CN104398390B - Silane coupling agent and its method are rinsed in dentine primary coat - Google Patents
Silane coupling agent and its method are rinsed in dentine primary coat Download PDFInfo
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- CN104398390B CN104398390B CN201410679144.4A CN201410679144A CN104398390B CN 104398390 B CN104398390 B CN 104398390B CN 201410679144 A CN201410679144 A CN 201410679144A CN 104398390 B CN104398390 B CN 104398390B
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- dentine
- silane coupling
- coupling agent
- primary coat
- flushing
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- 210000004268 dentin Anatomy 0.000 title claims abstract description 69
- 239000006087 Silane Coupling Agent Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000178 monomer Substances 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 230000001070 adhesive effect Effects 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 13
- 239000000853 adhesive Substances 0.000 claims abstract description 12
- 238000005115 demineralization Methods 0.000 claims abstract description 12
- 230000002328 demineralizing effect Effects 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims abstract description 9
- 238000011010 flushing procedure Methods 0.000 claims description 16
- 108010035532 Collagen Proteins 0.000 claims description 13
- 102000008186 Collagen Human genes 0.000 claims description 13
- 229920001436 collagen Polymers 0.000 claims description 13
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 229920002554 vinyl polymer Polymers 0.000 claims description 4
- VZRRCQOUNSHSGB-UHFFFAOYSA-N 4-hydroxy-4,6,6-trimethylbicyclo[3.1.1]heptan-3-one Chemical compound C1C2C(C)(C)C1CC(=O)C2(O)C VZRRCQOUNSHSGB-UHFFFAOYSA-N 0.000 claims description 3
- VTODXXLTALDBOX-UHFFFAOYSA-N CC(=C)C(=O)OCCCCCCCCCCCCCP(=O)(O)O Chemical group CC(=C)C(=O)OCCCCCCCCCCCCCP(=O)(O)O VTODXXLTALDBOX-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- GHXZTYHSJHQHIJ-UHFFFAOYSA-N Chlorhexidine Chemical compound C=1C=C(Cl)C=CC=1NC(N)=NC(N)=NCCCCCCN=C(N)N=C(N)NC1=CC=C(Cl)C=C1 GHXZTYHSJHQHIJ-UHFFFAOYSA-N 0.000 claims description 2
- 102000005741 Metalloproteases Human genes 0.000 claims description 2
- 108010006035 Metalloproteases Proteins 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 229960003260 chlorhexidine Drugs 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 claims description 2
- 229960000686 benzalkonium chloride Drugs 0.000 claims 1
- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical compound [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-UHFFFAOYSA-N 0.000 claims 1
- 229940125532 enzyme inhibitor Drugs 0.000 claims 1
- 239000002532 enzyme inhibitor Substances 0.000 claims 1
- 238000005530 etching Methods 0.000 abstract description 6
- 230000002688 persistence Effects 0.000 abstract description 5
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 3
- 230000036541 health Effects 0.000 abstract description 3
- 230000002378 acidificating effect Effects 0.000 abstract description 2
- 238000004026 adhesive bonding Methods 0.000 abstract 1
- 239000011347 resin Substances 0.000 description 13
- 229920005989 resin Polymers 0.000 description 13
- 102000002274 Matrix Metalloproteinases Human genes 0.000 description 9
- 108010000684 Matrix Metalloproteinases Proteins 0.000 description 9
- 239000000835 fiber Substances 0.000 description 8
- 239000007767 bonding agent Substances 0.000 description 7
- 239000004744 fabric Substances 0.000 description 6
- CFKBCVIYTWDYRP-UHFFFAOYSA-N 10-phosphonooxydecyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCCCCCCCCOP(O)(O)=O CFKBCVIYTWDYRP-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 159000000007 calcium salts Chemical class 0.000 description 4
- 238000000016 photochemical curing Methods 0.000 description 4
- 102000035195 Peptidases Human genes 0.000 description 3
- 108091005804 Peptidases Proteins 0.000 description 3
- 239000004365 Protease Substances 0.000 description 3
- 239000002810 dentin bonding agent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 2
- 102000005600 Cathepsins Human genes 0.000 description 2
- 108010084457 Cathepsins Proteins 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 description 2
- 235000018417 cysteine Nutrition 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- 210000000214 mouth Anatomy 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 150000003839 salts Chemical group 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- -1 10- methacryloxypropyl decylphosphonic acid esters Chemical class 0.000 description 1
- 208000010392 Bone Fractures Diseases 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 102100026735 Coagulation factor VIII Human genes 0.000 description 1
- 102000010834 Extracellular Matrix Proteins Human genes 0.000 description 1
- 108010037362 Extracellular Matrix Proteins Proteins 0.000 description 1
- 206010017076 Fracture Diseases 0.000 description 1
- 101000911390 Homo sapiens Coagulation factor VIII Proteins 0.000 description 1
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 description 1
- 208000003941 Impacted Tooth Diseases 0.000 description 1
- 229940122014 Lyase inhibitor Drugs 0.000 description 1
- 102000002151 Microfilament Proteins Human genes 0.000 description 1
- 108010040897 Microfilament Proteins Proteins 0.000 description 1
- 108010077465 Tropocollagen Proteins 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000002723 alicyclic group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229930014669 anthocyanidin Natural products 0.000 description 1
- 150000001452 anthocyanidin derivatives Chemical class 0.000 description 1
- 235000008758 anthocyanidins Nutrition 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- ANFBUVUHZHKENQ-UHFFFAOYSA-N benzene;chloroamine Chemical class ClN.C1=CC=CC=C1 ANFBUVUHZHKENQ-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 208000002925 dental caries Diseases 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000016674 enamel mineralization Effects 0.000 description 1
- 210000002744 extracellular matrix Anatomy 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
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- 238000001764 infiltration Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000002697 lyase inhibitor Substances 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 210000001724 microfibril Anatomy 0.000 description 1
- 210000003632 microfilament Anatomy 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 238000000352 supercritical drying Methods 0.000 description 1
- 210000004357 third molar Anatomy 0.000 description 1
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- 230000010148 water-pollination Effects 0.000 description 1
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- 229910052725 zinc Inorganic materials 0.000 description 1
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- Dental Preparations (AREA)
Abstract
The present invention provides a kind of dentine primary coat and rinses silane coupling agent and its method, described dentine silane coupling agent is the situation that defect of teeth is repaired for the department of stomatology, pretreatment dentin surface is rinsed into the primary coat of dentine silane coupling agent, reapply Self-etching bond agent vertex-gluing graph body and dentine, department of stomatology primary coat rinses dentine silane coupling agent containing 60% 99.4% alcohol water blend, 0.5% 30% faintly acid function monomer and 0.1% 10% NMPIs.Make the slight demineralization of dentine containing weakly acidic 10 MDP；NMPI reduces the degraded of collagenous fibres；The method pretreatment dentine rinsed simultaneously with primary coat; the MDP Ca of generation are made more firmly to be engaged in hydroxyapatite; tooth adhesive strength can further be improved and persistence is bonded; the engagement of tooth and direct or indirect dummy is set more firmly, persistently, preferably to protect the health of tooth body residue tissue.
Description
Technical field
The present invention relates in department of stomatology field, more particularly to a class dentine primary coat-flushing silane coupling agent (primer) and
Its method (etch-＆-rinse approach).For by department of stomatology dummy for example high-molecular organic material, ceramics, metal or
Other composites, are directly or indirectly adhered to the tooth of defect.
Background technology
With social economy, the sustainable development of culture, the aesthetic standards of people are also constantly being improved, and countries in the world are to tooth
Input in terms of tooth beauty and health is also more and more.The main content of dental prosthetics reparation is direct resin fill reparation
With indirect resin bonding reparation, and these restorative procedures all refer to the bonding to a key problem, i.e. dentine.Nearly 20
Nian Lai, dentin bonding agent and adhesive technology are rapidly developing, and the adhesive effect of dentine is significantly increased.But, bonding
Process is complicated physics, a chemical process, depends not only on the structure or state of bonding agent and bonding interface, binding agent with
The process for treating surface of bonding plane, moreover, the particularity of internal environment of oral cavity for example temperature change, high humility, microorganism, protease and
The degraded of the degraded and bonding agent of the collagen of exposure in itself has all severely impacted tooth sheet in bite stress, and dentine
Matter adhesive strength and persistence.
Solvent of the water usually as most of dentin bonding agents.In order to Dentin bonding have preferably wetting and/
Or acid etching dentin surface ability, increase the concentration of hydrophilic ion exchange resin monomer in bonding agent.Due to it is hydrophilic from
Subtree alicyclic monomer promotes the absorption of moisture, more not volatile in bonding agent intermediate ion resin monomer concentration more high-moisture.Water
Divide the plasticizing be detained and not only increase polymer（plasticization）, and cause polymer mechanical performance reduction and
The reduction of the adhesive strength of resin-dentine.In addition, hydrophily dentin bonding agent is also easily by moisture in dentinal tubule
The influence of infiltration, moreover, hydrophilic ion exchange resin monomer contains ester bond, compared with facile hydrolysis.
Calculate by volume, dentine is made up of 50% inorganic matter, 30% collagenous fibres and 20% water.The nothing of dentine
Machine thing can be divided into the outer inorganic matter of fiber（To separate collagenous fiber bundle）With inorganic matter in fiber（In tropocollagen molecule fiber
Gap）.In dentinal fibers after inorganic matter demineralization, collagenous fibres microfilament（microfibril）Interior gap about 1.26-1.33
Nm, and the nm of functional monomer molecule such as HEMA about 2.2 minimum in bonding agent.Thus the functional monomer molecule in bonding agent
Stereochemical structure prevent it from infiltrating through the space that demineralization in fiber is produced completely.These spaces can be filled by water or hydrolysising protease
It is full, thus these collagenous fibres are easily hydrolyzed.The maximum difficulty of dentine adhesive technology is exactly that resin monomer can not be complete
The gap infiltrated through in the collagenous fibres produced by demineralization, causes resin monomer to be easily trapped in the top layer of mixed layer.So
Dentine bonding interface less stable, the early fracture being easily caused.
During present department of stomatology defect of teeth bonding, acid etching-flushing class used or from acid etching class adhesive system can be made
The release of calcium ion into dentine, so as to activate the matrix metalloproteinase (matrix in dentine
Metalloproteinases, MMPs), MMPs is one group of zinc/Ca-dependent protease, and drop can be played in neutral conditions
Solve the effect of extracellular matrix[4], so as to cause to be bonded the degraded of mixed layer collagenous fibres, it is lasting that influence dentine is bonded
Property[5]。
We are in the research of early stage it has also been found that Main Ingredients and Appearance phosphate in Self-etching bond agent can be main with tooth
Constituent hydroxyapatite or enamel formation soluble calcium salt and slightly solubility calcium salt [6], still, these soluble calcium
Salt can reduce the adhesive strength of enamel [7]。
1.Bertassoni LE, Stankoska K, Swain MV. Insights into the structure
and composition of the peritubular dentin organic matrix and the lamina
limitans [J]. Micron, 2012, 43: 229-236.
2.Liu Y, Tjäderhane L , Breschi L, Mazzoni A, Li N, Mao J, Pashley
DH, Tay FR.. Limitations in bonding to dentin and experimental strategies to
prevent bond degradation[J]. J Dent Res 2011, 90: 953-968.
3.Brackett MG, Li N, Brackett, WW, Sword, RJ, Qi YP, Niu LN, Pucci
CR,Dib A,Pashley DH, Tay FR.. The critical barrier to progress in dentine
bonding with the etch-and-rinse technique[J]. J Dent 2011, 39: 238-248.
4.Pashley DH, Tay FR, Yiu C, et al. Collagen degradation by host-
derived enzymes during aging. J Dent Res, 2004, 83:216-222
5.Martin-De Las Heras S, Valenzuela A, Overall CM. The matrix
metalloproteinase gelatinase A in human dentine. Arch Oral Biol, 2000, 45:
757-765.
6.Fu B*, Sun X, Qian W, Shen Y, Chen R, Hannig M. Evidence of Chemical
bonding to hydroxyapatite by phosphoric acid esters. Biomaterials, 2005, 26:
5104-5110.
7.Zhang ZL, Zhang L, Liang B, Tang T, Fu B *, Hannig M. The
Contribution of chemical bonding to the short- and long-term enamel bond
Strengths. Dental Materials 2013,29:e103-e112.
The content of the invention
Problem to be solved by this invention is to provide a kind of dentine primary coat-flushing silane coupling agent and its method, can be effective
Extend the persistence of dentine bonding, so that the service life of remaining dental tissue and its dummy is improved, protection patient oral cavity
The health of tooth.
The solution used to solve the problem of the present invention is as follows：
A kind of dentine primary coat-flushing silane coupling agent includes by mass percentage：60%-99.4% alcohol water blend,
0.5%-30% faintly acid function monomer and 0.1%-10% NMPIs.
The weight ratio of alcohol and water is 1 in described alcohol water blend:1.
Described faintly acid function monomer is 10- methacryloxypropyl decylphosphonic acid esters, makes dentine surface part slight
Demineralization, and collagen fabric silk within and between not demineralization.
Described NMPI be BZK, polyvinyl, OPC, glutaraldehyde or chlorine oneself
One kind in fixed.
The primary coat method of the dentine silane coupling agent is：Described dentine silane coupling agent pretreatment dentin surface 15-
60s, then steam rinses 30s, and is dried up with air gun, then carries out the bonding of dentine, by the phosphoric acid for washing off solubility
Ester-hydroxylapatite compound, strengthens the adhesive strength of dentine.
10- methacryloxypropyl decylphosphonic acid esters（10-MDP）It is a kind of phosphate of function admirable, with hydroxyapatite
（HAp）React the property calcium salt hard to tolerate of generation（MDP-Ca）" nanometer layer " structure is formed, strong adsorption is in HAp surfaces, this feature
Adhesive property can be strengthened.By washing off phosphate-hydroxylapatite compound of solubility, this method can be notable
Strengthen the adhesive strength of dentine, i.e., primary coat-flushing can be used as a kind of new tooth again after primary coat-flushing or acid etching-flushing
Tooth is bonded processing method.
Consider from the active angle for suppressing matrix metalloproteinase, using wide spectrum collagen lyase inhibitor such as Chlorhexidine, benzene
Chloramines etc., or the grafting quaternary amine salt groups on monomer are pricked, so as to suppress MMPs and cysteine cathepsin activity；Using
Collagenous fibres crosslinking agent such as glutaraldehyde, anthocyanidin etc., the degraded of resistance MMPs and cysteine cathepsin to collagen
Effect；So as to reduce the degraded of collagenous fibres, while using polyvinyl（PVPA）, be able to can also not only make to take off with MMPs
There is remineralization in collagenous fibres after ore deposit, strengthen the stability of mixed layer, so as to extend the persistence of dentine bonding.
The beneficial effects of the invention are as follows weakly acidic primary coat-flushing dentine silane coupling agent, by washing except solubility
Phosphate-hydroxylapatite compound, this method can significantly increase the adhesive strength of dentine；And tooth sheet can be made
The slight demineralization of matter surface part, collagen fabric（collagen fibers）It is also residual outside not exclusively exposure, collagen fabric
Stay hydroxyapatite, and within collagen fabric silk and between（intra- and inter-fibrillar collagen）
Not demineralization.So, resin monomer need not be penetrated into collagen fabric silk, so that solving resin monomer in mixed layer can not penetrate into
Problem；Suppress MMPs activity, reduce the degraded of collagenous fibres；And with dentin collagen fiber mineralization potential.
Brief description of the drawings
Fig. 1 schemes for the SEM observations of control group；
Fig. 2 schemes for the SEM observations of embodiment one；
Fig. 3 schemes for the SEM observations of embodiment two；
Fig. 4 schemes for the SEM observations of example IV.
Embodiment
A kind of dentine primary coat-flushing silane coupling agent includes by mass percentage：60%-99.4% alcohol water blend,
0.5%-30% faintly acid function monomer and 0.1%-10% NMPIs.
The weight ratio of alcohol and water is 1 in described alcohol water blend:1.
Described faintly acid function monomer is 10- methacryloxypropyl decylphosphonic acid esters, makes dentine surface part slight
Demineralization, and collagen fabric silk within and between not demineralization.
Described NMPI be BZK, polyvinyl, OPC, glutaraldehyde or chlorine oneself
One kind in fixed.
The primary coat method of the dentine silane coupling agent is：Described dentine silane coupling agent pretreatment dentin surface 15-
60s, then steam rinses 30s, and is dried up with air gun, then carries out the bonding of dentine, by the phosphoric acid for washing off solubility
Ester-hydroxylapatite compound, strengthens the adhesive strength of dentine.
Silane coupling agent is used for before the processing of dentine bonding, the pretreatment for dentine.Use alcohol water blend（1:1w/
w）Different dentine silane coupling agents are prepared, wherein 10-MDP concentration is 0.5%-30%wt, and BAC concentration is 0.5-2%wt, and PVPA is
500-3000 μ g/ml, are configured to MDP and various concentrations that MMPs inhibitor is combined into, the wine of different dentine pretreatment times
The smart aqueous solution, such as MDP-BAC alcohol water blends, MDP-PVPA alcohol water blends, MDP- OPC alcohol water blends, by difference
Experimental group silane coupling agent be coated on dentin surface, after pretreatment dentine 15-60 s, steam rinses 30s, air gun drying.Again
Carry out the bonding of dentine.
Embodiment one
Alcohol 47.5%
Water 47.5%
10-MDP 5%
Embodiment two
Alcohol 47%
Water 47%
10-MDP 5%wt
BAC 1%wt
Embodiment three
Alcohol 47.5%
Water 47.5%
10-MDP 5% wt
PVPA 1000μg/ml
Effect observation
Micro-stretching strength test (μ TBS)：First flawless, N/D before experiment, without the bad people's third molar of dental caries in 37 °C of water
In bath after 24 hours, under flowing water, it will be perpendicular to cut at 1/3 in corona major axis hat with low speed slicer, 1/3 in exposure hat
Dentine, polished with 320#SiC on grinding and polishing apparatus after 30 s, it is stand-by with the s of distilled water flushing 30.Control group：Will be from acid etching
Bonding agent Clearfil S3 Bond are applied to after dentin surface 20s, and more than 5s, the s of photocuring 10 are blown by force, with compound resin point
Layer filling, per the mm of thickness degree 1, totally 4 layers, each photocuring 20s.Silane coupling agent group：Different dentine silane coupling agents is coated on tooth
Essential surface, stands after 30 s, and steam rinses 30s, air gun drying, then illustratively uses corresponding Self-etching bond agent Clearfil
S3 Bond are applied to dentin surface 20s, and more than 5s, the s of photocuring 10 are blown by force, compound resin slicing and filling is used, per thickness degree about 1
Mm, totally 4 layers, each s of photocuring 20.Under flowing water, sample is cut into about 1*1* perpendicular to bonding plane using cutting device at a slow speed
8mm dentine resin streaks.Then micro-stretching experiment is carried out using micro-stretching test instrument, draw speed is 1 mm/min.Use vernier
The length and width of kind of calliper dentine resin sliver transvers section, calculates bonding plane area.Micro-stretching intensity (μ TBS) uses MPa
Calculate（Fig. 1）.Residual resin dentine bar is stored in 37 DEG C of running water and stored, and a running water is changed weekly, in after 6 months
Micro-stretching strength test is carried out again.
Table 1
By the numerical value of table 1, the micro-stretching intensity behind embodiment one~3 6 month and 24 hours micro-stretching intensity at once are found
Numerical value is compared nothing and significantly sexually revised, and the control group of dentine silane coupling agent is not used, and micro-stretching strength values drop after 6 months
It is low substantially, it is seen then that the adhesion durability of embodiment one~tri- is good, and uses the embodiment one~tri- after silane coupling agent at once 24
Hour micro-stretching intensity is improved.
Scanning electron microscopic observation resin dentine mixed layer situation
Isolated Tooth cuts control group and silane coupling agent group after resin-dentine bar with above-mentioned processing, in 0.1mol/l salt
2s is handled in acid solution, 30s is rinsed, glutaraldehyde is fixed, alcohol series dehydration, critical point drying sprays to be observed with SEM after platinum and set
Fat-dentine interface conditions.Another part resin-dentine bar carries out SEM observations after 6 months again with above-mentioned storage.
Complete from the visible 24h groups dentine mixed layers of Fig. 1-Fig. 4, engagement is close, control group SEM again after 6 months
Observation resin-dentin interface has obvious crackle, and the resin-dentin interface of embodiment one~tri- is continuous whole, has no obvious
Crackle, has good bonding persistence compared with control group.
Claims (4)
1. a kind of dentine primary coat-flushing silane coupling agent, it is characterised in that by mass percentage by 60%-99.4% alcohol
The aqueous solution, 0.5%-30% faintly acid function monomer and 0.1%-10% NMPIs composition；Described
Faintly acid function monomer is 10- methacryloxypropyl decylphosphonic acid esters, makes the slight demineralization of dentine surface part, and collagen
Within filament and between not demineralization.
2. dentine primary coat-flushing silane coupling agent according to claim 1, it is characterised in that in described alcohol water blend
The weight ratio of alcohol and water is 1:1.
3. dentine primary coat-flushing silane coupling agent according to claim 1, it is characterised in that described matrix metalloprotease
Enzyme inhibitor is one kind in benzalkonium chloride, polyvinyl, OPC, glutaraldehyde or Chlorhexidine.
4. a kind of non-treatment purpose primary coat method of dentine primary coat-flushing silane coupling agent as claimed in claim 1, its feature exists
In:Described dentine primary coat-flushing silane coupling agent pretreatment dentin surface 15-60s, then steam rinses 30s, and uses air gun
Drying, by washing off phosphate-hydroxylapatite compound of solubility, strengthens the adhesive strength of dentine.
Priority Applications (1)
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| CN105342863B (en) * | 2015-12-11 | 2018-08-24 | 张凌 | Application of the epigallocatechin gallic acid fat in terms of improving dental resin adhesives reparation |
| CN106074182B (en) * | 2016-06-22 | 2019-02-26 | 何正娣 | A kind of laser preparation dentine dual liquid type Self-etching bond composition |
| EP3484435A1 (en) * | 2016-07-14 | 2019-05-22 | Unilever N.V. | Oral care composition comprising composite particles containing cationic germicide |
| CN107374979A (en) * | 2017-07-05 | 2017-11-24 | 浙江大学 | Purposes and captopril Dentin bonding of the angiotensin converting enzyme inhibitors such as captopril on Dentin adhensive |
| CN112494340B (en) * | 2020-11-02 | 2021-12-10 | 浙江大学 | Dental bonding pretreatment material and application |
| CN115300398B (en) * | 2022-08-10 | 2024-04-26 | 北京大学口腔医学院 | Method for promoting demineralization of dentin |
| CN115463037B (en) * | 2022-09-02 | 2023-09-22 | 辽宁爱尔创生物材料有限公司 | Dental pretreatment agent composition and preparation method thereof |
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