CN109152707A

CN109152707A - oral care composition comprising tricalcium silicate

Info

Publication number: CN109152707A
Application number: CN201780030939.4A
Authority: CN
Inventors: 李小科; 刘炜宁; 王进防; H·邢
Original assignee: Unilever NV
Current assignee: Unilever NV
Priority date: 2016-05-19
Filing date: 2017-04-13
Publication date: 2019-01-04
Also published as: WO2017198399A1; BR112018072432A2

Abstract

A kind of oral care composition is disclosed, it includes tricalcium silicate, soluble calcium source, phosphate source and physiologically acceptable carriers, wherein the tricalcium silicate and the soluble calcium source exist with the weight ratio of 1:3 to 20:1.

Description

Oral care composition comprising tricalcium silicate

Technical field

The present invention relates to oral care compositions, such as toothpaste, powder, chewing gum (gum), collutory.Particularly, this hair The bright oral care composition being related to comprising tricalcium silicate and soluble calcium source causes the sensibility of tooth to reduce and/or again Mineralising.It is used to treat the allergy of individual tooth the invention further relates to such composition and/or makes the remineralization of teeth of individual Purposes.

Background technique

Dental hypersensitivity is the temporary inductivity pain sensation for influencing to be up to 20% Adult group.Allergy tooth can to temperature, Pressure or chemical action are sensitive.

The dentine of tooth usually contains the channel of referred to as tubule, the channel provide tooth inside dental pulp region and Osmotic flow between external root surface.Dental hypersensitivity may be related with the generally increase of exposed root surface, exposure Root surface is the load cycling fatigue due to periodontal disease, brush wear or the nanoid enamel close to dentine enamel joint portion It is caused.When root surface exposure, dentinal tubule can also expose.

The current acceptable theory of dental hypersensitivity is fluid dynamic theory, the dentine based on open exposure Tubule permission fluid flows through the theory of tubule.The flowing excites the nerve endings in dental pulp.In SEM (scanning electron microscope) The opening of the clinical duplicate announcement different number for the sensitive teeth observed or partially enclosed dentinal tubule.

Treating dental hypersensitivity has different approach.One approach be by using comprising strontium ion, sylvite such as potassium nitrate, " the nerve depolarization agent " of saleratus, potassium chloride etc. come reduce in sensitive teeth nerve excitability.These nerves are gone Polarization agent is worked by the nerve transduction of interference pain stimulation, keeps nerve less sensitive.

Another approach is using complete or partial closing tubule " tubule sealer ", such as polystyrene bead, phosphorus ash Stone, polyacrylic acid, mineral hectorite clay etc..The exposure end that these tubule sealers pass through physical containment dentinal tubule It holds, to reduce dentine fluid motion and reduce stimulation relevant to shear stress described in fluid dynamic theory to rise Effect.

Still it continues to need and treats dental hypersensitivity with more effective approach.The present inventor is it has now unexpectedly been found that packet Oral care composition containing tricalcium silicate, soluble calcium source and phosphate source provides excellent small duct occlusion effect to reduce Tooth sensitivity.In addition, having further been discovered that such oral care composition also shows excellent remineralization of teeth effect.

Additional information

2008/068149 A of WO (Unilever) discloses a kind of oral care product comprising first chamber, institute Stating first chamber includes the insoluble calcium phosphate for not being synthos；The second separate composition comprising phosphate ion sources；With And the tool for every kind of composition to be delivered to dental surface.Preferred insoluble calcium phosphate is calcium silicates.

Above-mentioned additional information does not describe the oral care combination comprising tricalcium silicate, soluble calcium source and phosphate source Object.Particularly, the oral care composition can treat dental hypersensitivity and/or enhancing remineralization of teeth effect.

Test and definition

Dentifrice

For the purposes of the present invention, " dentifrice " means the paste of the cream for cleaning tooth or other surfaces in oral cavity, powder End, liquid, glue or other formulations.

Toothpaste

For the purposes of the present invention, " toothpaste " means the cream being used together with toothbrush paste or gel dentifrice.Particularly preferably Suitable for the toothpaste for cleaning tooth by scrubbing about two minutes.

Partial size

For the purposes of the present invention, " partial size " means D50 partial size.The D50 partial size of microparticle material is of wherein 50wt% Grain is relatively large in diameter and the lesser particle size diameter of the particle diameter of 50wt%.For the purposes of the present invention, using Malvern Mastersizer 2000 and Malvern ZetaSizer Nano series measure partial size and distribution.

Deposition aid

For the purposes of the present invention, " deposition aid " means to facilitate during the composition use by active matter such as silicon Sour tricalcium and/or other beneficial agents deposit the material to dental surface from the continuous phase of the composition.As used herein Beneficial agent means usually to be delivered to people's tooth and/or oral cavity including gum to enhance or improve the work of those dental tissue features Property object.

pH

PH is using value at a temperature of atmospheric pressure and 25 DEG C.When referring to the pH of oral care composition, it means that As the 5 part composition by weight pH that evenly dispersed and/or while being dissolved in 20 parts by weight of purified water measures at 25 DEG C.Particularly, pH It can be by being surveyed with indicator or pH meter test pH immediately after by 5g oral care composition and 20mL water hand mix 30s Amount.

Dissolubility

For the purposes of the present invention, " solvable " and " insoluble " means source (for example, such as calcium salt) under 25 DEG C and atmospheric pressure Dissolubility in water." solvable " means that source is dissolved in water to obtain the solution that concentration is at least 0.1 mol/L." insoluble " Meaning that source is dissolved in water to obtain concentration is the solution less than 0.001 mol/L.Therefore, " slightly soluble " is defined as meaning that source is molten Solution is in water to obtain concentration greater than 0.001 mol/L and less than the solution of 0.1 mol/L.

Substantially free of

For the purposes of the present invention, substantially free means the total weight based on oral care composition, comprising being less than 1.5 weight %, preferably smaller than 1.0 weight %, more preferably less than 0.75 weight %, still more preferably less than 0.5 weight %, even more Preferably smaller than 0.1 weight %, most preferably 0.0-0.01 weight %, and including all ranges included in it.

Two-phase

For the purposes of the present invention, " two-phase " means the composition with physically separated two independent phases.

Anhydrous composition

For the purposes of the present invention, " anhydrous composition " means that the water content of the composition is combined with the oral care The total weight of object is less than 1.5%, preferably 0.0% to 0.75%.

Viscosity

The viscosity of toothpaste is obtained under room temperature (25 DEG C) with No. 4 rotors of Brookfield viscometer and with the speed of 5rpm Value.Unless otherwise stated, value is with centipoise (cP=mPa.s) use.

Remineralization

For the purposes of the present invention, " remineralization " means on tooth that (that is, in the oral cavity) in situ generates calcium phosphate (including tooth 10 nanometers to 20 microns on tooth, preferably 75 nanometers to 10 microns and most preferably 150 nanometers to 5 microns thick layers, including wherein institute All ranges for including), a possibility that reducing tooth sensitivity, saprodontia, to make enamel by generating this new calcium phosphate Regeneration and/or the appearance for improving tooth by brightening.

It is miscellaneous

In addition in embodiment or it is otherwise explicitly indicated in the case where other than, the amount or anti-of material is indicated in this specification All numbers of condition, the physical property of material and/or purposes are answered optionally to be understood to be modified by word " about ".

Unless otherwise stated, all amounts are in terms of the weight of final oral care composition.

It should be noted that any specific upper limit value can be with any specific lower limit in any range of specified numerical value Value is associated.

To avoid doubt, word " comprising " is intended to mean "comprising", but be not necessarily " by ... form " or " by ... structure At ".In other words, listed step or option need not be exhaustive.

The disclosure of invention found herein, which should be considered covering multiple be subordinated in mutual claim, to be sent out Existing all embodiments, without consider no multiple subordinate or in case of redundancy it may be found that claim thing It is real.

When disclosing a feature about a specific aspect (such as composition of the invention) of the invention, in the disclosure Appearance is recognized as is suitable for the invention any other aspect (such as method of the invention) in the case of suitably modified.

Summary of the invention

In a first aspect, the present invention relates to a kind of oral care composition, it includes:

A) tricalcium silicate；

B) soluble calcium source；

C) phosphate source；With

D) physiologically acceptable carrier；

Wherein the tricalcium silicate and the soluble calcium source exist with the weight ratio of 1:3 to 20:1.

In second aspect, the present invention relates to a kind of oral care products of packaging, and it includes the first aspect of the present invention Oral care composition.

In the third aspect, the present invention relates to the sensibility for reducing individual tooth and/or make individual remineralization of teeth Method comprising the oral care composition of any embodiment of first aspect is applied to the tooth of the individual at least The step of one surface.

After considering the following detailed description and embodiment, all other aspect of the invention will be easy to become brighter It is aobvious.

Specific embodiment

It has been found that the oral care composition comprising tricalcium silicate, soluble calcium source and phosphate source can be effectively close The dentinal tubule for sealing exposure, provides excellent small duct occlusion effect, to reduce tooth sensitivity.

In addition, it has been found that such oral care composition can also show excellent remineralization of teeth effect.

Tricalcium silicate

Tricalcium silicate (Ca₃SiO₅) also write as 3CaOSiO sometimes₂, it is the main component of Portland cement.Silicic acid three Calcium due in its higher calcium content and lattice there are oxide ion rather than often with there is reactivity.It can be reacted with water to produce Raw afwillite (CSH) and calcium hydroxide.It is reacted according to following reaction with water:

2Ca₃SiO₅+6H₂O→3CaO·2SiO₂·3H₂O+3Ca(OH)₂

In preferred embodiments, the tricalcium silicate suitable for the present invention is from Kunshan Huaqiao New Materials Co., Ltd is obtained.

Tricalcium silicate can be crystalline or mesoporosity.Tricalcium silicate is preferably microgranular, because this allows and tooth Organize the maximum surface area of contact.It is preferred that the composition includes the particle containing tricalcium silicate.It is preferred that 10-100 weight Measure the particle tool comprising tricalcium silicate of %, especially 25-100 weight %, most especially 70-100 weight % being used in the present invention Have 100 nanometers to less than 50 microns, preferably 500 nanometers to 30 microns, it is 700 nanometers to 20 microns more preferable, most preferably 1 micron extremely 15 microns of partial size.

Other than calcium oxide, silica, the particle comprising tricalcium silicate also may include other components such as metal sun from Son, anion (such as phosphate radical).It is preferable, however, that the particle includes calcium oxide, silica, in an amount of from the particle weight At least 70%, more preferably at least 80%, still more preferably at least 90% and even more desirably at least the 95% of meter.Most preferably, Particle is made of (or at least substantially by) calcium oxide, silica.

In general, oral care composition of the invention includes 1-80 weight %, more preferable 3-50 weight %, most preferably 5-30 The tricalcium silicate of weight %, the total weight based on oral care composition, and including all ranges included in it.

Soluble calcium source

Soluble calcium source suitable for the present invention is only limitted to the range that the calcium source can be used in mouth.

The illustrative but unrestricted example for the solubility calcium Source Type that can be used in the present invention include such as calcium chloride, Calcium nitrate, calcium acetate, calcium lactate, calcium gluconate, calcium formate, calcium malate, calcium propionate, calcium butyrate, calcium bicarbonate, glycerol phosphorus Sour calcium, Calcium Ascorbate, its mixture etc..In preferred embodiments, calcium source is or mixtures thereof calcium chloride, calcium nitrate.

In general, oral care composition of the invention includes 0.1-20 weight %, more preferable 1-15 weight %, most preferably 2- The soluble calcium source of 10 weight %, the total weight based on oral care composition, and including all ranges included in it.

It is 1:5-20:1, more preferable 1:3-20:1, still more preferably 1:3-10 that oral care composition, which preferably comprises weight ratio: 1, the most preferably tricalcium silicate of 1:1.5-5:1 and soluble calcium source.

Phosphate source

The phosphate source that can be used in the present invention is only limitted to the model that the phosphate source can be used for suitable for the composition of mouth It encloses.The illustrative example of phosphate source type suitable for the present invention includes tertiary sodium phosphate, sodium dihydrogen phosphate, phosphoric acid hydrogen two Sodium, ammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, tripotassium phosphate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate, its mixture etc..Phosphorus The preferably water-soluble source in hydrochlorate source.

When in use, phosphate source usually accounts for 0.5-40 weight %, the more preferable 1-30 weight % of oral care composition, Most preferably 2-20 weight %, the total weight based on oral care composition, and including all ranges included in it.Preferred Embodiment in, phosphate source used is tertiary sodium phosphate and sodium dihydrogen phosphate, the weight of tertiary sodium phosphate and sodium dihydrogen phosphate Than for 1:4 to 4:1, preferably 1:3 to 3:1 and most preferably 1:2 to 2:1, including all ratios included in it.Another preferred Embodiment in, phosphate source used be or include at least sodium dihydrogen phosphate.

Optional components

It was found that oral care composition of the invention is in closing dentinal tubule to reduce tooth sensitivity and in enamel table It is effective in terms of the hydroxyapatite layer that induced synthesis is new on face.It is not intended to be limited to theory, it is believed that soluble The presence of calcium source increases the calcium ion concentration in oral cavity composition, and which enhance formed between calcium salt and phosphate source in oral cavity The reaction of calcium phosphate.Calcium phosphate precipitation can help deposition of the tricalcium silicate particle on dentine and/or enamel surfaces.Silicic acid three Calcium further can sustainably discharge calcium ion, to react with the phosphate source in saliva and/or the Si-OH base of tricalcium silicate Group can have affinity to the calcium ion in tooth, and which further enhances small duct occlusion effect and/or the remineralization function of tooth Effect.

Oral care composition of the invention can further include deposition aid.Deposition aid suitable for the present invention is only It is limited to the range that the deposition aid can be used in mouth.In preferred embodiments, deposition aid provides a large amount of calcium in mouth Ion and cheap and enrich.In especially preferred embodiment, deposition aid is in addition to including solubility in the composition Calcium salt other than calcium source.

The illustrative but non-limiting example for the deposition aid type that can be used in the present invention includes such as half hydrated sulfuric acid Or mixtures thereof calcium, calcium dihydrogen phosphate, calcium aluminate, calcium monohydrogen phosphate etc..In preferred embodiments, deposition aid is di(2-ethylhexyl)phosphate Or mixtures thereof hydrogen calcium, calcium sulfate hemihydrate.

It has been found that in the present invention the material as deposition aid be it is biocompatible, experience with the fast reaction of water simultaneously It is reabsorbed completely on dental surface, therefore it can be used for promoting oral care actives such as tricalcium silicate and/or other beneficial Agent is deposited to dental surface.

In general, oral care composition of the invention include 0.1-20 weight %, it is more preferable 0.2-15 weight %, still more excellent Select the deposition aid of 0.5-10 weight %, most preferably 1-5 weight %, the total weight based on oral care composition, and including All ranges included in it.

It is 20:1-1:5, more preferable 15:1-1:3, most preferably 10:1-1:1 that oral care composition, which preferably comprises weight ratio, Tricalcium silicate and deposition aid.

Composition of the invention is oral care composition, and generally comprises physiologically acceptable carrier.The load Body preferably at least includes surfactant, thickener, wetting agent or combinations thereof.

Preferably, oral care composition includes surfactant.Preferably, the composition includes with the composition Poidometer at least 0.01%, more preferably at least 0.1% and most preferably 0.5% to 7% surfactant.Suitable surface is living Property agent includes anionic surfactant, such as C₈To C₁₈Alkyl sulfate (such as NaLS), C₈To C₁₈Alkyl sulphur Base succinate (such as sodium sulfosuccinate dioctyl ester), C₈To C₁₈Alkyl sulfoacetate (such as lauryl sulfoacetate sodium), C₈To C₁₈Alkyl sarcosine salt (such as sodium lauryl sarcosinate), C₈To C₁₈(it can be optionally comprising up to 10 for alkylphosphonic Ethylene oxide and/or propylene oxide unit) and sulfated monoglycerides sodium salt, magnesium salts, ammonium salt or ethanolamine salt.It is other suitable The surfactant of conjunction includes nonionic surface active agent, the Polyethoxylated fatty acids sorbitan being such as optionally present Ester, ethoxylated fatty acid, the ester of polyethylene glycol, fatty mono glyceride and fatty acid diglyceride ethoxylate, with And ethylene oxide/propylene oxide block polymer.Other suitable surfactant includes amphoteric surfactant, such as glycine betaine Or sulfobetaines.The mixture of any of above material also can be used.It is highly preferred that surfactant includes either anion Type surfactant.Preferred anionic surfactant is NaLS and/or neopelex.It is optimal Selection of land, the surfactant are NaLS.

Thickener can also be used for the present invention, and be only limitted to that the thickener can be added in the composition suitable for mouth Range.The illustrative example for the thickener types that can be used in the present invention includes sodium carboxymethylcellulose (SCMC), ethoxy Cellulose, methylcellulose, ethyl cellulose, bassora gum, Arabic gum, Karaya Gum, sodium alginate, carrageenan, Guar Glue, xanthan gum, Irish moss, starch, modified starch, the thickener based on silica, including aerosil, silicic acid Magnalium (such as Veegum), carbomer Carbomer (acrylate of crosslinking) and its mixture.

Generally, it is preferred to xanthan gum and/or sodium carboxymethylcellulose and/or carbomer.When using carbomer, it is desired to have At least 700, those of 000 weight average molecular weight, and it is expected preferably have at least 1, those of 200,000 molecular weight, most It is preferred that at least about 2,500,000 those of molecular weight.The mixture of carbomer also can be used herein.

In especially preferred embodiment, carbomer is or mixtures thereof Synthalen PNC, Synthalen KP. Its polyacrylic acid for being described as high molecular weight and crosslinking, and with CAS 9063-87-0 mark.The material of these types can be from Supplier such as Sigma is commercially available.

In another especially preferred embodiment, sodium carboxymethylcellulose used (SCMC) is SCMC 9H.Its by It is described as with the sodium salt with the cellulose derivative of the carboxymethyl of the hydroxy combining of glucopyranose backbone monomers, and with CAS 9004-32-4 mark.It can be obtained from supplier such as Alfa Chem.

In another especially preferred embodiment, the thickener is xanthan gum.

Thickener usually accounts for 0.01- about 10 weight %, the more preferable 0.1-9 weight % of the composition, and most preferably 1.5-8 weight %, the total weight based on oral care composition, and including all ranges included in it.

When oral care composition of the invention is toothpaste or gel, usually there is about 30,000 to 180,000 li The viscosity of pool and preferably 60,000 to 170,000 centipoises and most preferably 65,000 to 165,000 centipoises.

Suitable wetting agent is preferred in oral care composition of the invention, and they include such as glycerol, mountain Pears sugar alcohol, propylene glycol, dipropylene glycol, two glycerol, glyceryl triacetate, mineral oil, polyethylene glycol (preferably PEG-400), alkane two Or mixtures thereof alcohol (such as butanediol and hexylene glycol), ethyl alcohol, pentanediol.Or mixtures thereof glycerol, polyethylene glycol, D-sorbite are Preferred wetting agent.

Wetting agent can the 10-90% based on the weight of oral care composition range exist.It is highly preferred that carrier is wet Agent accounts for the 25-80 weight % of the composition, and most preferably 45-70 weight %, based on the total weight of the composition, and including All ranges included in it.

Oral care composition of the invention containing this field be commonly used for enhancing physical property and performance it is various its Its ingredient.These ingredients include antimicrobial, anti-inflammatory agent, anti-caries agent, plaque buffers, fluoride source, vitamin, plant Extract, desensitizer, antilithic, biomolecule, flavoring agent, protein material, preservative, opacifier, colorant, pH are adjusted Agent, sweetener, particle abrasion material, polymerizable compound, buffer and salt are with the pH and ionic strength of buffer compositions, Yi Jiqi Mixture.Such components typically and collectively account for the composition less than 20 weight %, and preferably 0.0-15 weight %, and most It is preferred that the 0.01-12 weight % of the composition, including all ranges included in it.

Oral care composition of the invention can be used for reducing the sensibility of individual tooth and/or make individual remineralization of teeth Method in, at least one surface including the composition to be applied to individual tooth.Oral care composition of the invention Drug can be additionally or alternatively used as and/or in the manufacture of drug, to provide oral care benefit as described herein Place, such as sensibility for reducing individual tooth.Or and preferably, the purposes is non-therapeutic.

Preferably, oral care composition is substantially free of water, to prevent the premature reaction between calcium salt and phosphate source.

In preferred embodiments, oral care composition is single-phase anhydrous composition.

In another preferred embodiment, oral care composition is the two-phase combination comprising calcium phase and phosphate phase Object, wherein the tricalcium silicate and soluble calcium source are present in the calcium phase, and the phosphate source is present in phosphate Xiang Zhong.The two in independent phase mutually by being physically separated from each other.Two independences are mutually delivered to tooth can be with Be at the same or sequentially.In preferred embodiments, the phase is delivered simultaneously.

In general, dual phase composition by allow to be coextruded two-phase it is two-tube and be delivered, this is two-tube to have for calcium phase First compartment and second compartment for phosphate phase.

In preferred embodiments, one in such two-tube compartment surrounds another.In such embodiment, One phase exists as the sheath (sheath) of another phase in core.In especially preferred embodiment, core is Calcium phase, sheath are phosphate phases.

In another preferred embodiment, such two-tube with the two side-by-side compartment in same pipe.In such reality It applies in scheme, it is one that two phases are extruded from pipe, and such squeeze out is referred to as " contact squeezes out ".Pump head can be used for such double Guan Zhong, for two phases to be extruded as one from the pipe.

Dual-phase oral care composition can be the gel combination comprising two independent gel phases, and first phase is calcium Phase, second phase are phosphate phase.In the swab stick or pallet for applying calcium phase and phosphate phase above, then means of delivery can be related to The pallet and teeth contact are placed.

Usual composition can be packaged.In toothpaste or gel form, composition can be packaged in common plastics pressurized layer, metal In pipe or single compartment distributor.Sensitizing range can be applied directly to by any physical means such as toothbrush, finger tip or by applicator And the composition is applied to dental surface.

Even if the composition can also be effective when in for personal common oral hygiene routine.For example, can be by group Object is closed to brush on the tooth of individual.Composition can for example with 1 second to the 20 hours period of teeth contact.It is more preferable 1 second to 10 small When, still more preferably 10 seconds to 1 hour, and most preferably 30 seconds to 5 minutes.Composition can use daily, such as the every angel of individual With once, twice or thrice.When oral care composition is dual phase composition, the two-phase of composition quilt during application Mixing.Mixed phase usually continues 3 minutes to 10 hours on tooth, and more preferable 3 minutes to 8 hours.It can be applied daily.

Following embodiment is provided to promote the understanding of the present invention.There is provided the embodiment be not intended to limitation right want The range asked.

Embodiment

Embodiment 1

The present embodiment is confirmed by using the soluble calcium source combined with tricalcium silicate to the improved envelope of dentinal tubule It closes.All the components are indicated with the weight percent of total formulation, and are expressed as the content of active constituent.

Table 1

A. tricalcium silicate (the Ca from Kunshan Huaqiao New Materials Co., Ltd₃SiO₅)。

Method

Sample preparation

In order to evaluate closing effect to dentinal tubule, by test sample and water with ratio of the 1g to 2mL water mix with Slurries are made.Use only comprising tricalcium silicate sample 1 as compare.

37% phosphoric acid of people's dentine disk (dentine disk) is corroded into 1min, then by them according to identical side Case is handled by scrubbing with different slurries.8 people's dentine disks are divided into 4 groups (n=2).In the Tooth-brushing device for being equipped with toothbrush Lower slurries brush Xian dentine disk.The load brushed teeth is 170g+/- 5g, and operates automatic brush with the speed of 150rpm It washes.After scrubbing 1min, dentine disk is impregnated into 1min in toothpaste slurries.Then use distilled water flushing dentine disk, and It is placed in Mouthsimulator liquid (SOF) under the conditions of 37 DEG C and 60.0rpm of shaking bath.Impregnate about 3 to 4 hours after, using with Identical program in first step scrubs dentine disk by machine slurries.Repetition in one day is scrubbed three times, then by dentine Disk is maintained in 37 DEG C of shaking baths of simulating oral cavity environment, in SOF overnight (> 12 hours).Dentine sample is scrubbed 3 It is secondary.

Mouthsimulator liquid is made by the ingredient in combination table 2:

Table 2

The closed standards of grading of tubule

Regardless of the original-shape of dentine disk, a square (having a size of 4mm × 4mm) is all selected, and 50 A photos are shot under × enlargement ratio.In the square, select 5 points (size of each point is 150 μm of 150 μ m, in Between one, one, each angle), and observed under 1000 × enlargement ratio.Small duct occlusion can according to standard described in table 3 into Row assessment.Two dentine disks of each test group are measured.

Table 3

Scoring	Small duct occlusion
		0	All dentinal tubules are all open.
1	< 20% dentinal tubule is completely enclosed.
		2	The dentinal tubule of 20-50% is completely enclosed.
3	The dentinal tubule of 50-80% is completely enclosed.
		4	The dentinal tubule of 80-100% is completely enclosed.
5	All dentinal tubules are all completely enclosed.

As a result

SEM (scanning electronic microscope examination) photo of dentine disk is shot after 3 scrubs.Photo is analyzed simultaneously Scoring.As a result (standard deviation of error representative duplicate measurements) is summarised in the following table 4.

Table 4

As can be seen that the dentinal tubule of the dentine disk handled with the sample 3 and 4 comprising soluble calcium source is sealed extensively It closes.For sample 1 and 2, many dentinal tubules are still open.

Embodiment 2

The present embodiment confirms effect of the type of calcium silicates to small duct occlusion effect.All the components are with the weight of total formulation Measuring percentage indicates, and is expressed as the content of active constituent.

Table 5

B. the commercially available calcium silicates (CaSiO of the trade name Sorbosil CA40 from Pq Corp.₃)。

Method

As described in example 1 above, closing effect of dentinal tubule is evaluated using identical scheme.By dentine sample Scrub 3 times and 7 times.

As a result

After 3 times and 7 times scrubs, the SEM photograph of dentine disk is shot, is analyzed and is scored.As a result it is summarised in table 6 In (standard deviation of error representative duplicate measurements).

Table 6

A. having the value of different letters has significant difference (P < 0.01).

B. having the value of different letters has significant difference (P < 0.01).

After 3 scrubs, it can be seen that the sample 6 combined comprising tricalcium silicate and calcium chloride is shown and comprising silicic acid Calcium compares significant preferably small duct occlusion effect with the combined sample 8 of calcium chloride.Sample 6 and 8, which is all shown, to be better than not including Small duct occlusion effect of the sample 5 and 7 of calcium chloride.

After 7 scrubs, compared with sample 8, sample 6 still shows better small duct occlusion effect.SEM photograph understands Ground shows that dentinal tubule is closed extensively, and for sample 5 and 7, many tubules are in this of short duration toeatment period It is still open.

Embodiment 3

The present embodiment confirms small to dentine by using the soluble calcium source combined with calcium silicates in whole formulations The improvement of pipe is closed.All the components are indicated with the weight percent of total formulation, and are expressed as the content of active constituent.

Table 7

C. the commercially available silica of the trade name Sorbosil AC77 from Pq Corp..

D. the commercially available silica of the trade name Sorbosil AC43 from Pq Corp..

Method

As a result

After 3 times and 7 times scrubs, the SEM photograph of dentine disk is shot, is analyzed and is scored.As a result it is summarised in table 8 In (standard deviation of error representative duplicate measurements).

Table 8

C. having the value of different letters has significant difference (P < 0.01).

D. having the value of different letters has significant difference (P < 0.01).

After 3 scrubs, it can be seen that the sample 10 combined comprising tricalcium silicate and calcium chloride is shown and comprising silicic acid Calcium compares significant preferably small duct occlusion effect with the combined sample 12 of calcium chloride.

7 times scrub after, sample 10 and 12 show can analogy small duct occlusion effect.SEM photograph clearly illustrates tooth Tubules are closed extensively, and for sample 11, it is still open in this of short duration toeatment period of many tubules.

Embodiment 4

The present embodiment confirms in whole formulations by using the soluble calcium source combined with calcium silicates to dental surface On improved deposition.Sample used herein is such as sample 9-12 listed in embodiment 3.

Method

In order to evaluate the deposition on dental surface, test sample and water are mixed with ratio of the 1g to 2ml water tooth is made Cream slurries.

According to identical scheme, ox glaze mass is handled with different slurries by scrubbing.In the Tooth-brushing device for being equipped with toothbrush It is lower to scrub glaze mass with the slurries.The load brushed teeth is 170g+/- 5g, and operates automatic brushing with the speed of 150rpm. After scrubbing 1min, glaze mass is impregnated into 1min in toothpaste slurries.Then distilled water flushing glaze mass is used, and by it at 37 DEG C It is placed in SOF under the conditions of the shaking bath of 60.0rpm.After impregnating about 3 to 4 hours, using identical with first step Program scrubs glaze mass by the machine slurries.Glaze mass three times, is then maintained at Mouthsimulator by repetition scrub in one day In 37 DEG C of shaking baths of environment in SOF overnight (> 12 hours).Glaze mass is scrubbed 7 times.

As a result

After 7 scrubs, the SEM photograph on glaze mass surface is shot.From the top view of SEM photograph it is clear that sample 10 and 12 generate more preferable and finer and close deposition than sample 9 and 11 on tooth surfaces.Corresponding section SEM photograph is further shown Show, is forming mew layer on the surface of the glaze mass after the sample treatment.There is thickness with the processed glaze mass of sample 10 About 1.8 μm of mew layer, the mew layer are obtained than the new thickness for being about 0.5 μm with the thickness formed in the processed glaze mass of sample 12 It is more.And mew layer is not formed on the surface thereof in this of short duration toeatment period with the processed glaze mass of sample 9 and 11.Packet Sample 9 containing tricalcium silicate is shown than the deposition on the better enamel of sample 11 comprising calcium silicates.

Si, Ca and P element are identified in mew layer using the analysis that EDX (energy dispersion X-ray spectrum) carries out, and show silicon Sour doped calcium on tooth surfaces, and induces remineralization.

Embodiment 5

The present embodiment confirms that the concentration of soluble calcium source will affect small duct occlusion effect.All the components are with total formulation Weight percent indicates, and is expressed as the content of active constituent.

Table 9

Table 10

Method

As described in example 1 above, closing effect of dentinal tubule is evaluated using identical scheme.By dentine sample Scrub 3 times.

As a result

After 3 scrubs, the SEM photograph of dentine disk is shot, is analyzed and is scored.As a result it is summarised in table 11 (standard deviation of error representative duplicate measurements).

Table 11

E. having the value of different letters has significant difference (P < 0.01).

After 3 scrubs, the combined sample 14 comprising 5% calcium chloride and 10% tricalcium silicate shows and comprising 10% The combined sample 15 of calcium chloride and 5% tricalcium silicate is compared to significant preferably small duct occlusion effect.Sample 14 and 15 is both Show significant preferably small duct occlusion effect compared with the sample 13 and 17 respectively only comprising tricalcium silicate or calcium chloride.

After 3 scrubs, sample 14 is also showed that can analogy compared with the sample 18 and 19 comprising higher amount tricalcium silicate Small duct occlusion effect.SEM photograph clearly illustrates that all dentinal tubules are closed extensively.

Claims

1. a kind of oral care composition, it includes:

A) tricalcium silicate；

B) soluble calcium source；

C) phosphate source；With

D) physiologically acceptable carrier；

2. oral care composition according to claim 1, wherein the solubility calcium source is calcium chloride, calcium nitrate, second It is sour calcium, calcium lactate, calcium gluconate, calcium formate, calcium malate, calcium propionate, calcium butyrate, calcium bicarbonate, calcium glycerophosphate, anti-bad Or mixtures thereof hematic acid calcium, or mixtures thereof preferably calcium chloride, calcium nitrate.

3. oral care composition according to claim 1 or 2, wherein the phosphate source is water-soluble.

4. oral care composition according to any one of the preceding claims, wherein the tricalcium silicate is based on composition Weight with 1% to 80%, preferably 3% to 50% amount exist.

5. oral care composition according to any one of the preceding claims, wherein the tricalcium silicate and described solvable Property calcium source exist with the weight ratio of 1:3 to 10:1, preferably 1:1.5 to 5:1.

6. oral care composition according to any one of the preceding claims, wherein the phosphate source is tricresyl phosphate Sodium, sodium dihydrogen phosphate, disodium hydrogen phosphate, ammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, tripotassium phosphate, potassium dihydrogen phosphate, phosphorus Or mixtures thereof sour hydrogen dipotassium.

7. oral care composition according to any one of the preceding claims, wherein the phosphate source is tricresyl phosphate Or mixtures thereof sodium, sodium dihydrogen phosphate.

8. oral care composition according to any one of the preceding claims, wherein the phosphate source is based on composition Weight with 0.5% to 40%, preferably 1% to 30% amount exist.

9. oral care composition according to any one of the preceding claims, wherein the composition further includes choosing From deposition aid below: or mixtures thereof calcium dihydrogen phosphate, calcium sulfate hemihydrate, calcium aluminate, calcium monohydrogen phosphate.

10. oral care composition according to claim 9, wherein the deposition aid is calcium dihydrogen phosphate.

11. oral care composition according to claim 9 or 10, wherein the tricalcium silicate and the deposition aid with The weight ratio of 10:1 to 1:1 exists.

12. oral care composition according to any one of the preceding claims, wherein the oral care composition is Single-phase anhydrous composition.

13. the oral care composition according to any one of preceding claims 1 to 11, wherein the composition is to include The dual phase composition of calcium phase and phosphate phase, wherein the tricalcium silicate and the soluble calcium source are present in the calcium phase, And the phosphate source is present in the phosphate phase.

14. oral care composition according to claim 13, wherein the calcium phase and the phosphate are mutually in composition It is a physically separate before use.

15. a kind of sensibility for reducing individual tooth and/or the method for making individual remineralization of teeth comprising will be according to power Benefit require any one of 1 to 14 described in the composition tooth that is applied to the individual at least one surface the step of.