CN103340755A - Dental prosthetic material and preparation method thereof - Google Patents
Dental prosthetic material and preparation method thereof Download PDFInfo
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- CN103340755A CN103340755A CN2013102468702A CN201310246870A CN103340755A CN 103340755 A CN103340755 A CN 103340755A CN 2013102468702 A CN2013102468702 A CN 2013102468702A CN 201310246870 A CN201310246870 A CN 201310246870A CN 103340755 A CN103340755 A CN 103340755A
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Abstract
The invention discloses a dental prosthetic material and a preparation method thereof. The method comprises the following steps of (1) immersing dentin in an EDTA aqueous solution; and (2) putting the dentin treated by the step (1) in a sodium hyaluronate-calcium nitrate hydrogel, adding a dihydrogen phosphate ion and fluoride ion aqueous solution after standing; and reacting to obtain the dental prosthetic material, wherein the sodium hyaluronate-calcium nitrate hydrogel is a mixture of sodium hyaluronate and calcium nitrate aqueous solutions. With the preparation method provided by the invention, a dense dental prosthetic material with a bionic structure analogous to human enamel is grown on the surface of the isolated human dentin directly under an environment similar to human physiological conditions (37 DEG C, atm, pH6.0) through a simple chemical method. The film dental prosthetic material has an extremely similar structure to that of natural human enamel and has apatite hexagonal prism crystals and enamel crystal column microstructures. Mechanical properties of the dental prosthetic material are between that of natural human enamel and that of the dentin.
Description
Technical field
The present invention relates to a kind of dental prosthetic material and preparation method thereof.
Background technology
Dentin constitutes the main part of tooth body, is positioned at enamel and cemental internal layer, also is the sidewall of pulp cavity and root pipe, and color is yellowish.Its mineral accounts for 65%～75%, and organic matter accounts for 20%, and all the other 5%～10% are water, so mineralising is not as enamel, but has bigger elasticity than enamel.Average microhardness is about 1/5 of enamel, but higher in both intersection hardness, is about 3 times of nearly marrow end, can strengthen the support to enamel fiber thus.
If use microscopic examination, can see the tubule that many queueing disciplines are arranged in the dentin, be called dentinal tubule, nerve fiber is arranged in the pipe, after dentin exposes, can experience stimulations such as the external world is hot and cold, sour, sweet, and cause pain.Dentin hypersensitiveness refers to that mainly enamel wrecks, the dentin expose portion, and when being subjected to the stimulations such as (brushing teeth, sting hard thing) of (acid, alkali) of temperature (hot and cold), chemistry and machinery, caused sensation of aching unusually.The irritated quality of life that can greatly reduce the patient, bring difficulty for feed and other daily routines, also may cause other oral diseases simultaneously.
Main by the medicine desensitization therapy on the clinical oral at present, make medicine infiltrate dentinal tubule, make protein coagulation, or in the medicine body deposition tubule itself, stop environmental stimuli to import into, reach the desensitization purpose.There is shortcoming equally in this method: one, there are bigger difference in medicine and Dentinal composition, and the desensitization effect that reaches by protein coagulated way is not lasting; Two, drug desensitizations such as sulphur phenol, thymol, ammoniacal silver nitrate, 75% sodium fluoride, there is bigger zest in itself, and the process patient for the treatment of need bear bigger misery.Therefore, need the method for a kind of more Johnson ﹠ Johnson thing compatibility, be used for repairing and treating dentin hypersensitiveness, ectrogeny, and the damage that is brought by dental caries.Different with enamel is, dentin has certain damage self-repairing capability: after the tooth eruption, because wearing and tearing, wound, dental caries or operation process etc. are former thereby when dentin is stimulated, can form third phase dentin at the marrow end of dentinal tubule, i.e. reparative dentin.But this process can not stop extraneous damage to stimulate fully, can not revert to the original state that does not sustain damage, and also needs a kind of effective medical means to remove to carry out clinical treatment.Find a kind of have the dental prosthetic material of good biocompatibility or find a kind of can perfect method of repairing enamel lesions, attracting numerous scientists.Because Dentinal main body composition is the lithotroph mineral, by simple chemistry and the method for acellular is repaired or the essence of regenerating is possible.
Summary of the invention
The purpose of this invention is to provide a kind of dental prosthetic material and preparation method thereof.
The preparation method of a kind of dental prosthetic material provided by the present invention comprises the steps:
(1) dentin is soaked in the EDTA aqueous solution;
(2) dentin after step (1) is handled is placed hyaluronate sodium-lime nitrate hydrogel; After leaving standstill, continue to add dihydrogen phosphate ions and fluorion aqueous solution, namely obtain described dental prosthetic material through reaction;
Described hyaluronate sodium-lime nitrate hydrogel is the mixture of hyaluronate sodium and calcium nitrate aqueous solution.
In the above-mentioned preparation method, the molecular weight of described hyaluronate sodium can be 120,000～140,000 dalton.
In the above-mentioned preparation method, in the step (1), the molar concentration of described EDTA aqueous solution can be 0.25～0.4mol/L;
The temperature of described immersion can be 60～70 ℃, and the time can be 6～7 hours, as soaking 6 hours down at 60 ℃.
In the above-mentioned preparation method, in the step (2), the pH value of described hyaluronate sodium-lime nitrate hydrogel can be 6.0～7.0, as 6.0;
In described hyaluronate sodium-lime nitrate hydrogel, the mass ratio of described hyaluronate sodium and described lime nitrate can be 2:2.3～2.4, as 2:2.36.
In the above-mentioned preparation method, the molar concentration of described calcium nitrate aqueous solution can be 0.10～0.20mol/L, specifically can be 0.167mol/L.
In the above-mentioned preparation method, in the step (2), the dihydrogen phosphate ions in described dihydrogen phosphate ions and the fluorion aqueous solution is from NH
4H
2PO
4
Fluorion in described dihydrogen phosphate ions and the fluorion aqueous solution is from NH
4F.
In the above-mentioned preparation method, in the step (2), in described dihydrogen phosphate ions and the fluorion aqueous solution, the molar concentration of described dihydrogen phosphate ions can be 0.15～0.18mol/L, as 0.15mol/L, the molar concentration of described fluorion can be 0.05～0.06mol/L, as 0.05mol/L.
In the above-mentioned preparation method, in the step (2), the mol ratio of lime nitrate, described dihydrogen phosphate ions and described fluorion can be 4.5～5:3:0.5～2, specifically can be 5:3:1.
In the above-mentioned preparation method, in the step (2), described reaction can be carried out under 35～40 ℃ condition 2～7 days.
The present invention further provides the dental prosthetic material by method for preparing.
The present invention also provides hyaluronate sodium to fluoridize application in the calcium hydroxy phosphate crystal growth in regulation and control.
Preparation method provided by the invention, by simple chemical method, approximate Human Physiology condition (37 ℃, atm, pH6.0) in the environment, directly grown dental prosthetic material fine and close, that have similar human enamel's biomimetic features in the people dentin surface that exsomatizes.The structure of the dental prosthetic material of this film like and natural human enamel are very similar, have apatite six prismatic crystal and enamel crystal column micro structure, and mechanical property are between natural human enamel and dentin.Method mild condition, the process for preparing dental prosthetic material of the present invention is simple, raw material is cheap, has clinical value, prepared dental prosthetic material is expected to substitute existing dental prosthetic material and repairs the dentin damage that dental caries or other dental disorder cause, and also can be used as the prevention that essential tubule packing material is used for dentin hypersensitiveness.
Description of drawings
Fig. 1 is the typical SEM image of the regeneration intrinsic layer surface topography of employing the inventive method preparation.
Fig. 2 is the XRD spectra of the regeneration essence of employing the inventive method preparation.
Fig. 3 is the loading-unloading curve of 5000 μ N load control nano-indenter test.
The specific embodiment
Employed experimental technique is conventional method if no special instructions among the following embodiment.
Used material, reagent etc. if no special instructions, all can obtain from commercial channels among the following embodiment.
The preparation of embodiment 1, dental prosthetic material
Get the stripped mankind and grind one's teeth in sleep or wisdom teeth, with low speed diamond custting machine the crown portion branch is scaled off, again rest parts is cut into the thin slice of 1～2mm.With dentin 0.3mol/L EDTA solution water-bath heat treated, heating-up temperature is 60 ℃, and the time is 6h, washes out remaining solution with deionized water, and is stand-by.
Take by weighing 3.936g Ca (NO
3)
24H
2O adds about 80mL deionized water, the electromagnetic agitation dissolving, and 100mL volumetric flask standardize solution obtains ionic calcium soln, and its molar concentration is 0.167mol/L.Take by weighing 1.725g KH
2PO
4, and 0.185gNH
4F, the electromagnetic agitation dissolving, 100mL volumetric flask standardize solution obtains dihydrogen phosphate-fluorion aqueous solution, and in this aqueous solution, the molar concentration of dihydrogen phosphate is 0.15mol/L, and the molar concentration of fluorion is 0.05mol/L.
Measure the ionic calcium soln 6mL of above-mentioned preparation, add 0.20g high molecular weight sodium hyaluronate (120,000～140,000 dalton) powder, (pH value is 6.0 to forming uniform hyaluronate sodium-lime nitrate hydrogel at 50 ℃ of following electromagnetism heated and stirred 30min, the mass ratio of hyaluronate sodium and lime nitrate is 0.20:0.236), to be placed in one with the dentin section that the EDTA solution-treated is crossed, place to be cooled to room temperature.Drip above-mentioned dihydrogen phosphate-fluorion aqueous solution 4mL again, contain 0.10mol/L Ca in the reaction system this moment
2+, 0.06mol/L H
2PO
4 -, 0.02mol/L F
-Cut into slices with dentin.Reaction system is sealed with sealing film, place 37 ℃ calorstat, left standstill 4 days.
Take out reacted dentin section, use deionized water rinsing three times, dry naturally in the air, obtain the dentin of regenerating.
The typical SEM image of regeneration adamantine layer surface topography as shown in Figure 1, wherein, the scale of Fig. 1 (a) is 50.0 μ m; The scale of Fig. 1 (b) is 10.0 μ m; The scale of Fig. 1 (c) is 2.0 μ m.Dentin shows by the compact arranged lens cylinder of a branch of bundle and covers as can be seen from Fig. 1 (a); Fig. 1 (b) shows that further the structure of this crystal column presents typical six prism structures, and direction of growth height unanimity; Fig. 1 that amplification is higher (c) then clearly demonstrates the hexagonal cross-section that diameter is about the typical phosphorite crystal of 1 μ m.
From Fig. 1 (a)-Fig. 1 (c), it can also be seen that the surface topography of regeneration zone is closely neat, have six prismatic crystal structures and the cluster shape crystal column structure of similar natural enamel.
The chemical composition of above-mentioned enamel regeneration zone characterizes with X-ray diffraction (XRD) and X-ray electron spectrum (EDS), and the XRD spectra before and after the regeneration as shown in Figure 2.Wherein, the dentin after Fig. 2 (a) expression was regenerated 4 days with said method, the dentin that Fig. 2 (b) expression was only handled with EDTA.As can be seen, the XRD figure spectrum of the strong peak that the XRD spectra of the dentin regeneration zone of employing method for preparing is main and hydroxyapatite matches from Fig. 2 (a); Very big 002 peak of intensity is parallel with enamel surfaces with 004 peak explanation crystal face, and namely crystal is grown along the c direction of principal axis, and what see in this point and the SEM image is consistent.
EDS result shows that the Ca/P ratio in the regeneration zone is that 1.59, F/Ca ratio is 0.13.Ca/P than very near the Ca/P in hydroxyapatite (HA) or the fluor-apatite (FA) than 1.67, owing to the error of EDS analysis means itself, the result is less than normal to be normal.From F/Ca recently, fluorine content is lower than FA and is higher than HA, illustrate that crystal in the regeneration zone is partially fluorinated hydroxyapatite (fluoridated hydroxyapatite FHA), is the same with the chemical composition of natural enamel.
The regeneration enamel that adopts method for preparing is carried out 5000 μ N load control nano-indenter test, probe with onesize defeat into, the degree of depth that is pressed into that mechanical strength is big is little, the loading-unloading curve of 5000 μ N load control nano-indenter test is shown in Fig. 3 (a) and Fig. 3 (b), 3(a wherein) be dentin after the regeneration 4 days, Fig. 3 (b) is natural teeth essence.The Natural tooth Enamel that from Fig. 3 (a) and Fig. 3 (b), can visually see and the adamantine mechanical property of regeneration, the enamel of namely regenerating 4 days〉mechanical strength of natural enamel.
6 repetitions are established in experiment, and the average statistics result of 6 impression data is with the formal representation of mean+SD, and natural enamel is as shown in table 1 with the quantitative assay result of regeneration enamel mechanical property.
Dentinal mechanical property before and after table 1 regeneration
Data in the table 1 can be confirmed top qualitative results, no matter are elastic modelling quantity or hardness, and 4 days enamel of regeneration is arranged〉natural enamel, and no matter be elastic modelling quantity or hardness, regeneration be about 4 times of natural teeth essence.
Claims (10)
1. the preparation method of a dental prosthetic material comprises the steps:
(1) dentin is soaked in the EDTA aqueous solution;
(2) dentin after step (1) is handled is placed hyaluronate sodium-lime nitrate hydrogel; After leaving standstill, continue to add dihydrogen phosphate ions and fluorion aqueous solution, namely obtain described dental prosthetic material through reaction;
Described hyaluronate sodium-lime nitrate hydrogel is the mixture of hyaluronate sodium and calcium nitrate aqueous solution.
2. method according to claim 1, it is characterized in that: in the step (1), the molar concentration of described EDTA aqueous solution is 0.25～0.4mol/L;
The temperature of described immersion can be 60～70 ℃, and the time can be 6～7 hours.
3. method according to claim 1 and 2, it is characterized in that: in the step (2), the pH value of described hyaluronate sodium-lime nitrate hydrogel is 6.5～7.4;
In described hyaluronate sodium-lime nitrate hydrogel, the mass ratio of described hyaluronate sodium and described lime nitrate is 2:2.3～2.4.
4. according to each described method among the claim 1-3, it is characterized in that: the molar concentration of described calcium nitrate aqueous solution is 0.10～0.20mol/L.
5. according to each described method among the claim 1-4, it is characterized in that: in the step (2), the dihydrogen phosphate ions in described dihydrogen phosphate ions and the fluorion aqueous solution is from NH
4H
2PO
4
Fluorion in described dihydrogen phosphate ions and the fluorion aqueous solution is from NH
4F.
6. according to each described method among the claim 1-5, it is characterized in that: in the step (2), in described dihydrogen phosphate ions and the fluorion aqueous solution, the molar concentration of described dihydrogen phosphate ions is 0.15～0.18mol/L, and the molar concentration of described fluorion is 0.05～0.06mol/L.
7. according to each described method among the claim 1-6, it is characterized in that: in the step (2), the mol ratio of lime nitrate, described dihydrogen phosphate ions and described fluorion is 4.5～5:3:0.5～2.
8. according to each described method among the claim 1-7, it is characterized in that: in the step (2), described being reflected under 35～40 ℃ the condition carried out 2～7 days.
9. the dental prosthetic material of each described method preparation among the claim 1-8.
10. hyaluronate sodium is fluoridized application in the calcium hydroxy phosphate crystal growth in regulation and control.
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| CN201310246870.2A CN103340755B (en) | 2013-06-20 | 2013-06-20 | Dental prosthetic material and preparation method thereof |
| PCT/CN2013/001026 WO2014201592A1 (en) | 2013-06-20 | 2013-08-30 | Dental prosthetic material and preparation method therefor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106265093A (en) * | 2016-08-09 | 2017-01-04 | 北京大学 | A kind of dental prosthetic material and preparation method thereof |
| CN106823001A (en) * | 2017-04-12 | 2017-06-13 | 吉林大学 | A kind of biologic bracket material, preparation method and applications for dental root regeneration |
| CN113208930A (en) * | 2021-05-07 | 2021-08-06 | 首都医科大学附属北京口腔医院 | Preparation method of mineral filling material generated in situ in tooth root canal system |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5149536A (en) * | 1991-12-06 | 1992-09-22 | Ratkus Victor L | Dental root canal bacterialcidal lubricant |
| CN101444454A (en) * | 2008-12-16 | 2009-06-03 | 北京大学 | Method for preparing dental prosthetic material |
| CN102028552A (en) * | 2010-11-29 | 2011-04-27 | 四川大学 | Dentin surface bionic hydroxyapatite coating preparation method |
| CN102068318A (en) * | 2010-12-21 | 2011-05-25 | 四川大学 | Manufacturing method of biological tooth root bracket material |
-
2013
- 2013-06-20 CN CN201310246870.2A patent/CN103340755B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5149536A (en) * | 1991-12-06 | 1992-09-22 | Ratkus Victor L | Dental root canal bacterialcidal lubricant |
| CN101444454A (en) * | 2008-12-16 | 2009-06-03 | 北京大学 | Method for preparing dental prosthetic material |
| CN102028552A (en) * | 2010-11-29 | 2011-04-27 | 四川大学 | Dentin surface bionic hydroxyapatite coating preparation method |
| CN102068318A (en) * | 2010-12-21 | 2011-05-25 | 四川大学 | Manufacturing method of biological tooth root bracket material |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106265093A (en) * | 2016-08-09 | 2017-01-04 | 北京大学 | A kind of dental prosthetic material and preparation method thereof |
| CN106265093B (en) * | 2016-08-09 | 2020-03-27 | 北京大学 | Dental restoration material and preparation method thereof |
| CN106823001A (en) * | 2017-04-12 | 2017-06-13 | 吉林大学 | A kind of biologic bracket material, preparation method and applications for dental root regeneration |
| CN106823001B (en) * | 2017-04-12 | 2019-11-05 | 吉林大学 | A kind of biologic bracket material for dental root regeneration, preparation method and applications |
| CN113208930A (en) * | 2021-05-07 | 2021-08-06 | 首都医科大学附属北京口腔医院 | Preparation method of mineral filling material generated in situ in tooth root canal system |
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| CN103340755B (en) | 2014-11-26 |
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Effective date of registration: 20180920 Address after: 100080 Beijing Haidian District Zhongguancun North Street 127-1, 1 floor 107-10 room. Patentee after: Beijing salamander Technology Co., Ltd. Address before: 100871 No. 202 Cheng Fu Road, Haidian District, Beijing. Patentee before: Peking University |
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Address after: 310000 room 129, 1 / F, building 18, Xinjian village, Chunjiang street, Fuyang District, Hangzhou City, Zhejiang Province Patentee after: Hangzhou salamander Technology Co.,Ltd. Address before: 100080 Beijing Haidian District Zhongguancun North Street 127-1, 1 floor 107-10 room. Patentee before: Beijing salamander Technology Co.,Ltd. |
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