CN1168093A - Oral compositions - Google Patents

Oral compositions Download PDF

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Publication number
CN1168093A
CN1168093A CN96191427A CN96191427A CN1168093A CN 1168093 A CN1168093 A CN 1168093A CN 96191427 A CN96191427 A CN 96191427A CN 96191427 A CN96191427 A CN 96191427A CN 1168093 A CN1168093 A CN 1168093A
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China
Prior art keywords
composition
pyrophosphate
agent
sodium
add
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CN96191427A
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Chinese (zh)
Inventor
T·M·拉耶
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Procter and Gamble Co
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Procter and Gamble Co
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Publication of CN1168093A publication Critical patent/CN1168093A/en
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/20Halogens; Compounds thereof
    • A61K8/21Fluorides; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/24Phosphorous; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses

Abstract

The invention discloses a dentifrice composition comprising: a) from about 5 % to about 50 % by weight of sodium bicarbonate; b) a soluble fluoride ion source in an amount sufficient to provide from about 10ppm to about 3500ppm of fluoride ion; c) at least about 1.5 % by weight of tetrasodium pyrophosphate, of which some or all of the tetrasodium pyrophosphate is in the form of undissolved anhydrous tetrasodium pyrophosphate particles; and d) from about 50 % to about 94 % dentifrice carrier materials; and wherein further said composition has a soluble pyrophosphate ion content in the range from about 1 to about 100ppm.

Description

Composition for oral cavity
Technical field
The present invention relates to composition for oral cavity.Specifically, the present invention relates to contain so-called sodium bicarbonate (sodium bicarbonate) Dentrifice composition of pyrophosphate anticalculus agent, it has the stability and the aesthetic property of improvement.
Background of invention
Tartar claims tartar sometimes again, is the deposit that is formed at place, dental surface gingiva crack.Tartar mainly appears at the place near the salivary duct mouth of pipe on the gum; For example descend the tongue side surface of anterior tooth arrangement, the surface of grinding one's teeth in sleep in cheek side surface of grinding one's teeth in sleep in top first and second and rear portion far away.
Tartar after the formation comprises inorganic part, mainly is calcium phosphate, is and bone, enamel and the similar hydroxyapatite lattice structure of enamel.Wherein also have organic moiety, by the epithelial cell that comes off, from cell, saliva liquid precipitate thing, food debris and various microorganism constitute.
Along with the development that forms the back tartar, if need not dye or bleaching by external medicament, it can become conspicuous white and yellow.Very not attractive in appearance.
Regular machinery removal tartar is the conventional method in the dental clinic.Proposed also that many chemistry or biological medicament are used to suppress the formation of tartar or after it forms with its removal.Pyrophosphate is the known chemical agent that suppresses tartar formation effect that has, and for example at the Parran of this incorporated by reference, the United States Patent (USP) 4,999 in the 12 days March in 1991 of Jr. etc. is described in 184.
The Dentrifice composition that contains pyrophosphate and sodium bicarbonate (aka, sodium bicarbonate) also is known, and is existing illustrated in the United States Patent (USP) 5,180,576 in for example on January 19th, 1993 such as Winston of this paper incorporated by reference.But, obtain and contain the stable Dentrifice composition that can effectively suppress sodium bicarbonate that tartar forms and pyrophosphate and have difficulty in the processing.The pyrophosphate that before had been dissolved in these Dentrifice compositions easily crystallizes into the Sodium pyrophosphate decahydrate crystal afterwards again.These crystal can not become to grow up to big glass particles, and are attractive in appearance and have influence on the tartar effect.
Obviously, United States Patent (USP) 5,180,576 have recognized this problem and have illustrated with a kind of manufacture method and avoided, this method uses sodium bicarbonate to salt out alkali metal pyrophosphate salts.Thus, it is said that dissolved pyrophosphate content is lower in the final composition, and the undissolved Sodium pyrophosphate decahydrate that remaining pyrophosphate is salted out by sodium bicarbonate.But with the water diluted composition time, these undissolved pyrophosphate crystal can very fast dissolving as in use.So, the another kind of method that this carries out an invention again just, for example at the Parran of this incorporated by reference, the United States Patent (USP) 4,684 on August 4th, 1987 such as Jr is described in 518.
From PCT application US94/03280, know again, can be by controlled condition in whole mixed process to guarantee being lower than about 20% pyrophosphate dissolving, prepare not only aesthetic approved but also have effectiveness contain pyrophosphate/sodium bicarbonate Dentrifice composition.In fact, the method in the above-mentioned application has still been dissolved the pyrophosphate of total amount about 5%.In order to reduce the crystalline danger of ten hydration pyrophosphates as far as possible, need further to reduce the content of soluble pyrophosphates.
So one of purpose of the present invention provides a kind of easy method of controlling, be used to prepare the stable Dentrifice composition that contains sodium bicarbonate and pyrophosphate.The present invention also aims to the Dentrifice composition that contains sodium bicarbonate and pyrophosphate that provides stable, pyrophosphate granule wherein has predetermined and/or consistent particle size.Another object of the present invention is by the control processing conditions, for example controls the pyrophosphate ion concentration that is dissolved in the compositions and is lower than 100ppm, is more preferably to be lower than 10ppm, prepares such stable compositions.
By following specifying, above-mentioned and other purpose of the present invention will be conspicuous.
All percentages used herein and ratio all by weight, all mensuration are all carried out at 25 ℃, unless otherwise mentioned.
Brief summary of the invention
According to the content of first aspect present invention, a kind of Dentrifice composition is provided, wherein comprise:
A) by weight, about 5% to about 50% sodium bicarbonate;
B) be enough to provide the soluble fluoride ion source of about 10ppm to about 3500ppm fluorion;
C) by weight, at least about 1.5% tetrasodium pyrophosphate, having in these tetrasodium pyrophosphates partly or entirely is undissolved anhydrous tetrasodium pyrophosphate particle form; With
D) about 50% to about 94% dentifrice carrier material;
And then the solubility pyrophosphate ion about 1 that contains in the described compositions is to about 100ppm, and about 1.5 is better to about 10ppm, and about 2 to about 5ppm also will get well.
The invention still further relates to the method for making above-mentioned Dentrifice composition, may further comprise the steps:
A) form the dentifrice carrier material pre-composition that comprises one or more materials, these materials are selected from bonding/thickening agent, wetting agent, buffer agent, polishing material, surfactant, sweeting agent, deodorant tune, titanium dioxide and composition thereof, described pre-composition comprise at least a or multiple binder and are enough to make in herein the step b) pH greater than one or more buffer agents of about 8;
B) in pre-composition, add the water that is enough to the hydration binder, form paste;
C) in the paste that forms, add sodium bicarbonate;
D) be lower than about 30 ℃ then, be lower than about 25 ℃ better, pH disposable or add tetrasodium pyrophosphate in paste when being advisable greater than about pH8 in batches.
Be preferably, all in compositions contain and add tetrasodium pyrophosphate again after sodium salt all adds.And, in embodiment preferably, bonding/thickening agent and buffer agent should add pre-composition in batches, and to form multilamellar binder layer and buffer agent layer at interval in last pre-composition, this is very valuable for obtain best paste rheology in the binding agent hydration step.
The present invention relates to a kind of manufacture method that contains the sodium bicarbonate Dentrifice composition of pyrophosphate anticalculus agent.The Dentrifice composition made from the inventive method can be a toothpaste-like or gelatinous." toothpaste " refers to pasty state or gel preparation at this, unless otherwise mentioned.The invention still further relates to the sodium bicarbonate/pyrophosphate tartar Dentrifice composition that contains anhydrous tetrasodium pyrophosphate.
Method and composition of the present invention comprises several essential components, and optional component.Hereinafter will specify the condition of these components and the inventive method.
A) pyrophosphate
Pyrophosphate used in this method and the compositions must comprise tetrasodium pyrophosphate.This material can be anhydrous salt form or ten hydrated forms, or other in dentifrice composition with the kind of solid form stable existence.This salt is its solid particulate form, can be crystal form or amorphous form, and the granular size of salt preferably is small enough to also in use be easy to dissolving by approval on attractive in appearance.
Though the tetrasodium pyrophosphate salt particle is the necessary composition of the inventive method and compositions, should be realized that, can contain other pyrophosphate of low concentration in the inventive method and the compositions.Concrete salt comprises pyrophosphoric acid four alkali metal salts except that tetrasodium pyrophosphate, pyrophosphoric acid dihydro two alkali metal salts, and pyrophosphoric acid one hydrogen three alkali metal salts and composition thereof, alkali metal wherein is sodium or potassium.(at the Kirk﹠amp of this incorporated by reference; The chemical technology encyclopaedia of Othmer (Encyclopedia of Chemical Technology) second edition, 15 volumes, IntersciencePublishers has more detailed description to pyrophosphate in (1958)).The hydration of these salt and anhydrous form all can use.Because these salt than the easier dissolving of tetrasodium pyrophosphate salt, must limit their existence in the inventive method and compositions, to contain the pyrophosphate ion of solubility in the compositions of avoiding preparing, had better not include these more diffluent salt.
The content of pyrophosphate is any tartar effective dose in these compositionss, and generally being enough to provides, and by weight, at least about 1.0%, about 1.5% to about 10% is good, is more preferably about 3.0% to about 6% P 2O 7 -4Should be appreciated that P 2O 7 -4Concentration is can be to the amount (i.e. theoretical amount under suitable pH) that compositions provides, and after final products pH forms, may have other pyrophosphate form (HP for example 2O 7 -3).So the tetrasodium pyrophosphate concentration of using in the inventive method and the compositions by Dentrifice composition weight, is advisable with about 1.5% to about 15%, about 2% to about 10% is better.
B) sodium bicarbonate
Sodium bicarbonate claims sodium bicarbonate again, is a kind of multiduty household products, comprises being used for dentifrice and collutory.It is a kind of white powder agent, and if water soluble not stabilized, is easy to discharge carbon dioxide in aqueous systems.The present composition contains, and by Dentrifice composition weight, about 5% to about 50% sodium bicarbonate, and about 10% to about 30% is better.
C) soluble fluoride ion source
Also contain soluble fluoride ion source in the present composition.The consumption of soluble fluoride ion source is enough to provide the fluorion of about 10ppm to about 3500ppm.Fluoride is a sodium fluoride preferably, stannous fluoride, indium and sodium monofluorophosphate.Above salt and other are disclosed in United States Patent (USP) 3,678,154 on July 18th, 1972 such as the United States Patent (USP) 2,946,1735 in July 26 nineteen sixty such as Norris and Widder.Last two patents are all in this incorporated by reference.
D) dentifrice carrier material
In the preparation process of dentifrice composition of the present invention, need in compositions, add one or more dentifrice carrier materials." dentifrice carrier material " refer in this article, and be any concerning being used in according to safety and effective substances in the dentifrice composition of the present invention's preparation.This class material is well-known in the art, and those skilled in the art can make one's options easily according to its physical characteristic that is required of Dentrifice composition and the appearance characteristics of preparation.The dentifrice carrier material account for usually present composition weight with 50% to about 94%, about 69% to about 80% better.
The present invention contains binder usually so that ideal denseness to be provided.Binder is a CVP Carbopol ETD2050 preferably, carrageenin, water-soluble cellulose ether salt such as carboxyethyl cellulose and sodium carboxymethyl cellulose and carboxymethyl hydroxyethyl cellulose sodium.Also can use natural gum, karaya for example, zanthan, Radix Acaciae senegalis and Tragacanth.Colloid aluminosilicate magnesium or fine silica also can be used as the thickening agent of part with the further organizational structure of improving.Can use by about 0.2% to 5.0% the thickening agent of the total restatement of compositions.
In order to prevent that compositions from hardening because of being exposed in the air, should comprise certain wetting agent in the toothpaste.Some wetting agent can also provide ideal sweet taste or fragrance for dentifrice composition.Suitable wetting agent comprises glycerol, sorbitol, and other edible polyhydric alcohol, and composition thereof, its content is about 15% to about 70% of composition weight.
Can also be added with titanium dioxide in the present composition.Titanium dioxide is white powder, for compositions provides pigment.Titanium dioxide accounts for about 0.25% to about 1% of composition weight usually.
Also contain water in the compositions of this method.The water that is used to prepare commodity toothpaste preferably should be deionized water and not have organic impurities.It is good that water accounts for about 12% to 45%, about 15% to about 35% of composition weight usually, and about 20% to about 30% is better.Comprise the free water of adding and the water of bringing into by other material of sorbitol and so in these water contents.
The pH of the present composition regulates by buffer agent.Buffer agent refers to the pH of compositions to be brought up to the reagent more than about pH8 in this article, and such pH adds sodium bicarbonate and tetrasodium pyrophosphate to suit.This class reagent comprises tertiary sodium phosphate, sodium hydroxide and sodium carbonate.The concentration of sodium carbonate is about 0.5% to about 2% of composition weight.
Can also contain the polishing material in the compositions.The polishing material that is considered for the present composition can be any can the adamantine material of excessive wear.Comprising example gel or precipitated silica; calcium carbonate, the former dicalcium phosphate of two hydrations, calcium pyrophosphate; tricalcium phosphate; poly-calcium metaphosphate, insoluble sodium hexametaphosphate, hydrated alumina and resin abrasivus; the granulating condensation product of carbamide and formaldehyde for example; and for example at other material described in 25 days the United States Patent (USP) of in Decembers, 1962 such as Cooley 3,070,510 of this reference.Also can use the mixture of abrasivus.
Preferably various types of silica dental section abrasivus, because their unique benefit is to have and special clean the teeth and polish performance, and enamel and enamel that can the excessive wear tooth.Silicon dioxide buffing compound and other buffing compound as used herein, its granular size are usually between about 0.1 to 30 micron, and be better between 5 to 15 microns.Abrasive silicas can be precipitated silica or silica dioxide gel, the United States Patent (USP) 3 on March 2nd, 1970 such as Pader for example, 538,230 and the United States Patent (USP) 3 in DiGiulio1975 June 21,862,307 described silica xerogels, above patent are incorporated by reference in this article all.Be preferably W.R.Grace﹠amp; Company, the silica xerogel of the trade mark of Davison Chemical Division " Syloid " by name.Precipitated silica comprises " Zeodent " of J.M.Huber Corporation preferably, and particularly name is called the silicon dioxide of " Zeodentl19 ".These abrasive silicas have illustrated at United States Patent (USP) 4,340 in 583 (July 29 nineteen eighty-two).
The content of abrasivus, by weight, about 6% to 70% to be good, about 15% to about 25% is better.
Dentifrice composition can also contain surfactant.Suitable is more stable, and can be in the pH of broad scope blistered surfactant, comprise non-soap anionic, nonionic, cationic, amphoteric ion type and both sexes synthetic organic detergent.The suitable reagent of many these classes is disclosed in 27 days the United States Patent (USP) of in JIUYUE, 1977 such as Gieske 4,051,234 of this reference.Preferably use at this and to be about alkyl sodium sulfate and the Polyethylene Glycol of composition weight 4% to about 3% respectively.
Can also in the present composition, add deodorant tune.Suitable deodorant tune comprises wintergreen oil, Oleum menthae, Oleum Menthae Rotundifoliae, Sassafras oil and Herba Origani oil.Operable sweeting agent comprises aspartame, acesulfame (acesulfame), glucide, glucose, fructose and cyclamate sodium.The deodorant tune and the sweeting agent that are used in the toothpaste are generally about 0.005% to about 2% of composition weight.
The present composition can also contain optional medicament (for example triclosan (triclosan)) and other anticalculus agent.Optionally anticalculus agent comprise known synthetic anionic polymer (copolymer (for example Gantrez) that comprises polyacrylate and maleic anhydride or maleic acid and ethylene methacrylic ether, of United States Patent (USP) 4,627,977 at the Gaffar of this incorporated by reference etc.; And for example poly-aminopropanesulfonic acid (AMPS)), Quadrafos (tripolyphosphate for example; Hexametaphosphate), diphosphate (EHDP for example; AHP), polypeptide (for example poly-aspartate and polyglutamic acid) and composition thereof.
Dentifrice composition is prepared from by according to manufacture method above-mentioned component being mixed.This method may further comprise the steps:
A) form the dentifrice carrier material pre-composition that comprises one or more materials, these materials are selected from bonding/thickening agent, wetting agent, buffer agent, polishing material, surfactant, sweeting agent, deodorant tune, titanium dioxide and composition thereof, described pre-composition comprise at least a or multiple binder and are enough to make in herein the step b) pH greater than one or more buffer agents of about 8;
B) in pre-composition, add the water that is enough to the hydration binder, form paste;
C) in the paste that forms, add sodium bicarbonate;
D) be lower than about 30 ℃ then, be lower than about 25 ℃ better, pH disposable or add tetrasodium pyrophosphate in paste when being advisable greater than pH8 in batches.
Be preferably, concerning method and composition of the present invention, be dissolved in the pyrophosphate amount in the mixture, press pyrophosphate ion and measure, about 1 to 100ppm, about 1.5 is better to about 10ppm, and about 2 is better to about 5ppm.The method that a kind of mensuration is dissolved in the pyrophosphate amount in mixture and the compositions will describe among the embodiment hereinafter and give an example.
Following examples further describe and have illustrated embodiment within the scope of the present invention.
Embodiment
Following paste and gel dentifrice have the pyrophosphate ion of content about 3.3%. composition paste gel sodium acid carbonate 20.000 20.000 water 19.773 19.773 silica 1s 5.000 15.000 glycerine 15.000 15.000 sorbierites (70%) 14.061 14.111 tetrasodium pyrophosphate 5.045 5.045 sodium alkyl sulfates (28%) 4.000 4.000PEG-6 3.000 3.000 sodium carbonate 1.250 1.250 deodorant tunes 1.000 1.000 carboxymethyl celluloses 0.800 0.800 saccharin sodium 0.400 0.400 titanium dioxide 0.350 0.000 sodium fluoride 0.321 0.321FD ﹠ amp; Blue No. 1 (the Blue No.1) 0.000 0.300 of C
Be prepared as follows paste composition.At ambient temperature at wetting agent (sorbitol; glycerol; PEG-6) granulated mixture that adds saccharin sodium, sodium fluoride, sodium carbonate, sodium carboxymethyl cellulose and titanium dioxide in; sodium carbonate and sodium carboxymethyl cellulose (CMC) are divided into two batches of addings separately; order is a sodium carbonate, CMC, sodium carbonate; CMC forms so-called " stratiform " granulate mixture thus.The water that adds capacity in this liquid pre-composition adds silicon dioxide then with the hydration binding agent then.In this mixture, add sodium bicarbonate, add the tetrasodium pyrophosphate of solid form then.Add deodorant tune and sodium alkyl sulfate solution, make last paste product.
The following mensuration of finishing soluble pyrophosphates concentration in the compositions.
Take by weighing 3.00 ± 0.001g toothpaste, put into 50ml polypropylene centrifuge tube; Add deionized water (9.0ml) and six beades then.Adding a cover the back mixed accurate 2 minutes on vortex stirring instrument.Inclusions is transferred in the centrifuge tube of a 25ml, add a cover the back 10 ℃ with 15, centrifugal 15 minutes of 000rpm.Draw the 1.0ml supernatant and add in the 100ml volumetric flask, be diluted to scale, fully mix with deionized water.Get this solution of 10ml, with deionized water dilution and fully mixing.Utilize ion exchange chromatography analysis.

Claims (9)

1. Dentrifice composition wherein comprises:
A) by weight, about 5% to 50% sodium bicarbonate;
B) be enough to provide the soluble fluoride ion source of about 10ppm to about 3500ppm fluorion;
C) by weight, the tetrasodium pyrophosphate at least about 1.5% wherein partly or entirely is undissolved anhydrous tetrasodium pyrophosphate particle form; With
D) about 50% to about 94% dentifrice carrier material;
Wherein, so described compositions have about 1ppm to the solubility pyrophosphate ion content of about 100ppm.
2. according to the described Dentrifice composition of claim 1, dentifrice carrier material wherein comprises one or more and is selected from bonding/thickening agent, wetting agent, water, buffer agent, polishing material, surfactant, sweeting agent, deodorant tune, the material of titanium dioxide and composition thereof.
3. Dentrifice composition according to claim 2, buffer agent wherein is selected from tertiary sodium phosphate, sodium hydroxide, sodium carbonate and composition thereof.
4. according to each described Dentrifice composition in the claim 1 to 3, wherein said compositions contains 1.5% to about 15% the tetrasodium pyrophosphate of having an appointment.
5. according to each described Dentrifice composition in the claim 1 to 4, wherein said compositions has about 1.5 to 10ppm solubility pyrophosphate ion content.
6. make the method according to each described Dentrifice composition in the claim 1 to 5, it may further comprise the steps:
A) form the dentifrice carrier material pre-composition that comprises one or more materials, these materials are selected from bonding/thickening agent, wetting agent, buffer agent, polishing material, surfactant, sweeting agent, deodorant tune, titanium dioxide and composition thereof, described pre-composition comprise at least a or multiple binder and are enough to make in herein the step b) pH greater than one or more buffer agents of about 8;
B) in pre-composition, add the water that is enough to the hydration binder, form paste;
C) in the paste that forms, add sodium bicarbonate;
D) be lower than about 30 ℃ then, be lower than about 25 ℃ better, pH disposable or add tetrasodium pyrophosphate in paste when being advisable greater than about pH8 in batches.
7. after containing the sodium component and all add, in compositions other of method according to claim 6, tetrasodium pyrophosphate wherein add again.
8. according to claim 6 or 7 described methods, buffer agent wherein comprises sodium carbonate.
9. according to each described method in the claim 6 to 8, binder wherein and buffer agent are added in the pre-composition in batches, to form multi-layer intercrossed binder layer and buffer agent layer in last pre-composition.
CN96191427A 1995-01-14 1996-01-05 Oral compositions Pending CN1168093A (en)

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CN104114142A (en) * 2011-12-01 2014-10-22 3M创新有限公司 One component self-adhesive dental composition, process of production and use thereof
CN108348409A (en) * 2015-11-13 2018-07-31 宝洁公司 Dentifrice composition with improved fluoride stability

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Publication number Priority date Publication date Assignee Title
CN104114142A (en) * 2011-12-01 2014-10-22 3M创新有限公司 One component self-adhesive dental composition, process of production and use thereof
CN108348409A (en) * 2015-11-13 2018-07-31 宝洁公司 Dentifrice composition with improved fluoride stability

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PE64496A1 (en) 1997-03-19
HUP9801282A2 (en) 1999-01-28
EP0794762A1 (en) 1997-09-17
GB9500746D0 (en) 1995-03-08

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