CN103340896B - A kind of compositions of dual anti-dentin hypersensitiveness and application thereof - Google Patents
A kind of compositions of dual anti-dentin hypersensitiveness and application thereof Download PDFInfo
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Abstract
The invention discloses a kind of compositions and application thereof of dual anti-dentin hypersensitiveness.The effective ingredient of the compositions of dual anti-dentin hypersensitiveness is account for the potassium salt of composition weight percentage ratio 0.3%-12% and the titaniferous bioactivity glass of 0.5%-15%.Dual anti-dentin hypersensitiveness of the present invention compositions, can be used for prevention and therapy (eliminate or alleviate) dentin hypersensitiveness, potassium salt release potassium ion fast pain relief (reducing the irritability of Intradental nerve) on the one hand, bioactivity glass can supplement dental structure mineral on the other hand, and form stable carbonated hydroxyapatite, the degree of depth can close dentinal tubule (changing the permeability of dentinal tubule), curative effect improves greatly, can fundamentally eliminate pain sense and anaphylaxis, reach the object for the treatment of both the principal and secondary aspects of a disease, again because of titaniferous in its composition, the apatite layer that dental surface is formed is firmer wear-resisting, resist daily stimulation better.
Description
Technical field
The present invention relates to a kind of compositions of dual anti-dentin hypersensitiveness, said composition comprises titaniferous bioactivity glass and potassium salt, can be used for prevention and therapy (eliminate or alleviate) dentin hypersensitiveness.
Background technology
Dentin hypersensitiveness is the more common symptom of dental disease, (machinery, chemistry, temperature and the osmotic pressure etc.) environmental stimuli that refers to that the dentin of exposure is subject to and the special symptom of aching of one that produces.Dentin hypersensitiveness's sickness rate is 8%-30%, within about 40 years old, is group of people at high risk, is the commonly encountered diseases of clinical oral, frequently-occurring disease.The symptom that dentin hypersensitiveness relates to and inducement are comparatively extensive, as: wedge shaped defect, periodontal atrophy, Root exposnre, tooth trauma, dentin expose, serious wearing and tearing, tooth preparation, the preparation of hole type, toothwash, scaling, discolor teeth, tune jaw etc.The principal pathogenetic reason of dental hypersensitiveness is when there is the situations such as the impaired or gingival atrophy of enamel, the dentinal tubule exposed is open state, air, hyperosmotic solution or thermal stimulus make the liquid generation change in flow in dentinal tubule, mechanically stir dental pulp content, and then indirect excitation free nerve endings wherein, cause impulsion, produce the pain sensation.
Dental pulp disease expert proposes six aspects for the treatment of dentin hypersensitiveness: 1. the outer end of dentinal tubule is closed or blocked to physical method; 2. chemical method solidifies the protoplasm of dentinal tubule; 3. chemical substance and dental tissue react to be formed and precipitate, block tubule; 4. induce dentinal permeability, close the nearly marrow end of dentinal tubule; 5. anaesthetize speciality and infiltrate dental pulp through tubule, block Intradental nerve end slightly; 6. some materials infiltrate dental pulp through tubule, suppress exciting of Intradental nerve.These six rules and regulations are received 2 points: one is the permeability changing dentinal tubule; Two is the irritabilitys reducing Intradental nerve.
Bioactivity glass was found by U.S. professor Hench in 1969, was a kind of bioactive materials.As everyone knows, the existing osteogenesis of bioactivity glass, has bone guided effect again, has good associativity with osseous tissue and soft tissue, and it is considered to the good biological material that can be applicable to reparation field.The reaction that bioactivity glass can occur rapidly with water and saliva, continue, release calcium ion and phosphate anion, supplement dental structure mineral, to be deposited in dentinal tubule or on, long term can produce stable crystalline hydroxyapatite layer and insert dentinal tubule, closes dentinal tubule, induces new dentium nitor face to be formed, change the permeability of dentinal tubule, reduce dentin hypersensitiveness's reaction.Again because it can form one deck stable crystalline hydroxyapatite layer at dental surface, effectively can fill up Cranial defect, enamel, dentin defect, form area of new bone, can fundamentally change the Cranial defect occurred on tooth, and then fundamentally can eliminate the phenomenon of dentin hypersensitiveness.
Titanium is a kind of body trace element, has good high-temperature capability, low-temperature flexibility and fracture toughness, can stimulate phagocyte, and immunity is strengthened.The intensity of titanium alloy is high, corrosion stability good, strong especially to the resistance of spot corrosion, acid etching, stress corrosion, has excellent resistance to corrosion to organic article, nitric acid, sulphuric acid etc. of alkali, chloride, chlorine.Titanium or titanium alloy has especially special character at medical field: 1) titanium can form rapidly the good titanium dioxide passivating film of biocompatibility in air and blood, and directly do not contact with when injected organism tissue, thus have and can not have dysgenic advantage to the metabolism of implant; 2) decay resistance in air and physiological environment makes implant can life-time service; 3) easily preparation is different structural interface, optimization pattern and porosity are to meet the needs of live body receptor tissue; 4) anaphylaxis is not found up to now.Titanium oxide adds in bioceramic material, and its biocompatibility, stiffness, wearability, corrosion stability can be made to improve.Titanium oxide is applied to existing a lot of research in bone renovating material.The bioceramic material containing titanium oxide of the warm ripple research of Jilin University's stomatological hospital may be used on Wistar neonatal rat parietal bone, find that this material has good cell compatibility (Wen Bo, Huang Ying, Xu Yongzhong. the research [J] of titanium oxide bioceramic cytocompatibility. Jilin University's journal (medicine) the 30th volume the 3rd phase in 2004 418 pages).Having containing the calcium phosphate bioceramic coating of titanium oxide of the preparation such as the Wang Yaming of Harbin University of Science and Technology's special cermacis institute good lures osteogenesis characteristic (Wang Yaming, Zhou Yu, Judd is prosperous, micro-arc oxidation prepares titania based porous composite boilogical ceramic coating [J], Rare Metals Materials and engineering, the 34th volume 1244 pages in 2005).
The mechanism of potassium salt desensitization is: potassium ion contained in potassium salt discharges, potassium ion enters into Dentinal tubule, affinity interaction is had with teleneuron, improve the transmission of Nerve impulse, by the signal of inhibition of Chemical Reaction teleneuron conducting pain, inhibit the remineralization of dental nerve, thus reduce Intradental nerve to hot and cold, sour, sweet irritability and sensitivity, anesthesia Intradental nerve, alleviating pain.If use a period of time continuously, potassium ion in dentinal tubule can be made to reach certain dynamic equilibrium, and effect is continuous and effective more.
Patent documentation U.S.3863006 discloses the toothpaste comprising potassium salt such as potassium nitrate, reduces the sensitivity of tooth after a few week of brushing teeth.It is produce topical application comprise the dental products of potassium nitrate and bring the reason of therapeutic desensitization that those skilled in the art believe that extracellular potassium concentration near the Intradental nerve under hypersensitive dentine raises.But independent potassium ion can not inaccessible dentinal tubule, is necessary to reuse potassium salt, to set up necessary concentration near Intradental nerve, to reduce the irritability of Intradental nerve, alleviating pain.
Patent documentation CN1306416A discloses a kind of two component desensitizing dental composition, and this dentifrice composition comprises a kind of potassium salt and a kind of tin salt.During use, these two kinds of compositions are used in combination by proportioning.This invention uses due to two kinds of salts simultaneously, and the mastic of toothpaste is unstable, therefore can not be applied in same pipe toothpaste, therefore use inconvenience.
Patent documentation CN101407373B discloses a kind of strontium-reinforced bioactive glass, uses it for the manufacture of dentifrice-toothpaste, obviously can play the effect of the symptoms such as anti-dental hypersensitiveness, gingival hemorrhage and anti-plaque.If but when only playing the effect of enhanced biological glass, the cost of strontium oxide is higher, and strontium oxide chance water releases large calorimetric, can decompose gradually with air, more unstable.
Patent documentation CN100536812C discloses a kind of energy and eliminates or alleviate the two component tooth composites that do not accommodate pain relevant with dentin hypersensitiveness, wherein compositions comprises with first toothpaste component with neutral pH of alkali metal phosphate buffer pH in 6.5 to 7.5 scopes, second toothpaste component with alkaline pH of pH in 8 to 12 scopes, and at least one component comprise can releasing fluoride ion be selected from sodium fluoride, potassium fluoride, sodium monofluorophosphate, the salt of stannous fluoride and prodan and can discharge potassium ion be selected from potassium nitrate, potassium citrate, potassium chloride, the salt of potassium bicarbonate and potassium oxalate, first and second components keep each other be separated until preparation and combine be used in require alleviate dentin hypersensitiveness tooth on, user finds that desensitization strengthens thus.But said composition belongs to toothpaste with fluoride, have certain harm to human body, and this compositions inherently can not repair the open dentinal tubule in irritated position.
Although prior art discloses the multiple compositions for prevention and therapy dentin hypersensitiveness, but these compositionss have cures the symptoms, not the disease, can produce dependency and the shortcoming such as price is higher, therefore still need to develop that curative effect strengthens, the compositions for prevention and therapy dentin hypersensitiveness for the treatment of both the principal and secondary aspects of a disease.
Summary of the invention
The object of this invention is to provide the compositions comprising the dual anti-dentin hypersensitiveness of two kinds of effective ingredient for prevention and therapy (eliminate or alleviate) dentin hypersensitiveness of the enhancing of a kind of curative effect, treating both the principal and secondary aspects of a disease.
The compositions of dual anti-dentin hypersensitiveness provided by the present invention, its effective ingredient is account for the potassium salt of composition weight percentage ratio 0.3%-12% and the titaniferous bioactivity glass of 0.5%-15%.
Described potassium salt is potassium nitrate, potassium chloride, potassium citrate, potassium oxalate, dipotassium hydrogen phosphate, potassium dihydrogen phosphate and potassium bicarbonate etc. dissolve in the potassium salt of the provided potassium ion source of glycerol or water one or more.
Described titaniferous bioactivity glass is particulate bioactive glass, and particle diameter is less than 100 μm, with mass ratio range, wherein containing following glass ingredient:
After described bioactivity glass and water or physiological solution are had an effect, can generate hydroxyapatite, in infrared spectrogram, demonstrate the characteristic peak of hydroxyapatite, wave number is at 602 ± 5cm
-1with 560 ± 5cm
-1the reflection peak at place.
Described bioactivity glass can be prepared by sol-gel process, high-temperature fusion sintering process or hydro-thermal method:
The concrete steps that described sol-gel process prepares bioactivity glass are: take dust technology as catalyst, by the alcoholic solution of raw material ethyl orthosilicate corresponding for glass ingredient, the alcoholic solution of triethyl phosphate, lime nitrate alcoholic solution, Chile saltpeter Ludox, butyl titanate alcoholic solution is feeding respectively, add reaction vessel successively under agitation, after stirring 90min, wet gel is obtained after rising to 40 DEG C of precipitation 24h-72h by room temperature, sieve after dry 12h-48h at 60 DEG C-100 DEG C again, siftage is put into Muffle furnace 600 DEG C-750 DEG C sintering 4h and is obtained the bioactive glass powder that particle diameter is less than 100 μm,
The concrete steps that described high-temperature fusion sintering process prepares bioactivity glass are: by feed oxygen SiClx corresponding for glass ingredient, calcium carbonate, sodium phosphate, sodium carbonate, sodium titanate powder feeding, dry after putting into ball mill wet grinding, put into corundum crucible, then melting in 1200 DEG C-1450 DEG C in Muffle furnace, shrend in distilled water after insulation 2h, ball mill pulverizing after the drying of shrend formation, sieving obtains the bioactive glass powder that particle diameter is less than 100 μm;
The concrete steps that described hydro-thermal method prepares bioactivity glass are: first by feed oxygen SiClx corresponding for glass ingredient, calcium carbonate, sodium phosphate, sodium carbonate, sodium titanate feeding, be put in ball milling 5h-10h in ball mill, on hydraulic press, block or cylinder is pressed into after drying and screening, then the powder body after compacting is put in high-pressure hydrothermal reaction kettle, after 180 DEG C of-250 DEG C of hydrothermal treatment consists 24h-72h, screens the bioactive glass powder that particle diameter is less than 100 μm.
The above dual anti-dentin hypersensitiveness compositions can be unguentum, paste, gel, solution, membrane or powder.
One or more in abrasivus, surfactant, sweeting agent, spice, thickening agent, adhesive, antiseptic and wetting agent etc. can also be comprised in described dual anti-dentin hypersensitiveness compositions:
Described abrasivus can be the mixture of one or more in calcium phosphate, calcium carbonate, calcium pyrophosphate, aluminium hydroxide, silicon oxide, and be preferably silicon oxide or silicon oxide and other one or more mixture, accounting for composition weight percentage ratio is 10%-16%;
Described surfactant can be the mixture of one or more in N-sodium lauroyl sarcosine, sodium lauryl sulphate and dodecylbenzene sodium sulfonate, and accounting for composition weight percentage ratio is 1%-3%;
Described sweeting agent can be the mixture of one or more in saccharin sodium, steviosin and xylitol, and accounting for composition weight percentage ratio is 0.1%-1.5%;
Described spice can be the one stayed in orchid, Herba Menthae, Fructus Citri Limoniae, green tea and Ilicis Purpureae, and accounting for composition weight percentage ratio is 0.5%-1.5%;
Described thickening agent can be one or both the mixture in silicon dioxide and aluminium-magnesium silicate, and accounting for composition weight percentage ratio is 5%-10%;
Described adhesive can be the mixture of one or more in carbomer, sodium carboxymethyl cellulose, guar gum and carrageenan, and be preferably carbomer or carbomer and the mixture of one or more wherein, accounting for composition weight percentage ratio is 0.2%-0.4%;
Described antiseptic can be one or both the mixture in hydroxy benzoic acid sodium and sodium sulfite, and accounting for composition weight percentage ratio is 0.05%-0.1%;
Described wetting agent can be the mixture of one or more in glycerol, Polyethylene Glycol, sorbitol and propylene glycol, and accounting for composition weight percentage ratio is 55%-70%.
Present invention also offers a kind of method preparing the compositions of dual anti-dentin hypersensitiveness, can comprise the following steps:
1) take raw material by formula, under rapid stirring, abrasivus, bioactive glass powder, potassium salt, sweeting agent, thickening agent, adhesive, antiseptic, surfactant are pre-dispersed in wetting agent respectively;
2) under the condition of vacuum, rapid stirring, according to a definite sequence by abrasivus scattered for step 1), bioactive glass powder, potassium salt, sweeting agent, thickening agent, adhesive, antiseptic, surfactant mix homogeneously, and rapid stirring;
3) add spice under low rate mixing condition, leave standstill, obtain dual dentin hypersensitiveness compositions.
Wherein, described step 2) in the rapid stirring time be 0.5h-1h; Time of repose in described step 3) is 10min-2h, is preferably 0.5h.
The above dual anti-dentin hypersensitiveness compositions also belongs to the present invention preparing the application in Related product.Related product is: for the pharmaceutical composition of anti-dentin hypersensitiveness; For preventing or treat the pharmaceutical composition of teeth corrosion, gingival hemorrhage; Or for cleaning one's teeth, the product of dental care or oral hygiene.
Adopt above scheme, the invention provides the dual anti-dentin hypersensitiveness compositions that a kind of main component comprises bioactivity glass and potassium salt, can be used for prevention and therapy (eliminate or alleviate) dentin hypersensitiveness, potassium salt release potassium ion fast pain relief (reducing the irritability of Intradental nerve) on the one hand, bioactivity glass can supplement dental structure mineral on the other hand, and form stable carbonated hydroxyapatite, the degree of depth can close dentinal tubule (changing the permeability of dentinal tubule), curative effect improves greatly, can fundamentally eliminate pain sense and anaphylaxis, reach the object for the treatment of both the principal and secondary aspects of a disease, again because of titaniferous in bioactivity glass composition, the apatite layer that dental surface is formed is firmer wear-resisting, resist daily stimulation better.
Below in conjunction with specific embodiment, the present invention is described in further details.
Accompanying drawing explanation
Fig. 1 is the infrared spectrum of the hydroxyapatite generated after titaniferous bioactivity glass Tris solution soaking 48h
Fig. 2 is the SEM figure of dentin hypersensitiveness position without the dentinal tubule of repairing
Fig. 3 uses the artificial saliva being dispersed with the present invention dual anti-dentin hypersensitiveness compositions to soak Dentinal SEM figure after five days
Fig. 4 uses the artificial saliva being dispersed with the present invention dual anti-dentin hypersensitiveness compositions to soak after five days to scheme at the SEM of the apatite layer of dentin surface's formation
Fig. 5 is through the Dentinal tooth of the present invention dual anti-dentin hypersensitiveness compositions, repairs, and every day schemes with the dentin SEM of laughable immersion 5min, imitation chemical stimulation in continuous five days, toothbrush grooming 40 imitation physical stimulations
Fig. 6 is after lactic acid demineralization, without the SEM figure of the enamel surface repaired
Fig. 7 uses the mastic simulation toothpaste being dispersed with the present invention dual anti-dentin hypersensitiveness compositions to brush teeth process to tooth after demineralization, and twice daily, each 5 minutes, after using one week continuously, adamantine SEM schemed
Detailed description of the invention
The invention provides a kind of dual anti-dentin hypersensitiveness compositions, be the synergism utilizing two kinds of desensitizeies, provide a kind of than single desensitizer more effectively, more thoroughly anti-dentin hypersensitiveness product.
Dual anti-dentin hypersensitiveness provided by the present invention compositions, its effective ingredient is account for the potassium salt of composition total weight 0.3%-12% and the titaniferous bioactivity glass of 0.5%-15%.Wherein:
Potassium salt is potassium nitrate, potassium chloride, potassium citrate, potassium oxalate, dipotassium hydrogen phosphate, potassium dihydrogen phosphate and potassium bicarbonate etc. dissolve in the mixing of one or more in the potassium salt of the provided potassium ion source of glycerol or water, does not have ratio to limit during mixing; The raw material selection that potassium nitrate, potassium chloride, potassium citrate, potassium oxalate, dipotassium hydrogen phosphate, potassium dihydrogen phosphate and potassium bicarbonate easily can obtain by reality, effect is suitable.
Titaniferous bioactivity glass is particulate bioactive glass, and particle diameter is less than 100 μm.Its composition by weight percentage, comprises (by weight percentage):
This titaniferous bioactivity glass by the proportioning raw materials of above-mentioned glass ingredient, can be prepared by sol-gel process, high-temperature fusion sintering process or hydro-thermal method:
The concrete steps that sol-gel process prepares bioactivity glass are: take dust technology as catalyst, by the alcoholic solution (ethanol molal quantity is 2 ~ 7 times of ethyl orthosilicate molal quantity) of raw material ethyl orthosilicate corresponding for glass ingredient, the alcoholic solution (ethanol molal quantity is the molal quantity such as grade of triethyl phosphate) of triethyl phosphate, lime nitrate alcoholic solution (ethanol molal quantity is 1.5 ~ 4.5 times of lime nitrate molal quantity), Chile saltpeter, magnesium nitrate, potassium nitrate, the weight ratio feeding that butyl titanate alcoholic solution (ethanol molal quantity is 2 ~ 7 times of ethyl orthosilicate molal quantity) calculates by glass ingredient, the order mentioned by described various raw material under agitation adds in reaction vessel successively, after stirring 90min, wet gel is obtained after rising to 40 DEG C of precipitation 24h-72h by room temperature, sieve after dry 12h-48h at 60 DEG C-100 DEG C again, under sieve, (less than 100 μm) powder is put into Muffle furnace 600 DEG C-750 DEG C sintering 4h and is obtained the bioactive glass powder that particle diameter is less than 100 μm,
The concrete steps that high-temperature fusion sintering process prepares bioactivity glass are: by feed oxygen SiClx corresponding for glass ingredient, calcium carbonate, sodium phosphate, sodium carbonate, magnesium carbonate, potassium carbonate, sodium titanate powder, the weight feeding calculated by glass ingredient, dry again after putting into ball mill wet grinding, put into corundum crucible, then melting in 1200 DEG C-1450 DEG C in Muffle furnace, shrend in distilled water after insulation 2h, after the drying of shrend molding again ball mill pulverizing, sieving obtains the bioactive glass powder that particle diameter is less than 100 μm;
The concrete steps that hydro-thermal method prepares bioactivity glass are: first by weight ratio feeding that feed oxygen SiClx corresponding for glass ingredient, calcium carbonate, sodium phosphate, sodium carbonate, magnesium carbonate, potassium carbonate, sodium titanate glass ingredient calculate, be put in ball milling 5h-10h in ball mill, on hydraulic press, block or cylinder is pressed into after drying and screening (200 order), then the powder body after compacting is put in high-pressure hydrothermal reaction kettle, after 180 DEG C of-250 DEG C of hydrothermal treatment consists 24h-72h, selects particle diameter to be less than the bioactive glass powder of 100 μm.
After bioactivity glass and water or physiological solution are had an effect, can generate hydroxyapatite, in infrared spectrogram, demonstrate the characteristic peak of hydroxyapatite, wave number is at 602 ± 5cm
-1with 560 ± 5cm
-1the characteristic peak at place.
In the present composition, employ the titaniferous bioactivity glass of special preparation, during use, this titaniferous bioactivity glass can generate with water and ptyaloreaction the hydroxyapatite being deposited on dental surface, and hydroxyapatite is more firm wear-resisting.
In the present invention, dual anti-dentin hypersensitiveness compositions can work with the form of unguentum, paste, gel, solution, membrane or powder, and time multi-form, base material is corresponding conventional materials, as glycerol, carrageenan, Polyethylene Glycol etc. wherein one or more.Other additive can also be comprised, as one or more in abrasivus, surfactant, sweeting agent, spice, thickening agent, adhesive, antiseptic and wetting agent etc. in dual anti-dentin hypersensitiveness compositions.Abrasivus can be the mixture of one or more in calcium phosphate, calcium carbonate, calcium pyrophosphate, aluminium hydroxide, silicon oxide, and be preferably silicon oxide or silicon oxide and other one or more mixture, during mixing, silicon dioxide accounts for more than 50%; The raw material selection that calcium phosphate, calcium carbonate, calcium pyrophosphate, aluminium hydroxide easily can obtain by reality, effect is suitable.It is 10%-16% that abrasivus accounts for composition weight percentage ratio.Surfactant can be the mixture of one or more in N-sodium lauroyl sarcosine, sodium lauryl sulphate and dodecylbenzene sodium sulfonate, does not have ratio to limit during mixing; The raw material selection that N-sodium lauroyl sarcosine, sodium lauryl sulphate and dodecylbenzene sodium sulfonate easily can obtain by reality, effect is suitable.It is 1%-3% that surfactant accounts for composition weight percentage ratio.Sweeting agent can be the mixture of one or more in saccharin sodium, steviosin and xylitol, does not have ratio to limit during mixing, and the raw material selection that easily can obtain by reality, effect is suitable.It is 0.1%-1.5% that sweeting agent accounts for composition weight percentage ratio.Spice can be the one stayed in orchid, Herba Menthae, Fructus Citri Limoniae, green tea and Ilicis Purpureae, and accounting for composition weight percentage ratio is 0.5%-1.5%.Thickening agent can be one or both the mixture in silicon dioxide and aluminium-magnesium silicate, does not have ratio to limit during mixing, and the raw material selection that easily can obtain by reality, effect is suitable.It is 5%-10% that thickening agent accounts for composition weight percentage ratio.Adhesive can be the mixture of one or more in carbomer, sodium carboxymethyl cellulose, guar gum and carrageenan, is preferably carbomer or carbomer and the mixture of one or more wherein, does not have ratio to limit during mixing; The raw material selection that sodium carboxymethyl cellulose, guar gum and carrageenan easily can obtain by reality, effect is suitable.It is 0.2%-0.4% that adhesive accounts for composition weight percentage ratio.Antiseptic can be one or both the mixture in hydroxy benzoic acid sodium and sodium sulfite, does not have ratio to limit during mixing, and the raw material selection that easily can obtain by reality, effect is suitable.It is 0.05%-0.1% that antiseptic accounts for composition weight percentage ratio.Wetting agent can be the mixture of one or more in glycerol, Polyethylene Glycol, sorbitol and propylene glycol, does not have ratio to limit during mixing, and the raw material selection that easily can obtain by reality, effect is suitable.It is 55%-70% that wetting agent accounts for composition weight percentage ratio.
The mechanism of compositions prevention and therapy (eliminate or alleviate) dentin hypersensitiveness of dual anti-dentin hypersensitiveness of the present invention is as follows:
1, potassium salt has the irritability and sensitivity that reduce Intradental nerve, anesthesia Intradental nerve, lenitive effect;
2, bioactivity glass can react with water and saliva, produces the stable crystalline hydroxyapatite layer be deposited in dentinal tubule, closes dentinal tubule, changes the permeability of dentinal tubule; Again because strengthening the titanium oxide of its material mechanical containing having in bioactivity glass component, the new hydroxyapatite layer formed is strengthened modification, and then tooth is strengthened, better resist daily stimulation, the present invention can reinforced bioactivity glass glass except with strontium disclosed in patent documentation CN101407373B, also make it have the advantage of better wearability, corrosion stability, the more important thing is mix titanium bioactive glass lure osteogenesis characteristic good;
3, potassium salt and titaniferous bioactivity glass two kinds of combination of components can produce synergistic function, can play effect of better and lasting anti-dentin hypersensitiveness compared with one-component.The present invention uses potassium salt to combine the bioactive materials of progressively mineralising sealing process in dentin surface, analgesic effect can be made better, and significantly can reduce the liquid stream in the tubule of stimulation pain.In the process of potassium salt relieving ease pain, can bioactivity glass be utilized to close dentinal tubule, induction dentium nitor face be formed, and plays the effect of reparation, fundamentally eliminates anaphylaxis.
Present invention also offers a kind of method preparing dual anti-dentin hypersensitiveness compositions, can comprise the following steps:
1) take raw material by formula, under rapid stirring, abrasivus, bioactive glass powder, potassium salt, sweeting agent, thickening agent, adhesive, antiseptic, surfactant are pre-dispersed in wetting agent respectively;
2) under the condition of vacuum, rapid stirring, according to a definite sequence by abrasivus scattered for step 1), bioactive glass powder, potassium salt, sweeting agent, thickening agent, adhesive, antiseptic, surfactant mix homogeneously, and rapid stirring;
3) add spice under low rate mixing condition, leave standstill, obtain dual dentin hypersensitiveness compositions.
In the preparation method of above-mentioned dual anti-dentin hypersensitiveness compositions, step 2) in the rapid stirring time be 0.5h-1h.Time of repose in step 3) is 10min-2h, is preferably 0.5h.
The application of described dual anti-dentin hypersensitiveness compositions in the pharmaceutical composition for the preparation of anti-dentin hypersensitiveness also belongs to protection scope of the present invention.
Described dual anti-dentin hypersensitiveness compositions is also belonging to protection scope of the present invention for the preparation of prevention or the application for the treatment of in the pharmaceutical composition of teeth corrosion, gingival hemorrhage.
Described dual anti-dentin hypersensitiveness compositions also belongs to protection scope of the present invention in the application for the preparation of cleaning one's teeth, in the product of dental care or oral hygiene.
Embodiment is implemented under premised on technical solution of the present invention, gives detailed embodiment and concrete operating process, and embodiment will contribute to understanding the present invention, but protection scope of the present invention is not limited to following embodiment.
In following embodiment, method therefor is conventional method if no special instructions.
The formula of embodiment 1-5 dual anti-dentin hypersensitiveness compositions and comparative example is as shown in table 1:
The formula of table 1 embodiment 1-5 dual anti-dentin hypersensitiveness compositions and comparative example
Bioactivity glass can prepare by aforementioned sol-gel process, high-temperature fusion sintering process or hydro-thermal method, no longer repeats.
Embodiment 1-5 paste dual anti-dentin hypersensitiveness compositions can be prepared according to the following steps:
1) take raw material by the percentage by weight in table 1, under rapid stirring, abrasivus, bioactive glass powder, potassium salt, sweeting agent, thickening agent, adhesive, antiseptic, surfactant are pre-dispersed in wetting agent respectively;
2) under the condition of vacuum, rapid stirring, according to a definite sequence by abrasivus scattered for step 1), bioactive glass powder, potassium salt, sweeting agent, thickening agent, adhesive, antiseptic, surfactant mix homogeneously, and rapid stirring 0.5h-1h;
3) add spice under low rate mixing condition, leave standstill 0.5h, obtain dual dentin hypersensitiveness compositions.
After testing, bioactivity glass prepared by embodiment 1-5 is particulate bioactive glass, and particle diameter is less than 100 μm.After bioactivity glass and water or physiological solution are had an effect, can generate hydroxyapatite, in infrared spectrogram (see figure 1), demonstrate the characteristic peak of hydroxyapatite, wave number is at 602 ± 5cm
-1with 560 ± 5cm
-1the reflection peak at place.
The oral cavity safety of test example one, detection the present invention dual anti-dentin hypersensitiveness compositions
Detect the oral cavity safety of dual anti-dentin hypersensitiveness compositions prepared by embodiment 1-5, carry out repeatedly oral stimulation reaction test according to the method specified in GB/T16886.10 and test, concrete grammar is as follows:
The cricetulus auratus of select health, just growing up, the mastic be made into embodiment 1-5 is directly as test sample.Before test after the normal saline flushing of upset cricetulus auratus buccal, inspection has without exception.Soak into test sample with cotton balls, record volume used, put into the buccal, both sides of animal.Time of contact should be no less than 5min.Remove cotton balls after contact, use normal saline flushing buccal, opposite side cheek pouch not setting-out product in contrast.Give sample every day 2 times, the morning 1 time, afternoon 1 time, totally 7 days.After last is to sample, 24h observes its medicine-feeding part with or without erythema and edema.And fill in experimental observation log.Perusal cheek pouch after taking-up test ball, and before each contact, (during multiple-contact) checks cheek pouch.Describe the general status of animal cheek pouch, and by the standard score system that table 2 provides, judge that each observation period cheek pouch surface erythema of animal is scored.In this test, each embodiment gets 3 cricetulus auratuses, and calculates its average mark after scoring respectively, and the mean score situation of embodiment 1-5 and comparative example 3 is listed in table 3.
Oral cavity reaction detection result is as shown in table 3, can find out that the mean score of embodiment 1-5 is starkly lower than blank group, shows that the oral cavity safety of dual anti-dentin hypersensitiveness compositions prepared by embodiment 1-5 is better.
Table 2 oral cavity reaction normal score system
| Reaction | Standard is scored |
| Without erythema | 0 |
| Pole slight erythema | 1 |
| Erythema is clear | 2 |
| Moderate erythema | 3 |
| Severe erythema (aubergine) is formed to eschar | 4 |
Table 3 oral cavity reaction normal is scored appraisal result
| Group | Mean score |
| Embodiment 1 | 0 |
| Embodiment 2 | 1 |
| Embodiment 3 | 0 |
| Embodiment 4 | 1 |
| Embodiment 5 | 0 |
| Comparative example 3 blank | 2 |
Oral histology evaluates: last is to 24h perusal cheek pouch after sample, euthanasia suslik, the tissue sample getting the representative position of cheek pouch is put into fixative and (is generally used 4% formalin, compound method is: directly dilute by 1:9 with PBS or 0.9% sodium chloride injection) carry out Histological evaluation under the microscope after internal fixtion (consumption of fixative is generally the 10-20 of tissue volume doubly, fixing 1-2 days).
Oral histology's evaluation criterion is as shown in table 4, score according to evaluation and can calculate oral mucosa stimulation index, concrete grammar is: in test group, the microscopic evaluation of all animals is scored addition, then divided by observation sum, draws test group mean score (maximum scoring is 16).Comprehensive perusal and Histological evaluation's result, test group mean score deducts blank group mean score and draws oral mucosa stimulation index.
Equally, in this test, each embodiment gets three cricetulus auratuses, and calculates its oral mucosa stimulation index after integration respectively.
Oral mucosa stimulation index appraisal result is as shown in table 5, can find out that the oral mucosa stimulation index of embodiment 1-5 is starkly lower than blank group, show by the paste dual anti-dentin hypersensitiveness compositions in embodiment 1-5 Golden Hamster multiple-contact oral cavity almost nonirritant.
Table 4 oral histology microscope standard score system
Table 5 oral histology microscope appraisal result
| Group | Stimulation index | The extent of reaction |
| Embodiment 1 | 2 | Extremely light |
| Embodiment 2 | 1 | Extremely light |
| Embodiment 3 | 2 | Extremely light |
| Embodiment 4 | 1 | Extremely light |
| Embodiment 5 | 1 | Extremely light |
| Comparative example 3 blank | 3 | Extremely light |
The tooth antiallergic effect of test example two, detection the present invention dual anti-dentin hypersensitiveness compositions
To embodiment 5, comparative example 1(single creature activity glass group), the single potassium salt group of comparative example 2() and comparative example 3(blank) four groups of samples carry out tooth antiallergic detection, 80 people suffering from dental hypersensitiveness are divided into four groups at random, often organize 20 people, all experimenters use the toothbrush of the same model of same manufacturer production.All experimenters at least use sample twice every day, smear sensitizing range or use sample to brush teeth, use six weeks continuously.
Test method: 1. clinical examination, probe is visited to draw and is suffered from odonthemodia position, record sensitivity; Trouble tooth and adjacent teeth are kept apart with lap, cold air vertically blows 1s apart from buccal surface 5mm, record sensitivity (i.e. pain level).Repeat 2 times, if 2 degree varies cause, degree of getting weighs; If cause 2 kinds of irritant reaction degree varies, severe one is answered in negate.2. sensitivity classification: the evaluation criteria that Ishikawa repaiies two is divided into 4 degree, 3 degree can be brought out insufferable pain for stimulation; 2 degree can be brought out obvious pain for stimulation, but can stand; 1 degree for stimulating the pain that can bring out comparatively slight or have sense of discomfort; 0 degree is that cold-peace mechanical stimulus is without pain.The odonthemodia position that whole test takes same method assessment experimenter to fix, experimenter, after tooth is upset, records sensitivity, base line assessment in 0 week; When 2 weeks mid-stage assessment and 6 weeks time latter stage assessment.3. efficacy assessment standard: effective for treatment before and after the number of degrees poor >=2; Effectively for number of degrees difference before and after treatment is 1; Invalid is 0 for treating front and back number of degrees difference; Worsen as before and after treatment, number of degrees difference is negative.Effective percentage (%)=(effective+effectively) number/treatment sum × %.
Testing result is as shown in table 6-table 8, and all experimenters (120 people) completing test records and sensitivity (i.e. pain level) rank before have evaluated the 0 use sample of thoughtful 6 weeks and after use.According to record result, after use sample, the anti-dentin hypersensitiveness effect that I group of dual antiallergic sample, II group of single creature activity glass sample and III group of single potassium salt sample can be certain; Make a concrete analysis of number of degrees difference before and after each group for the treatment of to find, I group of dual antiallergic sample is used to be better than other three groups, namely experimenter uses sensitivity (i.e. pain level) before and after I group of dual antiallergic sample to decline significantly, and decline time of occurrence comparatively early (first week starts), subject for pain's sensation that sensitivity (i.e. pain level) declines is not no longer repeatedly (before using sample, have the pain level of 29 people to be 3 degree in experimenter, 1 people's pain level is 2 degree.Use sample after one week, in its 25 people, the pain level of 4 people reduces to 2 degree, and the pain level of another people reduces to 1 degree by 2 degree.Use sample after 2 weeks, when one week, pain level is reduced in 4 people of 2 degree, and have people's pain level to continue to drop to 1 degree, the pain level of its excess-three people is still classified as 2 degree, and initial pain level is that 3 degree of experimenters have again 7 people to reduce to 2 degree at second week.Until in the 6th week tested 30 people pain level 3 degree 29 people in pain level all reduce, wherein 16 people reduce to 0 degree, no longer feels pain, 10 people reduce to 1 degree, 3 people reduce to 2 degree, and observation does not find the experimenter raised again after pain level reduces in six weeks), sensitivity has no recovery and (uses sample after one week, the experimenter reducing to 2 degree of pain level does not feel the rank of the pain of 3 degree again, there is not being superior to the pain perception of 1 degree in 1 people reducing to 1 degree, continue to observe to the 6th week, all there is not the phenomenon that pain level recovers in 30 experimenters that all pain level reduce, namely pain level no longer recovers after reducing.During as the 5th week, the 5 people's ranks being 3 degree at 4th week pain level reduce to 2 degree, 4th week pain level is that the 6 people's ranks that have of 2 degree reduce to 1 degree, 4th week pain level is that 13 people of 1 degree have 5 people's pain level to reduce to 1 degree, 4th week to the 5th Monday Zhou Zhezhong pain level have 1 people to keep 2 degree, have 8 people to keep 1 degree, 5 people are 0 degree always, do not occur the experimenter raised after pain level reduces; Its existing 5 people's pain level from 4th week reduce to 0 degree, until the 6th week this five people occurs pain perception not yet, show that the antiallergic persistent period is long, effect stability; II group of experimenter be not because the sample used is containing potassium salt, and the reparation damaged tooth of bioactivity glass needs certain hour, so the sensitivity downward trend of experimenter is poor compared with I group, fall time is I group of evening comparatively, and effect is also more stable; III group of sample used is only containing potassium salt, just can reduction of patient pain after using, so experimenter's sensitivity declines and I group of no difference of science of statistics, but potassium salt alleviating pain acting duration is shorter, and damaged tooth still exposes dentinal tubule, the easy irriate of dental nerve, so part experimenter sensitivity recovers simple, repeatedly, namely respite effect is better, but effect is unstable for pain perception; At use sample after 6 weeks, each group antiallergic effect has certain enhancing; IV group of blank sample not obvious anti-dentin hypersensitiveness effect.Table 7, 8 add up its effective percentage according to the difference of the sensitivity before and after treatment, I group of dual antiallergic sample use after two weeks effective percentage more than 50%, after six weeks, effective percentage is up to 86.7%, antiallergic effect is obviously better than the sample sets of single potassium salt and single creature activity glass, two kinds of compositionss are with the use of can rapid pain relief due to potassium salt, instant effect, bioactivity glass is potassium salt is lenitive while, reparation damaged tooth position slowly, when potassium salt DeGrain or after disappearing, because damaged part is repaired by bioactivity glass, no longer recover after patient pain's rank is reduced, namely patient is while pain level slowly reduces, damaged tooth position have also been obtained reparation, when meeting environmental stimuli again, pain can not be felt again, there is the synergistic function of antiallergic effect instant effect and antiallergic persistent period length, and in the test of six weeks, there is no the side effect finding the side effect relevant to test products and sample oral cavity soft tissue.
Table 6 experimenter sensitivity rank
The antiallergic curative effect of table 7 four groups of samples
The antiallergic curative effect statistics of table 8 four groups of samples
The Dental Erosion effect of test example three, the present invention dual anti-dentin hypersensitiveness compositions
1, to the repairing effect of dentin hypersensitiveness position without the dentinal tubule of repairing
Test method is:
(1) people's tooth specimen preparation: sample tooth is through removing adhering tissue, and with cutting machine, tooth cutting adult tooth is indulged portion's specimen, sterilization and ultrasonic cleaning, select flawless glaze paint to be trial zone, 600# sand paper polishes, and is coated with nial polish outside trial zone;
(2) get exposure Dentinal vertical portion tooth specimen 20, with the citric acid acid etching dentin 1min of 50%, then push away distilled water flushing tooth specimen 1min with 50ml, then dry for subsequent use;
(3) at random 12 tooth specimen are divided into A, B, C tri-groups, often organize 4, A group does not process observes dentin hypersensitiveness position; B group is soaked in the artificial saliva being dispersed with 1cm toothpaste sample (the present invention dual anti-dentin hypersensitiveness compositions prepared by embodiment 5), and every 12h changes a soak, continues 5 days, scanning electron microscopic observation; C group is soaked in the artificial saliva being dispersed with 1cm toothpaste sample (the present invention dual anti-dentin hypersensitiveness compositions prepared by embodiment 5) equally, chemical stimulation is simulated every 12h coca cola beverage infusion 5min, toothbrush 20 times is with analog physical mechanical stimulus, so repeatedly, continue 5 days, scanning electron microscopic observation.
Dentin hypersensitiveness position without repair dentinal tubule SEM picture as shown in Figure 2; The artificial saliva that use is dispersed with the present invention dual anti-dentin hypersensitiveness compositions (embodiment 5) is soaked Dentinal SEM picture after five days and as shown in Figure 3, can be found out that dentinal tubule is fully blocked; Use the artificial saliva being dispersed with the present invention dual anti-dentin hypersensitiveness compositions to soak after five days to scheme as shown in Figure 4 at the SEM of the apatite layer of dentin surface's formation, can find out, apatite layer thickness reaches 5 μm; Through the Dentinal tooth of the present invention dual anti-dentin hypersensitiveness compositions, repairs, every day schemes as shown in Figure 5 with the dentin SEM of the laughable 5min of immersion, imitation chemical stimulation in continuous five days, toothbrush grooming 20 imitation physical stimulations, can find out, dentinal tubule is still fully blocked.
2, to after lactic acid demineralization, without the adamantine repairing effect repaired
Test method is:
(1) enamel specimen preparation: sample tooth is through removing adhering tissue, and with cutting machine, tooth cutting adult tooth is indulged portion's specimen, sterilization and ultrasonic cleaning, select flawless glaze paint to be trial zone, 600# sand paper polishes, and is coated with nial polish outside trial zone;
(2) artificial caries glaze preparation: 8 are put in adamantine tooth specimen and soak 12h in lactic acid demineralization liquid and prepare artificial caries glaze, then with purified water cleaning, surface sweeping electron microscopic observation;
(3) tooth application is simulated: get 4, artificial caries glaze at random and be soaked in artificial saliva, sooner or later use toothpaste sample (the present invention dual anti-dentin hypersensitiveness compositions prepared by embodiment 5) 1cm after taking out every day on toothbrush, get wet the tooth 2min that brushes teeth, then 50ml purified water is added by tooth to conical flask, be put in jolting 3min in 37 DEG C of thermostatic water bath, purified water is dipped in artificial saliva after rinsing again, so repeatedly, remineralization is after one week, scanning electron microscopic observation.
After lactic acid demineralization, without repair enamel surface SEM picture as shown in Figure 6; Use the mastic simulation toothpaste being dispersed with the present invention dual anti-dentin hypersensitiveness compositions to brush teeth process to tooth after demineralization, after using one week continuously, adamantine SEM picture as shown in Figure 7, can find out, enamel surface formation apatite layer.
Compare summary according to SEM figure can draw; damaged tooth is after the present invention dual anti-dentin hypersensitiveness compositions-treated; dentinal tubule is blocked; and define new enamel; after daily chemistry, physical stimulation, still there is thicker apatite layer; illustrate that formed dentium nitor face is wear-resisting, corrosion resisting property good, not only effectively can treat dentin hypersensitiveness's reaction, and make tooth obtain strengthening.
What this description of test mixed titanium bioactive glass lures osteogenesis characteristic good.Here, bioactivity glass plays and mainly lures osteogenesis effect, and titanium is doped chemical, is luring osteogenesis to play assosting effect on, and what it mainly improved is that the osseous tissue that bioactivity glass is repaired is firm wear-resisting, and does not affect biocompatibility; And the use of titanium is low compared with the cost of strontium, good stability.
Claims (10)
1. a dual anti-dentin hypersensitiveness compositions, its effective ingredient is account for the potassium salt of composition weight percentage ratio 0.3%-12% and the titaniferous bioactivity glass of 0.5%-15%; Described potassium salt is one or more in the potassium chloride of the provided potassium ion source dissolving in glycerol or water, potassium citrate, potassium oxalate, dipotassium hydrogen phosphate, potassium dihydrogen phosphate and potassium bicarbonate; Described titaniferous bioactivity glass is particulate bioactive glass, and particle diameter is less than 100 μm, with mass ratio range, wherein containing following glass ingredient:
Described bioactivity glass can be prepared by sol-gel process, high-temperature fusion sintering process or hydro-thermal method:
The concrete steps that described sol-gel process prepares bioactivity glass are: take dust technology as catalyst, by the alcoholic solution of raw material ethyl orthosilicate corresponding for glass ingredient, the alcoholic solution of triethyl phosphate, lime nitrate alcoholic solution, Chile saltpeter Ludox, butyl titanate alcoholic solution is feeding respectively, add reaction vessel successively under agitation, after stirring 90min, wet gel is obtained after rising to 40 DEG C of precipitation 24h-72h by room temperature, sieve after dry 12h-48h at 60 DEG C-100 DEG C again, siftage is put into Muffle furnace 600 DEG C-750 DEG C sintering 4h and is obtained the bioactive glass powder that particle diameter is less than 100 μm,
The concrete steps that described high-temperature fusion sintering process prepares bioactivity glass are: by feed oxygen SiClx corresponding for glass ingredient, calcium carbonate, sodium phosphate, sodium carbonate, sodium titanate powder feeding, dry after putting into ball mill wet grinding, put into corundum crucible, then melting in 1200 DEG C-1450 DEG C in Muffle furnace, shrend in distilled water after insulation 2h, ball mill pulverizing after the drying of shrend formation, sieving obtains the bioactive glass powder that particle diameter is less than 100 μm;
The concrete steps that described hydro-thermal method prepares bioactivity glass are: first by feed oxygen SiClx corresponding for glass ingredient, calcium carbonate, sodium phosphate, sodium carbonate, sodium titanate feeding, be put in ball milling 5h-10h in ball mill, on hydraulic press, block or cylinder is pressed into after drying and screening, then the powder body after compacting is put in high-pressure hydrothermal reaction kettle, after 180 DEG C of-250 DEG C of hydrothermal treatment consists 24h-72h, screens the bioactive glass powder that particle diameter is less than 100 μm.
2. compositions according to claim 1, is characterized in that: after described bioactivity glass and water or physiological solution are had an effect, can generate hydroxyapatite, in infrared spectrogram, demonstrate the characteristic peak of hydroxyapatite, wave number is at 602 ± 5cm
-1with 560 ± 5cm
-1the reflection peak at place.
3. compositions according to claim 1 and 2, is characterized in that: described dual anti-dentin hypersensitiveness compositions can be unguentum, paste, gel, solution, membrane or powder.
4. compositions according to claim 3, is characterized in that: can also comprise one or more in abrasivus, surfactant, sweeting agent, spice, thickening agent, adhesive, antiseptic and wetting agent etc. in described dual anti-dentin hypersensitiveness compositions:
Described abrasivus is the mixture of one or more in calcium phosphate, calcium carbonate, calcium pyrophosphate, aluminium hydroxide, silicon oxide, and accounting for composition weight percentage ratio is 10%-16%;
Described surfactant is the mixture of one or more in N-sodium lauroyl sarcosine, sodium lauryl sulphate and dodecylbenzene sodium sulfonate, and accounting for composition weight percentage ratio is 1%-3%;
Described sweeting agent is the mixture of one or more in saccharin sodium, steviosin and xylitol, and accounting for composition weight percentage ratio is 0.1%-1.5%;
Described spice is stay the one in orchid, Herba Menthae, Fructus Citri Limoniae, green tea and Ilicis Purpureae, and accounting for composition weight percentage ratio is 0.5%-1.5%;
Described thickening agent is one or both the mixture in silicon dioxide and aluminium-magnesium silicate, and accounting for composition weight percentage ratio is 5%-10%;
Described adhesive is the mixture of one or more in carbomer, sodium carboxymethyl cellulose, guar gum and carrageenan, and accounting for composition weight percentage ratio is 0.2%-0.4%;
Described antiseptic is one or both the mixture in hydroxy benzoic acid sodium and sodium sulfite, and accounting for composition weight percentage ratio is 0.05%-0.1%;
Described wetting agent is the mixture of one or more in glycerol, Polyethylene Glycol, sorbitol and propylene glycol, and accounting for composition weight percentage ratio is 55%-70%.
5. compositions according to claim 4, is characterized in that: described abrasivus is the mixture of one or more in silicon oxide or silicon oxide and calcium phosphate, calcium carbonate, calcium pyrophosphate and aluminium hydroxide.
6. compositions according to claim 4, is characterized in that: described adhesive is the mixture of one or more in carbomer or carbomer and sodium carboxymethyl cellulose, guar gum and carrageenan.
7. prepare a method for claim 4-6 arbitrary described dual anti-dentin hypersensitiveness compositions, comprise the following steps:
1) take raw material by formula, under rapid stirring, abrasivus, bioactive glass powder, potassium salt, sweeting agent, thickening agent, adhesive, antiseptic, surfactant are pre-dispersed in wetting agent respectively;
2) under the condition of vacuum, rapid stirring, according to a definite sequence by step 1) scattered abrasivus, bioactive glass powder, potassium salt, sweeting agent, thickening agent, adhesive, antiseptic, surfactant mix homogeneously, and rapid stirring;
3) add spice under low rate mixing condition, leave standstill, obtain dual dentin hypersensitiveness compositions.
8. preparation method according to claim 7, is characterized in that: described step 2) in the rapid stirring time be 0.5h-1h; Described step 3) in time of repose be 10min-2h.
9. preparation method according to claim 8, is characterized in that: described step 3) in time of repose be 0.5h.
10. described in any one of claim 1-6, dual anti-dentin hypersensitiveness compositions is preparing the application in Related product; Related product is:
For the pharmaceutical composition of anti-dentin hypersensitiveness;
For preventing or treat the pharmaceutical composition of teeth corrosion, gingival hemorrhage; Or
For the product of dental care or oral hygiene.
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| CN109044863A (en) * | 2018-10-31 | 2018-12-21 | 四川涑爽医疗用品有限公司 | A kind of antiallergy photocatalyst beautifying and whitening toothpaste and preparation method thereof |
| CN110101899A (en) * | 2019-04-10 | 2019-08-09 | 湖北中部医疗科技有限公司 | A kind of medical use hydrocolloid dressing and preparation method thereof |
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