CN112336634A

CN112336634A - Dentin adhesion pretreatment composition based on microenvironment-induced nanoparticle redeposition and application

Info

Publication number: CN112336634A
Application number: CN202011203081.7A
Authority: CN
Inventors: 李晓东; 罗巧洁; 舒畅; 许佳佳
Original assignee: Zhejiang University ZJU
Current assignee: Zhejiang University ZJU
Priority date: 2020-11-02
Filing date: 2020-11-02
Publication date: 2021-02-09
Anticipated expiration: 2040-11-02
Also published as: WO2022088520A1; CN112336634B

Abstract

The invention provides a dentin adhesion pretreatment composition based on microenvironment induced nanoparticle redeposition, which comprises a binary system or a ternary system, and is applied after dentin acid etching treatment and before an adhesive is used. The bonding pretreatment agent can rapidly form a large amount of ACP nano particles at polar sites of the demineralized dentin matrix under the induction of a natural mineralization environment formed by the demineralized dentin matrix after acid etching, and the chemically combined inorganic nano particles mask the polarity of the demineralized dentin matrix, eliminate the hydration capability of dentin organic matters and improve the compatibility of a demineralized dentin matrix phase and an adhesive phase of a bonding interface; the mechanical strength of the adhesive is improved, collapse caused by water volatilization is resisted, the dependence on water during dentin adhesion is eliminated, the sensitivity of clinical adhesion operation and instability of a mixed layer caused by water residue are reduced, and the adhesive can be prepared into a novel dental adhesion pretreatment agent and is suitable for all adhesive occasions in oral cavities.

Description

Dentin adhesion pretreatment composition based on microenvironment-induced nanoparticle redeposition and application

Technical Field

The invention belongs to the technical field of dental materials, and relates to a dentin adhesion pretreatment composition based on microenvironment induced nanoparticle redeposition and application thereof.

Technical Field

Dental defects caused by various reasons are the most common oral diseases in clinic. Due to the irreproducibility of enamel and the limited nature of dentin self-repair, reconstructed tooth tissues can be recovered only by artificial materials at present, and the functions of chewing, speaking, beauty and the like of the tooth tissues are recovered. The artificial material and the tooth tissue are bonded by the adhesive, and the performance of the bonding interface is relevant to the life span of the prosthesis.

Dentin is a composite structure mineralized on an organic matter scaffold mainly made of collagen, and the organic matter content of the dentin is 20%. The complex structure determines the complexity of the dentin bonding. During dentinogenesis, non-collagenous proteins (NCPs) secreted by odontoblasts, as well as Metal Matrix Proteases (MMPS) and other enzymes play an important role. NCPs can play an important regulatory role in the mineralization of dentin by binding to collagen fibers and affect the rate of apatite deposition and the appearance of its crystals. NCPs contain carboxyl and phosphate functional groups, have a large negative charge, and are capable of binding Ca²⁺、PO₄ ^3－Forming nuclei and further inducing a subsequent apatite crystal mineralization process. However, the nature of the non-collagenous protein determines that it becomes a disadvantage in the binding process. The hydration capability of the NCPs enables gel structures to be formed in the bonding process, and the infiltration and distribution of key bonding monomers in the bonding agent are seriously influenced, so that the bonding durability is further influenced. In addition, the strong water-binding ability of the adhesive makes water difficult to replace by an adhesive solvent in the bonding process, so that the mixed layer has high water content and many defects, and the stability of the mixed layer is not facilitated.

The demineralized dentin matrix is a natural mineralized environment, the natural mineralized environment is utilized to rapidly induce the formation of ACP nano particles, and the nano particles are chemically combined with the demineralized dentin matrix, so that the charge in the microenvironment of the demineralized dentin matrix can be covered, the hydration capability of NCPs is eliminated, and the demineralized dentin matrix is converted into a novel three-dimensional organic-inorganic hybrid structure. The hydration capability of demineralized dentin organic matters after biomimetic mineralization is greatly weakened, the specific surface area is increased, the residual moisture of the interface is reduced, the interface compatibility with key bonding monomers of the bonding agent is improved, and the infiltration and the uniform distribution of the bonding agent are facilitated; free water in the dentin collagen matrix and water molecules which are not tightly combined are replaced, so that a hybrid layer with fewer defects is formed; the mechanical strength of the demineralized dentin is improved, and collapse caused by water volatilization can be resisted, so that the dependence of the existing wet bonding technology on water is eliminated during dentin bonding; in addition, the improvement of mechanical strength reduces the strength difference between the composite phases of the mixed layer, reduces stress concentration and is also beneficial to the stability of a bonding interface and the durability of bonding; is applicable to all the existing dental adhesives.

Disclosure of Invention

The invention aims to provide a dentin adhesion pretreatment composition based on microenvironment-induced nanoparticle redeposition assistance, which comprises a binary system or a ternary system.

The binary system consists of two solutions, namely a solution A and a solution B, wherein the ratio of the solution A: calcium salt solution; solution B: a phosphate solution.

In the binary system, solution A and solution B are stored separately before use.

In the binary system, the solution A and the solution B can be respectively buffered by buffer solution, the pH of the solution is 5.0-9.0, and the buffer solution comprises but is not limited to Tris-HCl, Hepes and the like.

In the binary system, the solution A is soluble calcium salt, including but not limited to calcium chloride solution or calcium nitrate solution or a mixed solution of the two, and the calcium ion concentration in the solution A is 0.01 mM-1M, preferably, the calcium ion concentration is 1 mM-500 mM.

In the binary system, the solution B is soluble phosphate, monohydrogen phosphate or dihydrogen phosphate, including but not limited to lithium phosphate, lithium monohydrogen phosphate, lithium dihydrogen phosphate, sodium monohydrogen phosphate, sodium dihydrogen phosphate, potassium monohydrogen phosphate, potassium dihydrogen phosphate solution, ammonium phosphate, monoammonium phosphate, diammonium phosphate, or a mixture of two or more thereof, the total concentration of hydrogen phosphate and dihydrogen phosphate in the solution is 0.01 mM-1M, preferably 1 mM-500 mM.

In a binary system, the molar concentration ratio of the calcium ion concentration in the solution A to the total concentration of the phosphate radical, the hydrogen phosphate radical and the dihydrogen phosphate radical in the solution B is 10: 1-1: 10.

in a binary system, the volume ratio of the solution A to the solution B is 10: 1-1: 10 and mixing and using immediately after mixing.

In the dental adhesion pretreatment composition of the present invention, one or more functional substances such as antibacterial and enzyme inhibitor, including but not limited to sodium fluoride, chlorhexidine, polyhexamethylene biguanide or a salt thereof, captopril, etc., may be optionally added to the solution B without affecting the formation of calcium phosphate salt precipitates, and the concentration thereof is 0.001mM to 1M.

The ternary system consists of three solutions, namely a solution A, a solution B and a solution C, wherein the solution A is as follows: calcium salt solution; solution B: a phosphate solution; solution C: an organic monomeric reagent that can be chemisorbed to the insoluble calcium phosphate salt.

In the ternary system, the solution A, the solution B and the solution C are independently stored before use.

In the ternary system, the range of the solution A is consistent with that of the solution A in the binary system, and the range of the solution B is consistent with that of the solution B in the binary system.

In the ternary system, the solution A and the solution B can be respectively buffered by buffer solutions, the pH of the solution is 5.0-9.0, and the solution comprises but is not limited to Tris-HCl, Hepes and other buffer solutions.

In the ternary system, solution C is an organic monomer reagent solution which can be chemically adsorbed on insoluble calcium phosphate salt, the organic monomer reagent comprises but is not limited to one or more selected from 10-methacryloyloxydecyl phosphate (10-MDP), 2,4, 6-trimethylphenyl 2- [4- (dihydroxyphosphoric acid) -2-oxabutyl ] acrylate (MAEPA), ethyl 2- [4- (dihydroxyphosphoryl) -2-oxabutyl ] acrylate (EAEPA), n-dodecyl dihydrogen phosphate, ethyl dihydrogen phosphate, 4-methacryloyloxyethyl trimellitic acid (4-MET), 4-methacryloyloxytrimellitic anhydride (4-META), and the solvent in solution C can be water, ethanol, acetone or a mixture of the solvents, the concentration of the organic monomer reagent is 0.001 mM-10M.

It is another object of the present invention to provide the use of the dentin adhesion pre-treatment composition based on microenvironment-induced re-deposition of nanoparticles for the preparation of a dental adhesion pre-treatment agent.

The use of the dental adhesion pretreating agent prepared by the invention is realized by the following scheme: the dental adhesion pretreatment agent is applied to the surface of a clinical acid-treated tooth body before the adhesive is coated.

Whether a binary system or ternary system pretreatment composition, solution a and solution B are mixed prior to use and applied to the surface of the tooth immediately after mixing.

The time for coating the mixed solution of the solution A and the solution B can be 3 s-10 min, and the preferred coating time is 15 s-1 min.

The mixed solution may be repeatedly applied several times. The number of coating times may be 1 to 10, and preferably 1 to 3.

The ternary system dental adhesion pretreatment composition is characterized in that the solution A and the solution B are mixed and coated on the surface of a tooth body, and then the tooth body is washed by water vapor and then coated with the solution C.

The solution C can be applied for 3s to 1min, preferably for 5s to 10 s.

Solution C may be applied repeatedly several times. The number of coating times may be 1 to 10, and preferably 1 to 3.

After the binary system or ternary system dental bonding pretreatment composition is used, the surface of a tooth body to be bonded can be kept wet.

After the binary system or ternary system dental adhesion pretreating agent is used, the surface of a tooth body to be coated with the adhesive can be dried.

The binary system or ternary system dental adhesive pretreatment agent is suitable for all dental adhesives.

Through the treatment of the pretreatment agent, ACP nano-particles chemically combined with the demineralized dentin matrix are quickly formed in the demineralized dentin matrix, the hydration capability of dentin organic matters is eliminated, and the interface compatibility of a demineralized dentin matrix phase and an adhesive phase is improved; the mechanical strength of the adhesive is improved to resist the collapse of demineralized dentin matrix caused by water volatilization, thereby getting rid of the dependence on water during dentin adhesion, and reducing the sensitivity of clinical adhesion operation and the instability of a mixed layer caused by water residue.

The dentin bonding pretreatment composition based on microenvironment rapid induction of nanoparticle redeposition is a natural mineralization induction environment formed by demineralized dentin matrix, and is a thermodynamically unstable calcium phosphate precursor solution formed after calcium salt solution and phosphate solution are rapidly induced to be mixed, so that nano ACP particles are rapidly formed in the strongly polar demineralized dentin matrix, and a brand new organic/inorganic hybrid three-dimensional composite structure is formed. The dental bonding is carried out on the three-dimensional composite structure, is suitable for all adhesives in oral cavity, reduces the technical sensitivity of clinical bonding operation, and improves the bonding strength and the bonding durability.

Drawings

FIG. 1 illustrates the absorbance values of two solutions immediately after mixing to between 10 min.

FIG. 2 is a cryo-transmission electron micrograph of the two solutions immediately after mixing and during the time interval of 9 min.

FIG. 3 illustrates the diameter of the nanoparticles formed immediately after mixing the two solutions and between 9 min.

FIG. 4 is a surface topography of samples of examples two to seven observed by scanning electron microscopy.

FIG. 5 is a cross-sectional profile of the second to seventh samples observed by scanning electron microscopy.

Fig. 6 examples two to seven samples cross-section demineralized collagen layer thicknesses.

FIG. 7A nanometer indentor detects the surface hardness of the second, fourth and sixth samples of the example.

FIG. 8 the nanoindenter measures the surface elastic modulus of the second, fourth, and sixth samples of examples.

FIG. 9EDS shows the distribution of calcium and phosphorus in the cross section of the second, fourth and sixth samples.

FIG. 10 Transmission electron microscopy shows the morphology of collagen of examples two, four, and six.

FIG. 11 random optical reconstruction microscope observation of the position relationship between collagen and calcium in examples II, IV and VI.

FIG. 12 the thermogravimetric analyzer examined sixteen-eighteen samples of the examples.

FIG. 13 Infrared Spectrum of example sixteen-eighteen.

FIG. 14 shows the results of Single bond 2 bonding and stretching.

FIG. 15Spectrum bond elongation results.

FIG. 16Single bond 2 microleakage results.

FIG. 17Spectrum microleakage results.

FIG. 18 confocal laser scanning microscope was used to observe the distribution and intensity of Nile red fluorescence in the Single bond 2 mixed layer.

FIG. 19 confocal laser microscopy was used to observe the Nile Red fluorescence distribution and intensity in the Spectrum mixture.

FIG. 20 is a transmission electron microscope observation of the Single bond 2 mixed layer.

FIG. 21 Transmission electron microscope observation of the Spectrum mixed layer.

Detailed Description

The invention is further explained by the accompanying drawings and examples. The embodiments of the present invention are only for better illustrating the features of the present invention, and the present invention is not limited to these embodiments.

Example one

Tris-HCl buffered 9mM CaCl₂And 5.4mM K₂HPO₄Mixing in equal volume.

Example two

After phosphoric acid etching treatment, the surface of the tooth body is washed by water vapor and kept moist.

EXAMPLE III

After phosphoric acid etching treatment, the surface of the tooth body is washed by water vapor and dried by three guns.

Example four

Tris-HCl buffered 9mM CaCl₂And 5.4mM K₂HPO₄Mixing at equal volume, coating onto the tooth surface after phosphoric acid etching for 30s, and keeping wetAnd (6) moistening.

EXAMPLE five

Tris-HCl buffered 9mM CaCl₂And 5.4mM K₂HPO₄Mixing in equal volume, coating on the tooth surface after phosphoric acid etching, coating for 30s, and drying with three guns.

EXAMPLE six

Tris-HCl buffered 9mM CaCl₂And 5.4mM K₂HPO₄Mixing at equal volume, coating onto the tooth surface after phosphoric acid etching for 3min, and keeping wet.

EXAMPLE seven

Tris-HCl buffered 9mM CaCl₂And 5.4mM K₂HPO₄Mixing in equal volume, coating on the tooth surface after phosphoric acid etching for 3min, and drying with three guns.

Example eight

The absorbance of the solution at 450nm was recorded with a spectrophotometer from immediately after mixing to 10min after mixing in example, and as a result, as shown in FIG. 1, the absorbance of the solution increased with time.

Example nine

The observation of the nanoparticles in the solution immediately after mixing and 10min after mixing in the example was recorded by a cryo-transmission electron microscope, and as a result, spherical nanoparticles were formed in the solution from the time of observation, as shown in fig. 2.

Example ten

The analysis of the particle size of the nanoparticles recorded by observation of a cryo-transmission electron microscope shows that the diameter of the nanoparticles in the solution increases with time, and the diameter of the nanoparticles is 40nm to 200nm, as shown in FIG. 3.

Example twelve

The dental samples of examples two to seven were dehydrated according to the preparation method of the scanning electron microscope sample, and the surface morphology was observed by using the scanning electron microscope, as a result, as shown in fig. 4, nanoparticles were formed on the surfaces of the collagen of examples four to seven treated with the pretreatment composition, and the collagen mesh of examples five and seven was fluffy compared with the collagen mesh of example three.

EXAMPLE thirteen

The dental samples of examples two to seven were brittle-broken in liquid nitrogen, dehydrated according to the preparation method of the scanning electron microscope sample, and the cross-sectional morphology was observed using the scanning electron microscope, and as a result, as shown in fig. 5, the collagen meshes of examples two, four, and six were fluffy, and the collagen meshes of examples five and seven were fluffy compared with the collagen mesh of example three. The thickness of the collagen network in the cross-section of the samples of examples two to seven was analyzed, and as a result, as shown in fig. 6, the pretreatment composition treated samples were able to maintain a fluffy three-dimensional network structure in a dry state.

Example fourteen

The tooth samples of examples two, four and six were observed for strength of the sample surface with a nanoindenter, and the collagen mesh hardness (fig. 7) and elastic modulus of the pretreatment composition-treated samples were increased (fig. 8).

Example fifteen

The tooth samples of examples two, four and six were brittle-fractured in liquid nitrogen and dehydrated according to the preparation method of scanning electron microscope samples, and the distribution of calcium and phosphorus elements in the cross section was observed by EDS, and as a result, as shown in fig. 9, the peak of calcium and phosphorus elements was formed on the surface layer of the demineralized dentin matrix in the samples treated with the pretreatment composition.

Example sixteen

The samples of the second, fourth and sixth tooth bodies of example II were prepared according to the transmission specimen, and the collagen morphology was observed by transmission electron microscopy, and the results are shown in FIG. 10.

Example fifteen

Examples two, four, and six tooth samples were labeled with fluorescein to obtain collagen and calcium, respectively, and then placed in imaging buffer for observation under a random optical reconstruction microscope, and the results are shown in fig. 11, which confirmed the co-localization of calcium and collagen.

Example sixteen

Dentin powder was completely demineralized with EDTA.

Example seventeen

Tris-HCl buffered 9mM CaCl₂And 5.4mM K₂HPO₄After mixing in equal volume, the fully demineralized dentin powder was treated for 30 seconds and kept moist.

EXAMPLE eighteen

Tris-HCl buffered 9mM CaCl₂And 5.4mM K₂HPO₄Mixing at equal volume, treating completely demineralized dentin powder for 3min, and keeping wet.

Example nineteen

Examples sixteen-eighteen samples were examined by thermogravimetric analysis and warmed to 1000 c at 10 c/min, resulting in a reduction in bound water for the pretreatment composition treated dentin samples as shown in figure 12.

Example twenty

Example sixteen-eighteen samples were examined by infrared spectroscopy at 4000-650cm^-1The results of the in-region scan are shown in FIG. 13.

Example twenty one

The surfaces of the teeth of the second to fifth examples were coated with Singlebond 2 adhesive, lightly blown for 5 seconds after 20 seconds of coating, irradiated with light from a photo-curing lamp for 20 seconds, and then laminated with resin. Cutting along the direction perpendicular to the bonding interface of the long axis of the tooth body under the flowing water cooling of a slow cutting instrument to prepare a resin-tooth body strip sample with a bonding surface of 1mm multiplied by 1 mm. The resin-dental strips were divided into three portions, one portion was used for immediate micro-stretching experiments, and the other two portions were stored in artificial saliva and subjected to micro-stretching experiments after 3 months and 12 months. And (3) carrying out micro-stretching test on the resin-tooth body sample by using a micro-stretching tester until the sample is broken, and recording the load measured by the micro-stretching tester when the sample is broken. The interfacial width of the sample was measured and the micro tensile strength per unit cross sectional area of the sample was calculated. The results are shown in FIG. 14. The pretreatment composition treatment improves bond strength and bond durability.

Example twenty two

The dental surface of examples two to five was coated with Spectrum adhesive, lightly blown for 5s after 20s coating, irradiated with light from a light curing lamp for 20s, and then resin was layered on the surface. Cutting along the direction perpendicular to the bonding interface of the long axis of the tooth body under the flowing water cooling of a slow cutting instrument to prepare a resin-tooth body strip sample with a bonding surface of 1mm multiplied by 1 mm. The resin-dental strips were divided into three portions, one portion was used for immediate micro-stretching experiments, and the other two portions were stored in artificial saliva and subjected to micro-stretching experiments after 3 months and 12 months. And (3) carrying out micro-tensile test on each group of resin-tooth body samples by using a micro-tensile tester until the samples break, and recording the load measured by the micro-tensile tester when the samples break. The interfacial width of the sample was measured and the micro tensile strength per unit cross sectional area of the sample was calculated. The results are shown in FIG. 15. The pretreatment composition treatment improves bond strength and bond durability.

Example twenty three

The surface of the tooth bodies of the second to fifth examples was coated with Singlebond 2 adhesive, lightly blown for 20 seconds, irradiated with light for 20 seconds by a photo-curing lamp, and then laminated with resin. Cutting along the direction perpendicular to the bonding interface of the long axis of the tooth body under the flowing water cooling of a slow cutting instrument to prepare a resin-tooth body strip sample with a bonding surface of 1mm multiplied by 1 mm. The resin-dental strips were divided into three portions, one portion was used for immediate microleakage testing and the other two were stored in artificial saliva and kept for 3 and 12 months before microleakage testing. After the sample was soaked in the silver ammonia solution for 12 hours, silver ions were reduced with a developing solution. The deposition of silver on the mixed layer was observed with a scanning microscope in the back-scattering mode. The results are shown in fig. 16, where the pretreatment composition treated mixed layer had less silver deposition than the control.

Example twenty-four

The dental surface of examples two to five was coated with Spectrum adhesive, lightly blown for 5s after 20s coating, irradiated with light from a light curing lamp for 20s, and then resin was layered on the surface. Cutting along the direction perpendicular to the bonding interface of the long axis of the tooth body under the flowing water cooling of a slow cutting instrument to prepare a resin-tooth body strip sample with a bonding surface of 1mm multiplied by 1 mm. The resin-dental strips were divided into three portions, one portion was used for immediate microleakage testing and the other two were stored in artificial saliva and kept for 3 and 12 months before microleakage testing. After the sample was soaked in the silver ammonia solution for 12 hours, silver ions were reduced with a developing solution. The deposition of silver on the mixed layer was observed with a scanning microscope in the back-scattering mode. The results are shown in fig. 17, where the pretreatment composition treated mixed layer had less silver deposition than the control.

Example twenty-five

Nile Red was added to the Singlebond 2 adhesive. The surfaces of the teeth of examples two to five were coated with a Singlebond 2 adhesive containing nile red, lightly blown for 20 seconds, and then irradiated with light from a light curing lamp for 20 seconds, and then a layer of resin 1mm thick was stacked on the surface. Cutting along the direction perpendicular to the bonding interface of the long axis of the tooth body under the flowing water cooling of a slow cutting instrument to prepare a resin-tooth body sheet sample with a 1mm thick bonding surface. The fluorescence distribution and intensity in the mixed layer were observed with a confocal laser microscope. The results are shown in FIG. 18. The treatment with the pretreatment agent improves the penetration and uniform distribution of the hydrophobic nile red in the mixture.

Example twenty-six

Nile red was added to the Spectrum adhesive. The tooth surface of the second to fifth examples was coated with a Spectrum adhesive containing Nile Red, lightly blown for 5 seconds after 20 seconds, irradiated with a light curing lamp for 20 seconds, and then a layer of resin 1mm thick was stacked on the surface. Cutting along the direction perpendicular to the bonding interface of the long axis of the tooth body under the flowing water cooling of a slow cutting instrument to prepare a resin-tooth body sheet sample with a 1mm thick bonding surface. The fluorescence distribution and intensity in the mixed layer were observed with a confocal laser microscope. The results are shown in FIG. 19. The treatment with the pretreatment agent improves the penetration and uniform distribution of the hydrophobic nile red in the mixture.

Example twenty-seven

The surface of the tooth bodies of the second to fifth examples was coated with Singlebond 2 adhesive, lightly blown for 20 seconds, irradiated with light for 20 seconds by a photo-curing lamp, and then laminated with resin. Ultrathin sections were prepared according to the transmission electron microscopy article method and observed using a transmission electron microscopy, the results are shown in FIG. 20. The nano particles are among the collagen fibers of the tooth body and intertwine with the organic matrix of the tooth body.

Example twenty-eight

The dental surface of examples two to five was coated with Spectrum adhesive, lightly blown for 5s after 20s coating, irradiated with light from a light curing lamp for 20s, and then resin was layered on the surface. Ultrathin sections were prepared according to the transmission electron microscopy method and observed using a transmission electron microscopy, the results are shown in FIG. 21. The nano particles are among the collagen fibers of the tooth body and intertwine with the organic matrix of the tooth body.

Example twenty-nine

Tris-HCl buffered 9mM CaCl₂And Tris-HCl buffered 5.4mM K₂HPO₄Mixing at equal volume, coating onto the tooth surface after phosphoric acid etching, coating for 10min, keeping wet, and coating dental adhesive for bonding.

Example thirty

Tris-HCl buffered 9mM CaCl₂And Tris-HCl buffered 5.4mM K₂HPO₄Mixing in equal volume, coating onto the tooth surface after phosphoric acid etching for 10min, blow-drying with three guns, and coating dental adhesive for bonding.

Example thirty one

Tris-HCl buffered 9mM CaCl₂And Tris-HCl buffered 5.4mM K₂HPO₄Mixing at equal volume, coating onto the tooth surface after phosphoric acid etching, coating for 3s, keeping wet, and coating dental adhesive for bonding.

Example thirty-two

Tris-HCl buffered 9mM CaCl₂And Tris-HCl buffered 5.4mM K₂HPO₄Mixing in equal volume, coating on the tooth surface after phosphoric acid etching for 3s, and drying with three guns.

Example thirty-three

Tris-HCl buffered 9mM CaCl₂And Tris-HCl buffered 5.4mM K₂HPO₄After mixing in equal volume, the mixture was applied to the phosphoric acid-etched tooth surface for 30 seconds, the mixed solution was repeatedly applied 10 times, the mixture was kept wet, and a dental adhesive was applied for adhesion.

Example thirty-four

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄Mixing at equal volume, coating onto the tooth surface after phosphoric acid etching, coating for 30s, keeping wet, and coating dental adhesive for bonding.

Example thirty-five

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄Mixing in equal volume, coating onto the tooth surface after phosphoric acid etching, coating for 30s, drying with three guns, and coating dental adhesive for bonding.

Example thirty-six

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄Mixing at equal volume, coating onto phosphoric acid-etched tooth surface for 30s, repeatedly coating the mixed solution for 10 times, keeping wet, and coating dental adhesiveAnd (6) bonding the rows.

Example thirty-seven

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄Mixing in equal volume, coating onto the tooth surface after phosphoric acid etching, coating for 30s, repeatedly coating the above mixed solution for 3 times, blow drying with three guns, and coating dental adhesive for bonding.

Example thirty-eight

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄The volume ratio is 2: 1, coating the mixture on the surface of the tooth body after phosphoric acid etching, keeping the mixture wet for 30s, and coating a dental adhesive for bonding.

Example thirty-nine

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄The volume ratio is 2: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating the mixture for 30s, drying the mixture by three guns, and coating a dental adhesive for bonding.

Example forty

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄The volume ratio is 2: 1, coating the mixture on the surface of a tooth body which has been acid-etched with phosphoric acid, coating the mixture for 30 seconds, repeating the coating of the mixture for 4 times, keeping the mixture wet, and coating a dental adhesive for adhesion.

Example forty one

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄The volume ratio is 2: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating the mixture for 30s, repeatedly coating the mixture for 4 times, drying by three guns, and coating a dental adhesive for bonding.

Example forty two

Tris-HCl buffered 500mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄The volume ratio is 1: 10, coating the mixture on the surface of the tooth body after phosphoric acid etching, keeping the mixture wet for 30s, and coating a dental adhesive for bonding.

Example forty-three

Tris-HCl buffered 500mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄The volume ratio is 1: 10, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating the mixture for 30s, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example forty-four

Tris-HCl buffered 500mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄The volume ratio is 1: after 10 mixing, the mixture was applied to the phosphoric acid-etched tooth surface for 15 seconds, and the mixed solution was repeatedly applied 3 times to keep wet and apply a dental adhesive for adhesion.

Example forty-five

Tris-HCl buffered 500mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄The volume ratio is 1: 10 mixing, coating on the phosphoric acid-etched tooth surface, coating for 15s, repeatedly coating the above mixed solution for 3 times, blow-drying the tooth surface, and coating dental adhesive for bonding.

Example forty-six

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered 500mM K₂HPO₄The volume ratio is 10: 1, coating the mixture on the surface of the tooth body after phosphoric acid etching, coating the mixture for 15s, keeping the mixture wet, and coating a dental adhesive for bonding.

Example forty-seven

Hepes buffered 100mM CaCl₂And Hepes buffered 500mM K₂HPO₄The volume ratio is 10: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating the mixture for 30s, drying the tooth surface, and coating a dental adhesive for bonding.

Example forty-eight

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered 500mM K₂HPO₄The volume ratio is 10: 1, coating the mixture on the surface of a tooth body which has been acid-etched with phosphoric acid, coating the mixture for 15 seconds, repeating the coating of the mixture for 2 times, keeping the mixture wet, and coating a dental adhesive for adhesion.

Example forty-nine

Hepes buffered100mM CaCl₂And Tris-HCl buffered 500mM K₂HPO₄The volume ratio is 10: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating the mixture for 30s, repeatedly coating the mixture for 2 times, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example fifty

Tris-HCl buffered 100mM Ca (NO)₃)₂And Tris-HCl buffered 100mM K₂HPO₄Mixing at equal volume, coating onto the tooth surface after phosphoric acid etching, coating for 30s, keeping wet, and coating dental adhesive for bonding.

Example fifty one

Tris-HCl buffered 100mM Ca (NO)₃)₂And Tris-HCl buffered 100mM K₂HPO₄Mixing in equal volume, coating onto the tooth surface after phosphoric acid etching, coating for 30s, drying tooth surface, and coating dental adhesive for bonding.

Example fifty two

Tris-HCl buffered 100mM Ca (NO)₃)₂And Tris-HCl buffered 100mM K₂HPO₄Mixing at equal volume, coating onto phosphoric acid-etched tooth surface for 30s, repeatedly coating the mixed solution for 2 times, keeping wet, and coating dental adhesive for bonding.

Example fifty three

Tris-HCl buffered 100mM Ca (NO)₃)₂And Tris-HCl buffered 100mM K₂HPO₄Mixing in equal volume, coating onto the tooth surface after phosphoric acid etching, coating for 30s, repeatedly coating the mixed solution for 2 times, blow-drying the tooth surface, and coating dental adhesive for bonding.

Example fifty four

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution of (1) (solution A) and Tris-HCl buffered 100mM K₂HPO₄(solution B) and the like, then, the mixture was applied to the surface of the phosphoric acid-etched tooth, the mixture was kept wet for 30 seconds, and a dental adhesive was applied to the mixture to perform adhesion.

Example fifty five

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution of (1) (solution A) and Tris-HCl buffered 100mM K₂HPO₄(solution B) and the like, applying the mixture to the phosphoric acid-etched tooth surface, applying the mixture for 30 seconds, blow-drying the tooth surface, and applying a dental adhesive for bonding.

Example fifty six

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution of (1) (solution A) and Tris-HCl buffered 100mM K₂HPO₄(solution B) and the like, then, the mixture was applied to the phosphoric acid-etched tooth surface for 30 seconds, 2 times, and kept wet, and then, a dental adhesive was applied to the surface to bond the teeth.

Example fifty seven

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution of (1) (solution A) and Tris-HCl buffered 100mM K₂HPO₄(solution B) and the like, applying the mixture to the phosphoric acid-etched tooth surface, applying the mixture for 30 seconds, applying the mixture for 2 times, blow-drying the tooth surface, and applying a dental adhesive for bonding.

Example fifty eight

Tris-HCl buffered 100mM CaCl₂(solution A) and Hepes-buffered 10mM K₂HPO₄、50mM Na₂HPO₄Solution (solution B) volume ratio of 1: 2, coating the mixture on the surface of the tooth body which is acid-etched by phosphoric acid, keeping the mixture wet for 30s, and coating a dental adhesive for adhesion.

Example fifty nine

Hepes buffered 100mM CaCl₂(solution A) and Hepes-buffered 10mM K₂HPO₄、50mM Na₂HPO₄Solution (solution B) volume ratio of 1: 2, coating the mixture on the surface of the tooth body which is acid-etched by phosphoric acid, keeping the mixture wet for 30s, and coating a dental adhesive for adhesion.

Example sixty

Hepes buffered 100mM CaCl₂(solution A) and Hepes-buffered 10mM K₂HPO₄、50mM Na₂HPO₄Solution (solution B)The volume ratio is 1: 2 mixing, coating on the surface of the tooth body after phosphoric acid etching, coating for 30s, drying the tooth surface, and coating a dental adhesive for bonding.

Example sixty one

Hepes buffered 100mM CaCl₂(solution A) and Hepes-buffered 10mM K₂HPO₄、50mM Na₂HPO₄Solution (solution B) volume ratio of 1: 2, coating the mixture on the surface of the tooth body which has been acid-etched with phosphoric acid, coating the mixture for 30 seconds, repeating the coating of the mixture for 2 times, keeping the mixture wet, and coating a dental adhesive for adhesion.

Example sixty-two

Hepes buffered 100mM CaCl₂(solution A) and Hepes-buffered 10mM K₂HPO₄、50mM Na₂HPO₄Solution (solution B) volume ratio of 1: 2, coating the mixture on the surface of the tooth body which is acid-etched by phosphoric acid for 30s, repeatedly coating the mixture for 2 times, drying the tooth surface, and coating a dental adhesive for bonding.

Example sixty-three

Hepes buffered 100mM CaCl₂(solution A) and Hepes-buffered 10mM K₂HPO₄、20mM Na₂HPO₄、30mM NaH₂PO₄The solution (solution B) was mixed in equal volume, applied to the phosphoric acid-etched tooth surface, kept wet for 30 seconds, and applied with a dental adhesive for adhesion.

Example sixty-four

Hepes buffered 100mM CaCl₂(solution A) and Hepes-buffered 10mM K₂HPO₄、20mM Na₂HPO₄、30mM NaH₂PO₄And (5) mixing the solutions (solution B) in equal volume, coating the mixture on the surface of the tooth body after phosphoric acid etching, coating the mixture for 30s, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example sixty-five

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄10mM NaF (solution B) in a volume ratio of 2: 1 mixing, coating on the tooth surface after phosphoric acid etching,the coating was carried out for 20 seconds, and the adhesive was applied while keeping wet.

Example sixty-six

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄10mM NaF (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating the mixture for 20s, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example sixty-seven

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄10mM NaF (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of the tooth body after phosphoric acid etching for 15s, repeating the coating for 5 times, keeping the tooth body wet, and coating a dental adhesive for bonding.

Example sixty-eight

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄10mM NaF (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 15s, repeatedly coating for 5 times, drying the tooth surface, and coating a dental adhesive for bonding.

Example sixty-nine

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄10mM NaF solution (solution B) in a volume ratio of 1: 2, coating the mixture on the surface of the tooth body which is acid-etched by phosphoric acid, keeping the mixture wet for 30s, and coating a dental adhesive for adhesion.

Example seventy

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄10mM NaF solution (solution B) in a volume ratio of 1: 2, coating the mixture on the surface of the tooth body which is phosphoric acid-etched, coating for 30s, coating for 2 times, keeping the tooth body wet, and coating dental adhesive for bonding.

Example seventy one

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄10mM NaF (solution B) in a volume ratio of 1: 2 mixing, coating on the surface of the tooth body after phosphoric acid etching, coating for 30s, drying the tooth surface, and coating a dental adhesive for bonding.

Example seventy-two

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄10mM NaF solution (solution B) in a volume ratio of 1: 2 mixing, coating on the surface of the tooth body after phosphoric acid etching, coating for 30s, coating for 2 times, drying the tooth surface, and coating dental adhesive for bonding.

Example seventy-three

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄10mM NaF (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of the tooth body after phosphoric acid etching, keeping the mixture wet for 30s, and coating a dental adhesive for bonding.

Example seventy-four

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄10mM NaF (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating the mixture for 30s, drying the tooth surface, and coating a dental adhesive for bonding.

Example seventy-five

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄10mM NaF (solution B) in a volume ratio of 1: 1 mixing, coating on phosphoric acid-etched tooth surface for 30s for 2 times, keeping wet, and coating on toothThe adhesive is used for bonding.

Example seventy-six

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄10mM NaF (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating for 30s and 2 times, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example seventy-seven

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄10mM NaF (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of the tooth body after phosphoric acid etching, keeping the mixture wet for 30s, and coating a dental adhesive for bonding.

Example seventy-eight

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄10mM NaF (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating the mixture for 30s, drying the tooth surface, and coating a dental adhesive for bonding.

Example seventy nine

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄10mM NaF (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of the tooth body after phosphoric acid etching for 30s and 3 times, keeping the mixture wet, and coating dental adhesive for bonding.

Example eighty

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄10mM NaF (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating for 30s and 3 times, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example eighty one

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄1mM chlorhexidine solution (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of the tooth body after phosphoric acid etching, coating the mixture for 20s, keeping the mixture wet, and coating a dental adhesive for bonding.

Example eighty two

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄1mM chlorhexidine solution (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating the mixture for 20s, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example eighty three

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄1mM chlorhexidine solution (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of the tooth body after phosphoric acid etching for 15s, repeating the coating for 5 times, keeping the tooth body wet, and coating a dental adhesive for bonding.

Example eighty four

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄1mM chlorhexidine solution (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 15s, repeatedly coating for 5 times, drying the tooth surface, and coating a dental adhesive for bonding.

Example eighty-five

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 2, coating the mixture on the surface of the tooth body which is acid-etched by phosphoric acid, keeping the mixture wet for 30s, and coating a dental adhesive for adhesion.

Example eighty six

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 2, coating the mixture on the surface of the tooth body which is phosphoric acid-etched, coating for 30s, coating for 2 times, keeping the tooth body wet, and coating dental adhesive for bonding.

Example eighty seven

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 2 mixing, coating on the surface of the tooth body after phosphoric acid etching, coating for 30s, drying the tooth surface, and coating a dental adhesive for bonding.

Example eighty eight

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 2 mixing, coating on the surface of the tooth body after phosphoric acid etching, coating for 30s, coating for 2 times, drying the tooth surface, and coating dental adhesive for bonding.

Example eighty nine

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of the tooth body after phosphoric acid etching, keeping the mixture wet for 30s, and coating a dental adhesive for bonding.

EXAMPLE ninety

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating the mixture for 30s, drying the tooth surface, and coating a dental adhesive for bonding.

EXAMPLE ninety one

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of the tooth body after phosphoric acid etching for 30s and 2 times, keeping the mixture wet, and coating dental adhesive for bonding.

EXAMPLE ninety two

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating for 30s and 2 times, drying the surface of the tooth, and coating a dental adhesive for bonding.

EXAMPLES ninety three

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of the tooth body after phosphoric acid etching, keeping the mixture wet for 30s, and coating a dental adhesive for bonding.

Example ninety four

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution of (1) (solution A) and Tris-HCl bufferContaining 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating the mixture for 30s, drying the tooth surface, and coating a dental adhesive for bonding.

Example ninety-five

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of the tooth body after phosphoric acid etching for 30s and 3 times, keeping the mixture wet, and coating dental adhesive for bonding.

Example ninety six

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating for 30s and 3 times, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example ninety seven

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered solution containing 100mM K₂HPO₄10mM captopril solution volume ratio 2: 1, coating the mixture on the surface of the tooth body after phosphoric acid etching, coating the mixture for 20s, keeping the mixture wet, and coating a dental adhesive for bonding.

Example ninety eight

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered solution containing 100mM K₂HPO₄10mM captopril solution volume ratio 2: 1 mixing, coating onto phosphoric acid-etched tooth surface, coating for 20s, blow-drying, and coating with dental adhesiveAnd (6) bonding.

Example ninety nine

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered solution containing 100mM K₂HPO₄10mM captopril solution volume ratio 2: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 15s, repeatedly coating for 5 times, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂And a solution containing 50mM K₂HPO₄10mM captopril solution volume ratio of 1: 2, applying the coating on the surface of the tooth body after phosphoric acid etching, keeping the coating wet for 30s, and applying a dental adhesive for bonding.

Example one hundred and one

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂And Tris-HCl buffered solution containing 50mM K₂HPO₄10mM captopril solution volume ratio of 1: 2, applying the coating solution to the surface of the tooth body after phosphoric acid etching for 30s, applying the coating solution for 2 times, keeping the coating solution wet, and applying a dental adhesive for bonding.

Example one hundred and two

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂And Tris-HCl buffered solution containing 50mM K₂HPO₄10mM captopril solution volume ratio of 1: 2, coating the surface of the tooth body after phosphoric acid etching for 30s, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred and three

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂And Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄10mM captopril solution volume ratio of 1: 1, applying the coating on the surface of the tooth body after phosphoric acid etching, keeping the coating wet for 30s, and applying a dental adhesive for bonding.

Example one hundred and four

Tris-HCl buffered solutions containing 50mM Ca (NO)₃)₂、50mM CaCl₂And Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄10mM captopril solution volume ratio of 1: 1, applying the coating on the surface of the tooth body after phosphoric acid etching, keeping the coating wet for 30s, and applying a dental adhesive for bonding.

Example one hundred and fifty

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of the tooth body after phosphoric acid etching, coating the mixture for 20s, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred and six

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating the mixture for 20s, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example one hundred and seven

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of the tooth body after phosphoric acid etching for 15s, repeating the coating for 5 times, keeping the tooth body wet, and coating a dental adhesive for bonding.

Example one hundred and eight

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 15s, repeatedly coating for 5 times, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred and nine

Tris-HCl bufferChong contains 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 2, coating the mixture on the surface of the tooth body which is acid-etched by phosphoric acid, keeping the mixture wet for 30s, and coating a dental adhesive for adhesion.

Example one hundred to ten

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 2, coating the mixture on the surface of the tooth body which is phosphoric acid-etched, coating for 30s, coating for 2 times, keeping the tooth body wet, and coating dental adhesive for bonding.

Example one hundred and eleven

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 2 mixing, coating on the surface of the tooth body after phosphoric acid etching, coating for 30s, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred and twelve

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 2 mixing, coating on the surface of the tooth body after phosphoric acid etching, coating for 30s, coating for 2 times, drying the tooth surface, and coating dental adhesive for bonding.

Example one hundred and thirteen

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 1 mixing, coating onto tooth surface after phosphoric acid etching for 30s, and keeping wetMoistening, coating dental adhesive for bonding.

Example one hundred and fourteen

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating the mixture for 30s, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred and fifteen

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of the tooth body after phosphoric acid etching for 30s and 2 times, keeping the mixture wet, and coating dental adhesive for bonding.

Example one hundred sixteen

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating for 30s and 2 times, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example one hundred seventeen

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of the tooth body after phosphoric acid etching, keeping the mixture wet for 30s, and coating a dental adhesive for bonding.

Example one hundred and eighteen

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating the mixture for 30s, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred and nineteen

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of the tooth body after phosphoric acid etching for 30s and 3 times, keeping the mixture wet, and coating dental adhesive for bonding.

Example one hundred twenty

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating for 30s and 3 times, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example one hundred twenty one

Tris-HCl buffered 9mM CaCl₂And Tris-HCl buffered 5.4mM K₂HPO₄Mixing in equal volume, coating onto the tooth surface after phosphoric acid etching for 10min, washing with water vapor, coating with 15% 10-MDP ethanol solution (solution C) for 20s, keeping wet, and coating with dental adhesive for adhesion.

Example one hundred twenty-two

Tris-HCl buffered 9mM CaCl₂And Tris-HCl buffered 5.4mM K₂HPO₄Mixing in equal volume, coating onto the tooth surface after phosphoric acid etching for 10min, washing with water vapor, coating with 15% 10-MDP ethanol solution (solution C) for 20s, drying with three guns, and coating dental adhesive for bonding.

Example one hundred twenty three

Tris-HCl buffered 9mM CaCl₂And Tris-HCl buffered 5.4mM K₂HPO₄Mixing in equal volume, coating onto the tooth surface after phosphoric acid etching for 3s, washing with water vapor, coating with 15% 10-MDP ethanol solution (solution C) for 20s, keeping wet, and coating with dental adhesive for adhesion.

Example one hundred twenty four

Tris-HCl buffered 9mM CaCl₂And Tris-HCl buffered 5.4mM K₂HPO₄Mixing in equal volume, coating onto the tooth surface after phosphoric acid etching for 3s, washing with water vapor, coating with 15% 10-MDP ethanol solution (solution C) for 20s, drying with three guns, and coating dental adhesive for bonding.

Example one hundred twenty five

Tris-HCl buffered 9mM CaCl₂And Tris-HCl buffered 5.4mM K₂HPO₄Mixing in equal volume, coating onto the tooth surface etched with phosphoric acid for 30s, repeatedly coating the mixed solution for 10 times, washing with water vapor, coating with 15% 10-MDP ethanol solution (solution C) for 20s, keeping wet, and coating with dental adhesive for bonding.

Example one hundred twenty six

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄Mixing in equal volume, coating onto the tooth surface after phosphoric acid etching for 30s, washing with water vapor, coating with 15% 10-MDP ethanol solution (solution C) for 20s, keeping wet, and coating with dental adhesive for adhesion.

Example one hundred twenty seven

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄Mixing in equal volume, coating on the tooth surface etched by phosphoric acid,coating for 30s, after water vapor washing, coating 15% 10-MDP ethanol solution (solution C) for 20s, drying by three guns, and coating dental adhesive for bonding.

Example one hundred twenty eight

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄Mixing at equal volume, coating onto the tooth surface after phosphoric acid etching for 30s, repeatedly coating the mixed solution for 3 times, rinsing with water vapor, and coating 15%

10-MDP ethanol solution (solution C) for 20s, kept wet, and coated with dental adhesive for adhesion.

Example one hundred twenty nine

10-MDP ethanol solution (solution C) for 20s, drying by three guns, and coating dental adhesive for bonding.

Example one hundred thirty

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄The volume ratio is 2: 1, coating the mixture on the surface of a tooth body which is etched by phosphoric acid for 30s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred thirty one

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄The volume ratio is 2: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, drying by three guns, and coating a dental adhesive for bonding.

Example one hundred thirty two hundred

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄The volume ratio is 2: 1 mixing, coating on the tooth surface after phosphoric acid etching for 30s, and repeating the coatingSpreading the mixed solution for 4 times, washing with water vapor, coating 15% 10-MDP ethanol solution (solution C) for 20s, keeping wet, and coating dental adhesive for bonding.

Example one hundred and thirty three

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄The volume ratio is 2: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating the mixture for 30s, repeatedly coating the mixture for 4 times, washing the mixture by water vapor, coating a 15% 10-MDP ethanol solution (solution C) for 20s, drying the mixture by three guns, and coating a dental adhesive for bonding.

Example one hundred thirty four

Tris-HCl buffered 500mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄The volume ratio is 1: 10, coating the mixture on the surface of a tooth body which is etched by phosphoric acid for 30s, washing the tooth body by water vapor, coating a 15 percent 10-MDP ethanol solution (solution C) for 20s, keeping the tooth body wet, and coating a dental adhesive for bonding.

Example one hundred and thirty five

Tris-HCl buffered 500mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄The volume ratio is 1: 10, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s, coating a 15 percent 10-MDP ethanol solution (solution C) for 20s after water vapor washing, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example one hundred thirty six

Tris-HCl buffered 500mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄The volume ratio is 1: 10, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating the mixture for 15s, repeatedly coating the mixture for 3 times, washing the mixture by water vapor, coating a 15% 10-MDP ethanol solution (solution C) for 20s, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred thirty seven

Tris-HCl buffered 500mM CaCl₂And Tris-HCl buffered 100mM K₂HPO₄The volume ratio is 1: mixing 10 times, coating on phosphoric acid-etched tooth surface for 15s, repeatedly coating the above mixed solution for 3 times, and rinsing with water vaporThen coating 15% 10-MDP ethanol solution (solution C) for 20s, drying the tooth surface, and coating dental adhesive for bonding.

Example one hundred and thirty eight

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered 500mM K₂HPO₄The volume ratio is 10: 1, coating the mixture on the surface of a tooth body which is etched by phosphoric acid for 15s after mixing, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred and thirty-nine

Hepes buffered 100mM CaCl₂And Hepes buffered 500mM K₂HPO₄The volume ratio is 10: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred forty

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered 500mM K₂HPO₄The volume ratio is 10: 1 coating on the surface of the tooth body after phosphoric acid etching for 15s after mixing, repeatedly coating the mixed solution for 2 times, coating 15% 10-MDP ethanol solution (solution C) for 20s after water vapor flushing, keeping the mixture wet, and coating dental adhesive for bonding.

Example one hundred and forty one

Hepes buffered 100mM CaCl₂And Tris-HCl buffered 500mM K₂HPO₄The volume ratio is 10: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid, coating the mixture for 30s, repeatedly coating the mixture for 2 times, washing the mixture by water vapor, coating a 15% 10-MDP ethanol solution (solution C) for 20s, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example one hundred and forty-two

Tris-HCl buffered 100mM Ca (NO)₃)₂And Tris-HCl buffered 100mM K₂HPO₄Mixing at equal volume, coating onto phosphoric acid etched tooth surface for 30s, washing with water vapor, coating with 15% 10-MDP ethanol solution (solution C) for 20s, keeping wet, and coating with dental adhesiveAnd (6) bonding the rows.

Example one hundred forty-three

Tris-HCl buffered 100mM Ca (NO)₃)₂And Tris-HCl buffered 100mM K₂HPO₄Mixing in equal volume, coating onto the surface of tooth etched by phosphoric acid for 30s, washing with water vapor, coating with 15% 10-MDP ethanol solution (solution C) for 20s, drying tooth surface, and coating dental adhesive for adhesion.

Example one hundred forty four

Tris-HCl buffered 100mM Ca (NO)₃)₂And Tris-HCl buffered 100mM K₂HPO₄Mixing in equal volume, coating onto the tooth surface after phosphoric acid etching, coating for 30s, repeatedly coating the mixed solution for 2 times, washing with water vapor, coating 15% 10-MDP ethanol solution (solution C) for 20s, keeping wet, and coating dental adhesive for bonding.

Example one hundred forty-five

Tris-HCl buffered 100mM Ca (NO)₃)₂And Tris-HCl buffered 100mM K₂HPO₄Mixing in equal volume, coating onto the surface of tooth etched by phosphoric acid, coating for 30s, repeatedly coating the mixed solution for 2 times, washing with water vapor, coating with 15% 10-MDP ethanol solution (solution C) for 20s, drying tooth surface, and coating dental adhesive for bonding.

Example one hundred forty-six

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution of (1) (solution A) and Tris-HCl buffered 100mM K₂HPO₄(solution B) and the like, coating the mixture on the surface of the tooth body which is etched by phosphoric acid for 30s, washing the tooth body with water vapor, coating a 15% 10-MDP ethanol solution (solution C) for 20s, keeping the tooth body wet, and coating a dental adhesive for bonding.

Example one hundred forty-seven

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution of (1) (solution A) and Tris-HCl buffered 100mM K₂HPO₄(solution B) and the like, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s, washing the tooth body by water vapor, and coating a 15% 10-MDP ethanol solution(solution C) for 20s, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred forty eight

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution of (1) (solution A) and Tris-HCl buffered 100mM K₂HPO₄(solution B) and the like, coating the mixture on the surface of the dental body which is acid-etched by phosphoric acid for 30s and 2 times, washing the mixture with water vapor, coating a 15% 10-MDP ethanol solution (solution C) for 20s, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred and forty-nine

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution of (1) (solution A) and Tris-HCl buffered 100mM K₂HPO₄(solution B) and the like, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s and 2 times, washing the mixture by water vapor, coating a 15% 10-MDP ethanol solution (solution C) for 20s, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example one hundred fifty

Tris-HCl buffered 100mM CaCl₂(solution A) and Hepes-buffered 10mM K₂HPO₄、50mM Na₂HPO₄Solution (solution B) volume ratio of 1: 2, coating the mixture on the surface of a tooth body which is etched by phosphoric acid for 30s after mixing, coating a 15 percent 10-MDP ethanol solution (solution C) for 20s after water vapor washing, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred fifty-one

Hepes buffered 100mM CaCl₂(solution A) and Hepes-buffered 10mM K₂HPO₄、50mM Na₂HPO₄Solution (solution B) volume ratio of 1: 2, coating the mixture on the surface of a tooth body which is etched by phosphoric acid for 30s after mixing, coating a 15 percent 10-MDP ethanol solution (solution C) for 20s after water vapor washing, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred and fifty-two

Hepes buffered 100mM CaCl₂(solution A) and Hepes-buffered 10mM K₂HPO₄、50mM Na₂HPO₄Solution (solution B) volume ratio of 1: 2 coating the mixture on the surface of the tooth body which is acid-etched by phosphoric acid for 30s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred and fifty-three

Hepes buffered 100mM CaCl₂(solution A) and Hepes-buffered 10mM K₂HPO₄、50mM Na₂HPO₄Solution (solution B) volume ratio of 1: 2 coating the mixture on the surface of the tooth body after phosphoric acid etching for 30s, repeatedly coating the mixture for 2 times, washing with water vapor, coating 15% 10-MDP ethanol solution (solution C) for 20s, keeping the solution wet, and coating dental adhesive for bonding.

Example one hundred fifty-four

Hepes buffered 100mM CaCl₂(solution A) and Hepes-buffered 10mM K₂HPO₄、50mM Na₂HPO₄Solution (solution B) volume ratio of 1: 2 coating the mixture on the surface of the tooth body which is acid-etched by phosphoric acid for 30s, repeatedly coating the mixed solution for 2 times, washing by water vapor, coating a 15% 10-MDP ethanol solution (solution C) for 20s, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred and fifty-five

Hepes buffered 100mM CaCl₂(solution A) and Hepes-buffered 10mM K₂HPO₄、20mM Na₂HPO₄、30mM NaH₂PO₄The solution (solution B) is mixed in equal volume, coated on the surface of the tooth body after phosphoric acid etching for 30s, washed by water vapor and coated with 15% 10-MDP ethanol solution (solution C) for 20s, kept wet and coated with dental adhesive for bonding.

Example one hundred fifty six

Hepes buffered 100mM CaCl₂(solution A) and Hepes-buffered 10mM K₂HPO₄、20mM Na₂HPO₄、30mM NaH₂PO₄Mixing the solutions (solution B) in equal volume, coating onto the tooth surface after phosphoric acid etching for 30s, washing with water vapor, and coating with 15% 10-MDP ethanolAnd (4) drying the tooth surface for 20s by using the solution (solution C), and coating a dental adhesive for bonding.

Example one hundred fifty-seven

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄10mM NaF (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of a tooth body which is etched by phosphoric acid for 20s after mixing, coating a 15 percent 10-MDP ethanol solution (solution C) for 20s after water vapor washing, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred and fifty-eight

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄10mM NaF (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 20s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred and fifty-nine

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄10mM NaF (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of a tooth body which is subjected to phosphoric acid etching for 15s, repeatedly coating for 5 times, washing with water vapor, coating a 15% 10-MDP ethanol solution (solution C) for 20s, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred sixty

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄10mM NaF (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 15s, repeatedly coating for 5 times, washing by water vapor, coating a 15% 10-MDP ethanol solution (solution C) for 20s, drying the tooth surface, and coating a dental adhesive for bonding.

Example five one hundred sixty eleven

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄10mM NaFVolume ratio of solution (solution B) 1: 2, coating the mixture on the surface of a tooth body which is etched by phosphoric acid for 30s after mixing, coating a 15 percent 10-MDP ethanol solution (solution C) for 20s after water vapor washing, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred sixty-twelve

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄10mM NaF solution (solution B) in a volume ratio of 1: 2, coating the mixture on the surface of a tooth body which is subjected to phosphoric acid etching for 30s and 2 times, washing the mixture with water vapor, coating a 15% 10-MDP ethanol solution (solution C) for 20s, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred sixty-three

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄10mM NaF (solution B) in a volume ratio of 1: 2 coating the mixture on the surface of the tooth body which is acid-etched by phosphoric acid for 30s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred sixty four

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄10mM NaF solution (solution B) in a volume ratio of 1: 2, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s and 2 times, washing the mixture by water vapor, coating a 15 percent 10-MDP ethanol solution (solution C) for 20s, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example one hundred sixty-five

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄10mM NaF (solution B) in a volume ratio of 1: 1 mixing, coating on the tooth surface after phosphoric acid etching for 30s, rinsing with water vapor, and coating15% 10-MDP ethanol solution (solution C) for 20s, kept wet, and coated with dental adhesive for adhesion.

Example one hundred sixty six sixteen

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄10mM NaF (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred sixty-seventeen

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄10mM NaF (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s and 2 times, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor flushing, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred sixty-eight

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄10mM NaF (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s and 2 times, coating a 15 percent 10-MDP ethanol solution (solution C) for 20s after water vapor flushing, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example one hundred sixty-nine

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄10mM NaF (solution B) in a volume ratio of 1: 1 after mixing, coating with phosphorusThe acid-etched tooth surface was coated for 30 seconds, rinsed with water vapor and then coated with 15% 10-MDP ethanol solution (solution C) for 20 seconds, kept wet and then coated with dental adhesive for adhesion.

Example one hundred and seventy

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄10mM NaF (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred and seventy eleven

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄10mM NaF (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s and 3 times, washing the mixture by water vapor, coating a 15% 10-MDP ethanol solution (solution C) for 20s, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred and seventy-two

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄10mM NaF (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s and 3 times, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor flushing, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example one hundred and seventy-three

Tris-HCl buffered 100mM CaCl₂(solution)A) And Tris-HCl buffered solution containing 100mM K₂HPO₄1mM chlorhexidine solution (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of a tooth body which is etched by phosphoric acid for 20s after mixing, coating a 15 percent 10-MDP ethanol solution (solution C) for 20s after water vapor washing, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred seventy-four

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄1mM chlorhexidine solution (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 20s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred seventy-five

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄1mM chlorhexidine solution (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of a tooth body which is subjected to phosphoric acid etching for 15s, repeatedly coating for 5 times, washing with water vapor, coating a 15% 10-MDP ethanol solution (solution C) for 20s, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred seventy-six

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄1mM chlorhexidine solution (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 15s, repeatedly coating for 5 times, washing by water vapor, coating a 15% 10-MDP ethanol solution (solution C) for 20s, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred seventeen

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 2 mixing, coating onto the surface of tooth after phosphoric acid etching for 30s, washing with water vapor, coating with 15% 10-MDP ethanol solution (solution C) for 20s, keeping wet, and coating with dental adhesiveAnd (6) bonding.

Example one hundred, seven eighteen

Example one hundred and seventy-nineteen

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 2 coating the mixture on the surface of the tooth body which is acid-etched by phosphoric acid for 30s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred and eighty

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 2, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s and 2 times, washing the mixture by water vapor, coating a 15 percent 10-MDP ethanol solution (solution C) for 20s, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example one hundred eighty-eleven

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is etched by phosphoric acid for 30s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred eighty-twelve

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred eighty three

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s and 2 times, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor flushing, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred eighty four

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s and 2 times, coating a 15 percent 10-MDP ethanol solution (solution C) for 20s after water vapor flushing, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example one hundred eighty-five

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is etched by phosphoric acid for 30s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred eighty six

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred eighty-seventeen

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s and 3 times, washing the mixture by water vapor, coating a 15% 10-MDP ethanol solution (solution C) for 20s, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred and eighty eight

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄1mM chlorhexidine solution (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s and 3 times, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor flushing, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example one hundred and eighty nineteen

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered solution containing 100mM K₂HPO₄10mM captopril solution volume ratio 2: 1 mixing, coating onto the tooth surface after phosphoric acid etching for 20s, washing with water vapor, and coating with 15% 10-MDP ethanolSolution (solution C)20s was kept wet, and was applied with a dental adhesive for bonding.

Example one hundred and ninety

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered solution containing 100mM K₂HPO₄10mM captopril solution volume ratio 2: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 20s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred and nine eleven

Tris-HCl buffered 100mM CaCl₂And Tris-HCl buffered solution containing 100mM K₂HPO₄10mM captopril solution volume ratio 2: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 15s, repeatedly coating for 5 times, washing by water vapor, coating a 15% 10-MDP ethanol solution (solution C) for 20s, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred and nine twelve

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂And a solution containing 50mM K₂HPO₄10mM captopril solution volume ratio of 1: 2, coating the mixture on the surface of a tooth body which is subjected to phosphoric acid etching for 30s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred and ninety three

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂And Tris-HCl buffered solution containing 50mM K₂HPO₄10mM captopril solution volume ratio of 1: 2, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s and 2 times, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred and ninety-four

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂And Tris-HCl buffered solution containing 50mM K₂HPO₄、10mThe volume ratio of the M captopril solution is 1: 2, coating the mixture on the surface of a tooth body which is subjected to phosphoric acid etching for 30s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred and ninety-five

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂And Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄10mM captopril solution volume ratio of 1: coating the solution on the surface of a tooth body which is etched by phosphoric acid for 30s, coating the solution in 15 percent 10-MDP ethanol (solution C) for 20s after water vapor washing, keeping the solution wet, and coating a dental adhesive for bonding.

Example one hundred and ninety six

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂And Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄10mM captopril solution volume ratio of 1: coating the solution on the surface of a tooth body which is etched by phosphoric acid for 30s, coating the solution in 15 percent 10-MDP ethanol (solution C) for 20s after water vapor washing, keeping the solution wet, and coating a dental adhesive for bonding.

Example one hundred and ninety-seven

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of a tooth body which is etched by phosphoric acid for 20s after mixing, coating a 15 percent 10-MDP ethanol solution (solution C) for 20s after water vapor washing, keeping the mixture wet, and coating a dental adhesive for bonding.

Example one hundred and ninety-eight

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 2: 1 mixing, coating on the tooth surface after phosphoric acid etching for 20s, washing with water vapor, and coating with 15% 10-MDP BAlcohol solution (solution C) for 20s, drying the tooth surface, and coating a dental adhesive for bonding.

Example one hundred and nine nineteen

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 15s, repeatedly coating for 5 times, keeping the tooth body wet, washing the tooth body by water vapor, coating a 15% 10-MDP ethanol solution (solution C) for 20s, and coating a dental adhesive for bonding.

Example two hundred

Tris-HCl buffered 100mM CaCl₂(solution A) and Tris-HCl buffered 100mM K₂HPO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 2: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 15s, repeatedly coating for 5 times, washing by water vapor, coating a 15% 10-MDP ethanol solution (solution C) for 20s, drying the tooth surface, and coating a dental adhesive for bonding.

Example two hundred and one

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 2, coating the mixture on the surface of a tooth body which is etched by phosphoric acid for 30s after mixing, coating a 15 percent 10-MDP ethanol solution (solution C) for 20s after water vapor washing, keeping the mixture wet, and coating a dental adhesive for bonding.

Example two hundred and two

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 2, coating the mixture on the surface of a tooth body which is subjected to phosphoric acid etching for 30s and 2 times, washing the mixture with water vapor, coating a 15% 10-MDP ethanol solution (solution C) for 20s, keeping the mixture wet, and coating a dental adhesive for bonding.

Example two hundred and three

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 2 coating the mixture on the surface of the tooth body which is acid-etched by phosphoric acid for 30s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, drying the tooth surface, and coating a dental adhesive for bonding.

Example two hundred and four

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 2, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s and 2 times, washing the mixture by water vapor, coating a 15 percent 10-MDP ethanol solution (solution C) for 20s, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example two hundred and five

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is etched by phosphoric acid for 30s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, keeping the mixture wet, and coating a dental adhesive for bonding.

Example two hundred and six

Example two hundred and seven

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution of (2)Solution (solution A) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s and 2 times, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor flushing, keeping the mixture wet, and coating a dental adhesive for bonding.

Example two hundred and eight

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 50mM K₂HPO₄、10mM KH₂PO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s and 2 times, coating a 15 percent 10-MDP ethanol solution (solution C) for 20s after water vapor flushing, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example two hundred and nine

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is etched by phosphoric acid for 30s, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor washing, keeping the mixture wet, and coating a dental adhesive for bonding.

Example two hundred to ten

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 1 mixing, coating onto the surface of tooth body after phosphoric acid etching for 30s, washing with water vapor, coating with 15% 10-MDP ethanol solution (solution C) for 20s, blow-drying, and coating onto dental partThe adhesive is used for bonding.

Example two hundred and eleven

Example two hundred and twelve

Tris-HCl buffered solution containing 50mM Ca (NO)₃)₂、50mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄、10mM KH₂PO₄、10mM Na₂HPO₄、20mM NaH₂PO₄10mM NaF, 10mM captopril (solution B) in a volume ratio of 1: 1, coating the mixture on the surface of a tooth body which is acid-etched by phosphoric acid for 30s and 3 times, coating a 15% 10-MDP ethanol solution (solution C) for 20s after water vapor flushing, drying the surface of the tooth, and coating a dental adhesive for bonding.

Example two hundred and thirteen

Tris-HCl buffered CaCl 5mM₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 5mM K₂HPO₄The solution (solution B) is mixed in equal volume, coated on the surface of the tooth body after phosphoric acid etching for 30s, coated with 15% 10-MDP ethanol solution (solution C) for 30s after water vapor flushing, kept wet, and coated with dental adhesive for bonding.

Example two hundred fourteen

Tris-HCl buffered CaCl 5mM₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 5mM K₂HPO₄The solution (solution B) is mixed in equal volume, coated on the surface of the tooth body after phosphoric acid etching for 30s and 2 times, coated with 15% 10-MDP ethanol solution (solution C) for 30s after water vapor flushing, kept wet, and coated with dental adhesive for bonding.

Example two hundred and fifteen

Tris-HCl buffered CaCl 5mM₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 5mM K₂HPO₄The solution (solution B) is mixed in equal volume, coated on the surface of the tooth body after phosphoric acid etching for 30s, coated with 15% 10-MDP ethanol solution (solution C) for 30s after water vapor flushing, coated for 2 times, kept wet, and coated with dental adhesive for bonding.

Example two hundred to sixteen

Tris-HCl buffered CaCl 5mM₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 5mM K₂HPO₄The solution (solution B) is mixed in equal volume, coated on the surface of the tooth body after phosphoric acid etching for 30s and 2 times, coated with 15% 10-MDP ethanol solution (solution C) for 30s after water vapor flushing for 2 times, kept wet, and coated with dental adhesive for bonding.

Example two hundred seventeen

Tris-HCl buffered CaCl 5mM₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 5mM K₂HPO₄The solution (solution B) is mixed in equal volume, coated on the surface of the tooth body after phosphoric acid etching for 30s, coated with 15 percent 10-MDP ethanol solution (solution C) for 30s after water vapor flushing, dried on the tooth surface and coated with dental adhesive for bonding.

Example two hundred to eighteen

Tris-HCl buffered CaCl 5mM₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 5mM K₂HPO₄The solution (solution B) is mixed in equal volume, coated on the surface of the tooth body after phosphoric acid etching for 30s and 2 times, coated with 15 percent 10-MDP ethanol solution (solution C) for 30s after water vapor flushing, dried on the tooth surface and coated with dental adhesive for bonding.

Example two hundred and nineteen

Tris-HCl buffered CaCl 5mM₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 5mM K₂HPO₄The solution (solution B) is mixed in equal volume, coated on the surface of the tooth body after phosphoric acid etching for 30s, coated with 15 percent 10-MDP ethanol solution (solution C) for 30s after water vapor flushing for 2 times,drying the tooth surface, and coating the dental adhesive for bonding.

Example two hundred and twenty

Tris-HCl buffered CaCl 5mM₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 5mM K₂HPO₄The solution (solution B) is mixed in equal volume, coated on the surface of the tooth body after phosphoric acid etching for 30s and 2 times, coated with 15 percent 10-MDP ethanol solution (solution C) for 30s after water vapor flushing, coated for 2 times, dried on the tooth surface, and coated with dental adhesive for bonding.

Example two hundred twenty-one

Tris-HCl buffered 10mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄The solution (solution B) was mixed in equal volume, applied to the surface of the phosphoric acid-etched tooth for 30 seconds, rinsed with water vapor, applied with 5% 4-MET ethanol solution (solution C) for 20 seconds, kept wet, and applied with dental adhesive for adhesion.

Example two hundred twenty-two

Tris-HCl buffered 10mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄The solution (solution B) was mixed in equal volume, applied to the phosphoric acid-etched tooth surface for 10s, repeatedly applied for 3 times, then rinsed with water vapor, applied with 5% 4-MET ethanol solution (solution C) for 20s, kept wet, and applied with dental adhesive for adhesion.

Example two hundred twenty three

Tris-HCl buffered 10mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄The solution (solution B) is mixed in equal volume, coated on the surface of the tooth body after phosphoric acid etching, coated for 10s, repeatedly coated for 3 times, washed by water vapor, coated with 5% 4-MET ethanol solution (solution C) for 10s, repeatedly coated for 3 times, kept wet, and coated with dental adhesive for bonding.

Example twenty-hundred twenty-four

Tris-HCl buffered 10mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄The solution is mixed in equal volume and then coated on the teeth after phosphoric acid etchingCoating the surface of the body for 30s, washing with water vapor, coating 5% 4-MET ethanol solution (solution C) for 20s, drying the tooth surface, and coating dental adhesive for bonding.

Example twenty-hundred and twenty-five

Tris-HCl buffered 10mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄The solution is mixed in equal volume, coated on the surface of the tooth body after phosphoric acid etching, coated for 10s, repeatedly coated for 3 times, washed by water vapor, coated with 5 percent 4-MET ethanol solution (solution C) for 20s, dried on the tooth surface, coated with dental adhesive for bonding.

Example two hundred twenty six

Tris-HCl buffered 10mM CaCl₂Solution (solution A) of (1) and Tris-HCl buffered solution containing 10mM K₂HPO₄The solution is mixed in equal volume, coated on the surface of the tooth body after phosphoric acid etching, coated for 10s, repeatedly coated for 3 times, washed by water vapor, coated with 5% 4-MET ethanol solution (solution C) for 10s, repeatedly coated for 3 times, blown to dry the tooth surface, and coated with dental adhesive for bonding.

Claims

1. The dentin adhesion pretreatment composition is characterized by comprising a binary system and a ternary system, wherein the binary system consists of a solution A and a solution B, and the ternary system consists of the solution A, the solution B and the solution C.

2. The pretreatment composition of claim 1, wherein the solution a and solution B are in the same range in the binary system and the ternary system, and the ratio of solution a: soluble calcium salt solution, solution B: soluble phosphate solution, solution C in ternary system: an organic monomeric reagent solution capable of chemisorbing to an insoluble calcium phosphate salt.

3. The pretreatment composition of claim 2, wherein each of solution a and solution B is buffered with a buffer, wherein the pH of the solutions is 5.0 to 9.0, and the buffer is Tris-HCl, Hepes system.

4. The pretreatment composition of claim 2, wherein solution a is a soluble calcium salt selected from the group consisting of calcium chloride solution, calcium nitrate solution, and a mixture thereof, and the concentration of calcium ions in solution a is between 0.01mM and 1M.

5. The pretreatment composition of claim 2, wherein solution B is a soluble phosphate solution.

6. The soluble phosphate solution B according to claim 5, wherein the concentration of the phosphate, hydrogen phosphate and dihydrogen phosphate in the solution B is 0.01 mM-1M, and the solution is selected from lithium phosphate, lithium monohydrogen phosphate, lithium dihydrogen phosphate, sodium monohydrogen phosphate, potassium dihydrogen phosphate solution, ammonium phosphate, ammonium monohydrogen phosphate, ammonium dihydrogen phosphate solution, or a mixture of two or more thereof.

7. The soluble phosphate solution B according to claim 5, characterized by a soluble phosphate solution comprising one or more antibacterial, enzyme-inhibiting substances; the phosphate solution is in the same range as in claim 6, wherein the antibacterial and enzyme inhibiting substance is selected from the group consisting of sodium fluoride, chlorhexidine, polyhexamethylene biguanide or a salt thereof, captopril, and the concentration of the antibacterial and enzyme inhibiting substance in solution B is 0.001 mM-1M.

8. The pretreatment composition of claim 2, wherein solution C is selected from the group consisting of 10-methacryloyloxydecyl phosphate (10-MDP), 2,4, 6-trimethylphenyl 2- [4- (dihydroxyphosphate) -2-oxabutyl ] acrylate (MAEPA), ethyl 2- [4- (dihydroxyphosphoryl) -2-oxabutyl ] acrylate (EAEPA), n-dodecyl dihydrogen phosphate, and dihydrogen ethyl phosphate, one or more of 4-methacryloxyethyl trimellitic acid (4-MET) and 4-methacryloxytrimellitic anhydride (4-META), the solvent in the solution C is water, ethanol, acetone or a mixture of the solvents, and the concentration of the organic monomer reagent in the solution C is 0.001 mM-10M.

9. The pretreatment composition of claim 2, wherein the molar ratio of the calcium ion concentration in solution a to the sum of the phosphate, hydrogen phosphate, and dihydrogen phosphate concentrations in solution B is 10: 1-1: 10.

10. use of the pretreatment composition of claim 1 or 2 for preparing a dental adhesive pretreatment.

11. The use of claim 10, wherein the dental adhesive pretreatment is packaged separately from solution a, solution B and solution C.

12. The use according to claim 10, wherein the dental adhesive pretreatment is applied in a volume ratio of 10: 1-1: 10, mixing, and immediately applying to the surface of the demineralized dentin after mixing.

13. Use according to claim 10, wherein for the ternary system, after the solution a and the solution B have been mixed and applied to the demineralized dentin matrix, a water vapor rinse is carried out and then the solution C of the ternary system is used.