear polymer that formed：H-(OCH2CH2)n-OH.One supplier of PEG is
CARBOWAXTMThe Dow Chemical Company of brand.
Sweetener
The oral care composition of this paper can comprise sweetener.These include sweetener such as saccharin, dextrose, sucrose, breast
Sugar, maltose, levulose, aspartame, Sodium Cyclamate, D-trp, dihydrochalcone, acesulfame potassium, Sucralose,
Neotame and their mixture.Consumption in oral cavity composition for the sweetener is generally by weight of the composition
0.005% to 5%, or 0.01% to 1%, or 0.1% to 0.5%, or combinations thereof.
Fluoride sources
Described composition can comprise the anti-caries agent of effective dose.In one embodiment, anti-caries agent is fluoride sources.
There may be enough fluorine ions with offer fluorinion concentration in 25 DEG C of compositions, and/or in one embodiment, consumption is pressed
The weight meter of described composition can be about 0.0025% to about 5%, or by weight of the composition about 0.005% to about
2.0%, to provide anti-caries efficacy.The example of the suitable material of generation fluorine ion is disclosed in United States Patent (USP) 3,535,421 He
In 3,678,154.Representational fluoride sources include：Stannous fluoride, sodium fluoride, potassium fluoride, amine fluoride, sodium monofluorophosphate and
Zinc fluoride.In one embodiment, described dentifrice composition comprises fluoride sources, described fluoride sources be selected from stannous fluoride,
Sodium fluoride and their mixture.In one embodiment, described fluoride sources are sodium monofluorophosphate, and wherein institute
State composition and comprise by weight of the composition 0.0025% to 2%, or 0.5% to 1.5%, or 0.6% to 1.7%,
Or the sodium monofluorophosphate of combinations thereof.In another embodiment, described composition comprises the weight by described composition
The fluoride sources of meter 0.0025% to 2%.
pH
The pH of dentifrice composition can be more than pH 7.8, or pH 8 to 13, and more preferably 9 to 12, or it is more than pH 8, or it is more than 9,
Or 9 to 11, or 9 to 10, or combinations thereof.
Describe a kind of method for evaluating tooth powder pH.Via having the pH meter that auto thermal compensation (ATC) is popped one's head in, survey
Determine pH.Described pH meter can be read to 0.001pH unit.Described pH electrode is selected from one of following：(i)Orion Ross
Sure-Flow combines：Vitreum-VWR#34104-834/Orion#8172BN or VWR#10010-772/Orion#
8172BNWP；Epoxy resin body-VWR#34104-830/Orion#8165BN or VWR#10010-770/Orion#8165BNWP；
Semimicro epoxy resin body-VWR#34104-837/Orion#8175BN or VWR#10010-774/Orion#3175BNWP；Or
(ii) Orion PerpHect combination：VWR#34104-843/Orion#8203BN semimicro vitreum；Or (iii) suitable etc.
Jljl.Auto thermal compensation is popped one's head in as Fisher Scientific catalog number (Cat.No.) 13-620-16.
Deionized water prepares the tooth powder slurries of 25 weight %, then using SORVALL RC 28S centrifuge and SS-34
Rotor, centrifugation 10 minutes (or equivalent gravitation, 24149g power) under 15000 rpms.After one minute or after stable reading, comment
Determine the pH of supernatant.Every time after pH evaluation, it is washed with deionized electrode.Wipe any excessive water with laboratory level thin paper.
When not in use, electrode is made to remain immersed in pH 7 buffer solution or suitable electrode storage liquid.
PH adjusting agent
This paper dentifrice composition can comprise the pH adjusting agent of effective dose, or wherein said pH adjusting agent is pH buffer.As
Used herein, pH adjusting agent refers to can be used for the reagent adjusting the pH of dentifrice composition to pH scope identified above.PH adjusts
Section agent may include alkali metal hydroxide, ammonium hydroxide, organoammonium compound, carbonate, sesquicarbonate, borate, silicic acid
Salt, phosphate, imidazoles and their mixture.Specific pH reagent includes monosodium phosphate (sodium dihydrogen phosphate), tertiary sodium phosphate
(Trisodium phosphate dodecahydrate or " TSP "), Sodium Benzoate, benzoic acid, NaOH, potassium hydroxide, alkali carbonate, carbon
Sour sodium, imidazoles, pyrophosphate, sodium gluconate, lactic acid, sodium lactate, citric acid, sodium citrate, phosphoric acid.In an embodiment
In, using by weight of the composition 0.01% to 3%, preferably 0.1% to 1% TSP, and the weight by described composition
Gauge 0.001% to 2%, preferably 0.01% to 0.3% monosodium phosphate.Without being bound by theory, TSP and monosodium phosphate also may be used
There is calcium ion sequestering activity, thus providing certain mono-fluor phosphate stability (in those preparations comprising mono-fluor phosphate
In).
Anti-calculus agent
Described dentifrice composition can comprise the anti-calculus agent of effective dose, and in one embodiment, its content is pressed described
The weight meter of composition can be about 0.05% to about 50%, or by weight of the composition about 0.05% to about 25%, or
About 0.1% to about 15%.Non-limiting example includes those described in the 64th section of US2011/0104081 A1, and US
Those described in 2012/0014883 the 63rd to 68 section of A1, and those described in references cited therein.One
Example is the pyrophosphate as pyrophosphate ion source.In one embodiment, described composition comprises tetrasodium pyrophosphate
(TSPP) or disodium pyrophosphate, or combinations thereof, comprise by weight of the composition preferably 0.01% to 2%, more excellent
Select 0.1% to 1% pyrophosphate.Without being bound by theory, TSPP not only can provide calcium chelation, thus reducing dental plaque shape
Become, and may also provide additional mono-fluor phosphate and stablize beneficial effect (in those preparations comprising mono-fluor phosphate).
Surfactant
This paper dentifrice composition can comprise surfactant.Described surfactant be selected from anion surfactant,
Nonionic surfactant, amphoteric surfactant, zwitterionic surfactant, cationic surfactant or they
Mixture.Described composition can comprise content based on the overall weight of described composition about 0.1% to about 10%, and about 0.025%
To about 9%, about 0.05% to about 5%, about 0.1% to about 2.5%, about 0.5% to about 2%, or the table of about 0.1% to about 1%
Face activating agent.The non-limiting example of anion surfactant may include be described in US 2012/0082630 A1 the 32nd, 33,
Those in 34 and 35 sections.The non-limiting example of amphion or amphoteric surfactant may include and is described in US 2012/
Those of the 36th section of 0082630 A1；Cationic surfactant may include those being described in the 37th section of described bibliography；
And nonionic surfactant may include those being described in the 38th section of described bibliography.In one embodiment, institute
State composition and comprise by weight of the composition 0.1% to 5%, preferably 0.1% to 3%, or 0.3% to 3%, or
1.2% to 2.4%, or 1.2% to 1.8%, or 1.5% to 1.8%, or the anion surfactant bay of combinations thereof
Base sodium sulphate (SLS).
Thickener
This paper dentifrice composition can comprise one or more thickener.The consumption of thickener is by weight of the composition
Can be about 0.01% to about 15%, or about 0.1% to about 10%, or about 0.1% to about 5%.Non-limiting example may include US
In 2008/0081023 the 134th to 137 section of A1 and those described in references cited therein.
In embodiments, described composition comprises linear sulphated polysaccharide as thickener.Carrageenan or carragheen
It is an example of linear sulphated polysaccharide.In general, carrageenan can be changed based on degree of sulfation, and it includes：
K- carrageenan, ι-carrageenan and λ-carrageenan.The combination of carrageenan can be used.In one embodiment, described
Composition comprises by weight of the composition 0.1% to 3%, preferably 0.5% to 2%, or 0.6% to 1.8%, or they
Combination linear sulphated polysaccharide.In one embodiment, using ι-carrageenan.
In one embodiment, described composition comprises silica agents, preferably by leading to that sodium silicate solution obtains
Cross with sour stabilization removal to obtain the thickening silica of very fine granular.One commercially available example is to derive from
Huber Engineered Materials'sBrand silica is (for example103、124、
113、115、163、165、167).In one embodiment, described composition comprises by weight of the composition 0.5%
To 5% silica agents, preferably by weight of the composition 1% to 4%, or 1.5% to 3.5%, or 2% to
3%, or 2% to 5%, or 1% to 3%, or the silica agents of combinations thereof.
In one embodiment, described composition comprises carboxymethylcellulose calcium (" CMC ").CMC passes through with alkali and a chlorine
Acetic acid or its sodium salt are processed, and are obtained by cellulose.Different variants commercially to be characterized by viscosity.One commercially available
Example is derived from the Aqualon of Ashland Special IngredientsTMBrand CMC (such as AqualonTM7H3SF；
AqualonTM9M3SF AqualonTMTM9A；AqualonTMTM12A).In one embodiment, described composition comprises
0.1% to 3% CMC by weight of the composition, preferably by weight of the composition 0.5% to 2%, or
0.6% to 1.8%, or the CMC of combinations thereof.
In still another embodiment, described thickener can comprise linear sulphated polysaccharide (such as carrageenan), CMC,
And the purpose for cost savings preferably also comprises thickening silica, reach viscosity and the appropriate balance of elasticity simultaneously.One
In individual embodiment, described composition comprises thickener, and described thickener comprises：A () is based on the weight of described dentifrice composition
0.01% to less than 1.4%, and preferably 0.1% to 1.3%, more preferably 0.5% to 1.3% carrageenan；(d) press described tooth
The weight meter of compound powder is more than 0.4 weight % to 2 weight %, and preferably 0.5% to 1.8%, more preferably 0.6% to 1.8%
Carboxymethylcellulose calcium (CMC).In still another embodiment, above-mentioned thickener also comprises based on the weight of described dentifrice composition
0.5% to 5%, preferably 1% to 4% thickening silica.
There is low content wetting agent or do not contain wetting agent
Confectionery composition can be substantially free of or not contain wetting agent, or the wetting agent comprising low content.With regard to the object of the invention
For, term " wetting agent " include edible polyalcohol for example glycerine, sorbierite, xylitol, butanediol, propane diols and they
Combination.In one embodiment, described wetting agent is selected from sorbierite, glycerine and combinations thereof.In another enforcement
In scheme, described wetting agent is sorbierite.In one embodiment, described composition comprises by weight of the composition
0% to the wetting agent less than 20%, preferably by weight of the composition 0% to 10%, or 0% to 5%, or 0% to
3%, or 0% to 2%, or 0% to 1%, or it is less than 20%, or it is less than 19%, 18%, 15%, 12%, 8%, 7%, 6%,
4%, 3%, 2%, 1%, or it is less than 0.5%；Or be more than 1%, or it is more than 2%, 5%, 10%, or 15%；Or combinations thereof
Wetting agent.In still another embodiment, described composition comprises to be less than 20% sorb by weight of the composition
Alcohol.
In the embodiment of alternative, the composition of the present invention comprises wetting agent, preferably by weight of the composition
1% to 15% wetting agent.
Colouring agent
Confectionery composition can comprise colouring agent.Titanium dioxide is an example of colouring agent.Titanium dioxide is to composition
Increase the white powder of opacity.The content of titanium dioxide may generally be about 0.25% by weight of the composition to about
5%.
Flavouring agent
The composition of this paper can comprise by weight of the composition about 0.001% to about 5%, or about 0.01% to about
4%, or about 0.1% to about 3%, or about 0.5% to about 2%, or 1% to 1.5%, or 0.5% to 1%, or combinations thereof
Flavor composition.In the broadest sense, using term flavor composition include flavor ingredients or sensory agent,
Or sensation reagent or combinations thereof.Flavor ingredients may include those described in the 39th section of US 2012/0082630 A1；
And sensory agent and sensory agent composition may include those described in 40 45 sections, and described document is herein incorporated by reference.No
Including flavor composition definition in be " sweetener " (as described above).
Data
Analysis method
Consistent with CNS method GB8372-2008, the method for evaluating soluble fluoride ion is described.Letter
For it, using ISE (ISE) measure tooth powder in soluble fluoride ion.The example of fluorine ion measuring instrument is
SARTORIUS PP-50, but equivalent can be used.Described ion gauge can be furnished with the tool of Orion Research Inc.
There is single liquid to meet the fluorine ion electrode special of reference electrode, catalog number (Cat.No.) 9609BNWP, but equivalent can be used.Using being accurate to
Sample prepared by the balance of 0.0001 gram (g).20g tooth powder is weighed in the 50mL plasticity beaker of taring, is then gradually added into
50mL deionized water, makes magnetic stirring bar stir in plasticity beaker simultaneously, until tooth powder is fully dispersed in solution.Will be whole
Solution is slowly transferred to avoid producing foam (thus can accurately measure volume) in 100mL plasticity volumetric flask, and adds
Ionized water, to reach 100mL cumulative volume, then rocks solution to form slurries manually.Then the slurries being formed are transferred to
In 10mL centrifuge tube, and at ambient temperature, it is centrifuged 10 minutes with 15000 rpms (RPM) (24149g power).Then will
0.5mL supernatant is transferred in 2mL micro centrifugal pipe, and the 4mol/L HCl of 0.7mL is added in described pipe.Then will
Described lid envelope, heats 10 minutes in 50 DEG C of water-baths.Then pipe content is transferred in 50mL volumetric flask.Also by following thing
Matter is added in described flask：The 4mol/L NaOH of 0.7mL is to neutralize described solution；The citrate buffer of 5mL is (hereafter
Further describe)；Add deionized water until reaching 50mL cumulative volume in flask；Then sample solution is gently mixed.Pass through
By 100g sodium citrate, 60mL glacial acetic acid, NaCl and 30g of 60g NaOH all with water dissolves, pH is adjusted to 5.0～5.5,
And deionized water dilutes citrate buffer, until it reaches 1000mL cumulative volume, prepares above-mentioned citrate buffer.
Again refer to sample solution, whole 50mL solution is transferred in 50mL plasticity beaker, and use described fluorine ion measuring instrument
And electrode, content of fluoride ion is evaluated based on fluorine ion calibration curve.
By respectively by 0.5mL, 1.0mL, 1.5mL, 2.0mL and 2.5mL fluorine ion standard liquid (100mg/kg) accurately
Measure to five 50mL plasticity volumetric flasks, preparation standard fluorine ion curve (w/w%).By 5mL citrate buffer (as above institute
State prepared) it is added in each corresponding flask, then every part of solution is diluted to scale by deionized water.Then, respectively by every part
Solution is transferred in 50mL plasticity beaker, measures potential E under magnetic stirring, records potential value, and draws E-logc (wherein
" c " is concentration) calibration curve.
Describe a kind of method for evaluating tooth powder pH.Via having the pH meter that auto thermal compensation (ATC) is popped one's head in, survey
Determine pH.Described pH meter can be read to 0.001pH unit.Described pH electrode is selected from one of following：(i)Orion Ross
Sure-Flow combines：Vitreum-VWR#34104-834/Orion#8172BN or VWR#10010-772/Orion#
8172BNWP；Epoxy resin body-VWR#34104-830/Orion#8165BN or VWR#10010-770/Orion#8165BNWP；
Semimicro epoxy resin body-VWR#34104-837/Orion#8175BN or VWR#10010-774/Orion#3175BNWP；Or
(ii) Orion PerpHect combination：VWR#34104-843/Orion#8203BN semimicro vitreum；Or (iii) suitable etc.
Jljl.Auto thermal compensation is popped one's head in as Fisher Scientific catalog number (Cat.No.) 13-620-16.
Deionized water prepares the tooth powder slurries of 25 weight %, then using SORVALL RC 28S centrifuge and SS-34
Rotor, centrifugation 10 minutes (or equivalent gravitation, 24149g power) under 15000 rpms.After one minute or after stable reading, comment
Determine the pH of supernatant.Every time after pH evaluation, it is washed with deionized electrode.Wipe any excessive water with laboratory level thin paper.
When not in use, electrode is made to remain immersed in pH 7 buffer solution or suitable electrode storage liquid.
Fig. 1 describes the dentifrice formulations of embodiment 1 15.Then, described embodiment provides the number being summarized in table 1 below -5
According to.
Table 1 below shows, in preparation described in embodiment 1-5, the amount of carrageenan used is higher, after aging 6 weeks at 60 DEG C
Soluble fluoride ion stability better.Adopt higher temperature to aggravate the unstability of any fluorine ion over time.
As described in Fig. 1 preparation, embodiment 1-5 is briefly summarized.In addition to tester E (i.e. embodiment 1) does not comprise any carrageenan
Embodiment 2-5 significantly comprises different amounts of ι-carrageenan (0.4 weight % is to 2 weight %).Embodiment 1-5 comprises 17 weight %
Wetting agent sorbierite.Embodiment 1-3 comprises sodium carboxymethylcellulose, and embodiment 4 and 5 does not comprise.Embodiment 1-4 comprises to increase
Thick silica, and embodiment 5 does not comprise.
Table 1：
Referring to upper table 1, the embodiment 5 with 2 weight % ι-carrageenan only has the drop-out value of 527ppm, illustrate with
The minimum soluble fluoride ion that 1/1000000th (ppm) count declines (rightmost hurdle).Soluble fluoride ion declines lower, preparation
More stable.Embodiment 5 has the ι-carrageenan of maximum amount among five embodiments, thus illustrating optimal in five kinds of preparations
Soluble fluoride ion stability.Tester E (embodiment 1) has the worst soluble fluoride ion stability of 910ppm.Embodiment
2nd, the amount of ι-carrageenan increases (being respectively 0.4,0.8 and 1.3 weight %) and illustrates soluble fluoride ion stability in 3 and 4
Increase, as declined what ppm value was confirmed by 893,711 and 648 soluble fluoride ion respectively.Sum it up, table 1 illustrates, angle
Fork dish glue is more, and the soluble fluoride ion stablizing described preparation is more.
Table 2 below illustrates, wait weight basis under show fluorine ion stability in terms of, λ-carrageenan be three kinds of carrageenans it
In optimal.As described in Fig. 1 preparation, embodiment 6-10 is briefly summarized.Embodiment 6,7 and 8 is respectively provided with 1 weight %, 2 weights
The ι of amount % and 3 weight %-carrageenan percentage by weight (weight %) increases.Embodiment 9 has the k- Irish moss of 2 weight %
Glue type, and embodiment 10 has the λ-carrageenan type of 2 weight %.
Table 2：
Referring to upper table 2, the embodiment 10 with 2 weight % λ-carrageenan only has the drop-out value of 671ppm, illustrates
Minimum soluble fluoride ion in terms of ppm declines (rightmost hurdle).Embodiment 7,8 and 10 is respectively provided with equivalent (2 weight %)
Each corresponding carrageenan type.λ-carrageenan (embodiment 10) is maximally effective to soluble fluoride ion stability, and k- angle
Fork dish glue (embodiment 9) is the most poorly efficient (1047).It should be noted that the amount of the ι-carrageenan of embodiment 6,7 and 8 is respectively
Increase, illustrate that soluble fluoride ion stability value increases (declined by 1011,828 and 749 relatively low ppm respectively and confirm).
Table 3 below illustrates, the dentifrice formulations comprising carrageenan are more excellent than two kinds of control formulation in fluorine ion stability.
Described in Fig. 1 preparation, embodiment 11,12 and 13 is briefly summarized.Embodiment 11 comprises the ι-carrageenan of 1.4 weight %.Right
According to thing A (embodiment 11) and tester B (embodiment 13) preparation, there is no any carrageenan.Tester A and tester B preparation
It is respectively provided with the sodium carboxymethylcelluloses (CMC) slightly more than embodiment 11 and thickening silica, it will be appreciated that comparison
Thing B also has tetrasodium pyrophosphate (TSPP).
Table 3：
Referring to table 3, data considers the possible fluorine ion stability effect of CMC, silica and TSP.Give and comprise angle
Fork dish glue embodiment 11 at 60 DEG C 4 weeks and 6 weeks and at 30 DEG C about one year soluble fluoride ion decline (ppm) relatively
Low, show compared with control formulation, carrageenan provides the fluorine ion stability of improvement in described preparation.Embodiment 12 is not wrapped
Containing carrageenan, but comprise tetrasodium pyrophosphate (TSPP).
Table 4 below illustrates, the pH more than 8.0 provides more preferable fluorine ion stability in dentifrice formulations described herein.By Fig. 1
Described in preparation, embodiment 11,14 and 15 is briefly summarized.Embodiment 11 is pH 9.4, and comprises the ι-angle of 1.414 weight %
Fork dish glue, and it is further noted that comprise CMC and silica.Tester C (embodiment 14) and tester D (embodiment
15) preparation is respectively 7.8 and 8.3 relatively low pH.Tester C and D also all comprise the ι of respectively 2 weight % and 1.4 weight %-
Carrageenan.The percentage by weight of the silica of tester C and D, saccharin and mono-fluor phosphate is slightly different from embodiment 11.With
Embodiment 11 is compared, and tester C and D also has the calcium carbonate (25 weight % are to 42 weight %) of lower content and high level
Water (65.32 weight % are to 48.96 weight %).
Table 4：
Referring to table 4, in three samples comprising ι-carrageenan, have 9.4 highest pH embodiment 11 at 60 DEG C
Lower 4 weeks, because compared with tester C and D of the high decline percentage being respectively provided with 60% and 58%, having 47% solubility
Fluorine ion declines and has optimal fluorine ion stability effect.Therefore, as shown by data, when being related to fluorine ion stability, pH
8.3 are better than 7.8, and pH 9.4 is better than 8.3.
Dimension value preset disclosed herein is not understood as being strictly limited to cited exact numerical.On the contrary, unless in addition
Indicate, otherwise each such dimension is intended to indicate that described value and around the functionally equivalent scope of this value.For example, it is disclosed as
The dimension of " 40mm " is intended to indicate that " about 40mm ".
Unless expressly excluded or in other words limited, by every herein cited document, including any cross reference
Or Patents or patent application and the application claim priority to it or any patent application of its advantage or patent,
All it is incorporated by reference in its entirety accordingly herein.Quoting of any document is not as disclosure any with the present invention or this paper to it
The accreditation of claimed prior art, or be not to its own or with any other bibliography or multiple reference
The combination of document proposes, advises or discloses the accreditation that this invents any aspect.Additionally, any implication when term in the present invention
Or define any implication with same term in the file being incorporated by reference or define during contradiction it should obey in the present invention
The middle implication giving this term or definition.
Although having illustrate and described specific embodiments of the present invention, those skilled in the art are come
Say and change and change it is readily apparent that multiple other can be made in the case of without departing from spirit and scope of the present invention.Therefore,
It is intended to cover all these changes and the modification belonging in the scope of the invention in claims.
Claims (15)
1. a kind of dentifrice composition, described dentifrice composition comprises：
(a) by weight of the composition 45% to 75% water；
(b) by weight of the composition 25% to 50% calcic abrasive material；
(c) by weight of the composition 0.0025% to 2% fluoride sources；
(d) by weight of the composition 0.01% to 7% linear sulphated polysaccharide；With
E pH that () is more than 8.
2. composition according to claim 1, wherein said pH is more than 8.0, and preferably described pH is more than 8.5, more preferably
The described pH in ground is equal to or more than pH 9.
3. composition according to claim 1 and 2, wherein said linear sulphated polysaccharide is carrageenan, preferably institute
State the described carrageenan that composition comprises by weight of the composition 0.1% to 6%.
4. composition according to claim 3, wherein carrageenan are selected from k- carrageenan, ι-carrageenan, λ-angle fork
Dish glue.
5., according to composition in any one of the preceding claims wherein, wherein said water is by weight of the composition
50% to 60%.
6., according to composition in any one of the preceding claims wherein, wherein said calcic abrasive material comprises calcium carbonate, wherein excellent
Calcium carbonate described in selection of land is selected from natural whiting, the calcium carbonate grinding, winnofil and the combinations thereof of fine gtinding；
Wherein more preferably described calcium carbonate is selected from natural whiting, the calcium carbonate grinding and the combinations thereof of fine gtinding.
7., according to composition in any one of the preceding claims wherein, the weight of described composition pressed by wherein said calcic abrasive material
It is calculated as 27% to 47%, preferably described calcic abrasive material is 27% to 37% by weight of the composition.
8., according to composition in any one of the preceding claims wherein, wherein said composition also comprises by described composition
The surfactant of weight meter 0.1% to 12%, preferably comprises by weight of the composition 1% to 9% described table
Face activating agent, more preferably wherein said surfactant is anion surfactant, still more preferably wherein said cloudy from
Sub- surfactant is NaLS.
9., according to composition in any one of the preceding claims wherein, wherein said fluoride sources are sodium monofluorophosphate.
10., according to composition in any one of the preceding claims wherein, wherein said composition also comprises wetting agent, preferably
Wherein said wetting agent is 1% to 20% by weight of the composition, and more preferably wherein said wetting agent presses described group
The weight of compound is calculated as 1% to 10%, even more preferably still wherein said wetting agent be selected from glycerine, sorbierite and they
Combination.
A kind of 11. dentifrice compositions, described dentifrice composition comprises：
(a) by weight of the composition 45% to 75% water；
(b) by weight of the composition 25% to 50% calcic abrasive material；
(c) by weight of the composition 0.0025% to 2% fluoride sources；With
(d) by weight of the composition 0.01% to 7% λ-carrageenan.
12. compositions according to claim 11, wherein said λ-carrageenan has D- galactolipin -2- sulfuric ester-D-
Galactolipin -2,6- di-sulfate repetitive, provide based on the weight of described λ-carrageenan 30% to 40% sulfuric ester to contain
Amount, wherein preferably described λ-carrageenan is 0.1% to 6% by weight of the composition.
13. compositions according to claim 11 or 12, wherein said pH is more than 8, and preferably described pH is more than 8.0, more
Preferably described pH is more than 8.5, and even more preferably still described pH is equal to or more than pH 9.
14. compositions according to claim 11,12 or 13, wherein said calcic abrasive material comprises calcium carbonate, preferably institute
Stating calcic abrasive material is 27% to 47% by weight of the composition.
The 15. a kind of adamantine methods of process, methods described is included with according to tooth powder in any one of the preceding claims wherein
The step of composition brushing teeth.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNPCT/CN2014/077529 | 2014-05-15 | ||
| PCT/CN2014/077529 WO2015172344A1 (en) | 2014-05-15 | 2014-05-15 | Dentifrice compositions with improved fluoride stability |
| PCT/CN2015/077634 WO2015172651A1 (en) | 2014-05-15 | 2015-04-28 | Dentifrice compositions with improved fluoride stability |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106456462A true CN106456462A (en) | 2017-02-22 |
Family
ID=54479164
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|---|---|---|---|
| CN201580024067.1A Pending CN106456462A (en) | 2014-05-15 | 2015-04-28 | Dentifrice compositions with improved fluoride stability |
Country Status (8)
| Country | Link |
|---|---|
| EP (1) | EP3142630A1 (en) |
| CN (1) | CN106456462A (en) |
| AR (1) | AR100467A1 (en) |
| AU (1) | AU2015258611B2 (en) |
| BR (1) | BR112016025826B1 (en) |
| CA (1) | CA2948196C (en) |
| MX (1) | MX363625B (en) |
| WO (2) | WO2015172344A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108135825A (en) * | 2015-11-13 | 2018-06-08 | 宝洁公司 | Dentifrice composition with improved consumer experience |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MX2018005918A (en) | 2015-11-13 | 2018-08-28 | Procter & Gamble | Dentifrice compositions with improved fluoride stability. |
| BR112019000469A2 (en) * | 2016-07-15 | 2019-04-24 | The Procter & Gamble Company | process of preparing oral care compositions |
| WO2023020817A1 (en) * | 2021-08-19 | 2023-02-23 | Unilever Ip Holdings B.V. | Oral care composition comprising iota carrageenan and kappa carrageenan |
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| CN1284854A (en) * | 1997-12-18 | 2001-02-21 | 尤尼利弗公司 | Oral care composition |
| CN1505501A (en) * | 2001-04-24 | 2004-06-16 | 密执安特种矿石公司 | Fluoride compatible calcium carbonate |
| CN102014858A (en) * | 2008-04-28 | 2011-04-13 | 宝洁公司 | Oral care compositions |
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| GB8927073D0 (en) * | 1989-11-30 | 1990-01-31 | Unilever Plc | Oral compositions |
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| US20040120902A1 (en) * | 2001-04-24 | 2004-06-24 | Wernett Patrick Clinton | Fluoride compatible calcium carbonate |
| CA2634758A1 (en) * | 2005-12-20 | 2007-07-05 | The Procter & Gamble Company | Oral care compositions comprising zinc and phytate |
| US20080274062A1 (en) * | 2007-05-02 | 2008-11-06 | Chantal Bergeron | Glycyrrhizic acid compounds as a foamer in chemically-derived surfactant-free dentifrice |
| CN101292943B (en) * | 2008-06-20 | 2010-04-14 | 陕西太和科技股份有限公司 | Nanometer zinc oxide toothpaste |
| CN101690699A (en) * | 2009-09-29 | 2010-04-07 | 广东名臣有限公司 | Teeth-cleaning whitening toothpaste composition |
| EP2753292B1 (en) * | 2011-09-08 | 2018-06-27 | Unilever N.V. | Tooth remineralizing dentifrice |
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- 2015-04-28 CN CN201580024067.1A patent/CN106456462A/en active Pending
- 2015-04-28 WO PCT/CN2015/077634 patent/WO2015172651A1/en active Application Filing
- 2015-04-28 BR BR112016025826-6A patent/BR112016025826B1/en active IP Right Grant
- 2015-04-28 AU AU2015258611A patent/AU2015258611B2/en active Active
- 2015-04-28 CA CA2948196A patent/CA2948196C/en active Active
- 2015-04-28 EP EP15792524.9A patent/EP3142630A1/en not_active Withdrawn
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Also Published As
| Publication number | Publication date |
|---|---|
| EP3142630A1 (en) | 2017-03-22 |
| MX363625B (en) | 2019-03-28 |
| AR100467A1 (en) | 2016-10-05 |
| MX2016015017A (en) | 2017-08-10 |
| AU2015258611B2 (en) | 2018-02-15 |
| WO2015172651A1 (en) | 2015-11-19 |
| AU2015258611A1 (en) | 2016-11-17 |
| CA2948196C (en) | 2019-07-09 |
| BR112016025826B1 (en) | 2020-12-08 |
| CA2948196A1 (en) | 2015-11-19 |
| WO2015172344A1 (en) | 2015-11-19 |
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