CN113208931A - Preparation method of dental tubule plugging material, product and application thereof - Google Patents
Preparation method of dental tubule plugging material, product and application thereof Download PDFInfo
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- CN113208931A CN113208931A CN202110684935.6A CN202110684935A CN113208931A CN 113208931 A CN113208931 A CN 113208931A CN 202110684935 A CN202110684935 A CN 202110684935A CN 113208931 A CN113208931 A CN 113208931A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/831—Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
- A61K6/838—Phosphorus compounds, e.g. apatite
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/20—Protective coatings for natural or artificial teeth, e.g. sealings, dye coatings or varnish
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
- C01B25/325—Preparation by double decomposition
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Abstract
The invention discloses a preparation method of a dental tubule plugging material, which comprises the following steps: preparing an ethanol solution of calcium salt with the concentration of 2-50 g/L as a solution A; preparing an ethanol solution containing 0.5-15 g/L of phosphoric acid compound and 10-600 g/L of triethylamine to be used as a solution B; mixing the solution A and the solution B, and standing to obtain a calcium phosphate ion oligomer solution C, wherein the mixing volume ratio of the solution A to the solution B is 2-10: 1; and centrifuging the calcium phosphate oligomer solution C, and then re-dispersing the calcium phosphate oligomer solution C in water to obtain an aqueous calcium phosphate oligomer solution D serving as a dental tubule plugging material. The invention also discloses the dental tubule plugging material prepared by the preparation method and application of the dental tubule plugging material in dental tubule plugging and dentin repair. The dental tubule plugging material provided by the invention can form a continuous plugging layer on the surface of dentin by means of smearing and the like, and is firmly combined on the surface of dentin, so that the plugging of the dental tubule is realized; the dentinal tubule material can help to restore the mechanical properties of the dentin, and is beneficial to the dentin to resist external stress.
Description
Technical Field
The invention relates to the technical field of dental prosthetic materials, in particular to a preparation method and application of a dental tubule plugging material.
Background
Dentin sensitivity, the most common of the oral diseases. Sensitive dentin is stimulated by external factors such as temperature, chemicals and mechanical action, which can cause symptoms such as soreness. Dentinal sensitivity is primarily a result of exposure to dentin as the integrity of the outer enamel is compromised. The occlusion of the dental tubule is an effective treatment measure for dentin sensitivity, but clinically used occlusion materials often contain toxic components, and only an ultrathin layer can be formed on the surface of the dentin, so that the occlusion materials are extremely easy to damage, and the treatment is ineffective.
In view of the fact that the main inorganic component of dentin is calcium phosphate, remineralization measures based on calcium phosphate are considered to be effective restorative measures. For example, chinese patent publication No. CN106890095A discloses a dental restorative material for promoting remineralization of dentin, which comprises a polypeptide solution and a nano amorphous calcium phosphate suspension sequentially applied to the surface of dentin. However, because of the limitations of conventional synthesis methods, calcium phosphates synthesized in the past are all powders, and it is difficult to obtain a continuous whole for plugging. So far, few direct restorative works have used laser-induced deposition, dentin modification-induced deposition, etc. to obtain a relatively integral occluding layer, but these methods take a long time, and the teeth are subject to complicated changes in oral environment every day, and these methods are difficult to be used clinically.
In conclusion, the calcium phosphate material is designed to directly realize rapid and effective continuous occlusion of the dental tubule, and has important significance in treating dentin hypersensitivity.
Disclosure of Invention
The invention aims to provide a preparation method of a dentin tubule plugging material, which takes water-phase calcium phosphate oligomer as a precursor, and the precursor can form a protective layer on the surface of dentin, can permeate into dentin tubules and is tightly combined with dentin, thereby realizing the plugging of the dentin and enhancing the mechanical property thereof.
The technical scheme adopted by the invention is as follows:
(1) preparing an ethanol solution of calcium salt with the concentration of 2-50 g/L as a solution A;
(2) preparing an ethanol solution containing 0.5-15 g/L of phosphoric acid compound and 10-600 g/L of triethylamine to be used as a solution B;
(3) mixing the solution A and the solution B, and standing to obtain a calcium phosphate ion oligomer solution C, wherein the mixing volume ratio of the solution A to the solution B is 2-10: 1;
(4) and (4) centrifuging the calcium phosphate oligomer solution C obtained in the step (3) and then re-dispersing the calcium phosphate oligomer solution C in water to obtain an aqueous calcium phosphate oligomer solution D serving as a dental tubule plugging material.
The calcium phosphate oligomer solution is dispersed in water to form a water-phase calcium phosphate oligomer solution which is then used as a tubule plugging material, so that the calcium phosphate oligomer plugging material has better biocompatibility; the solvent of the solution is water, and the solution can be quickly volatilized at room temperature, so that the solution is favorable for quick plugging application; the resulting material is fluid, easy to handle, and can conform to various shapes of tooth surfaces.
The calcium salt is one or more of calcium chloride, calcium nitrate, calcium citrate and the like, and the concentration of calcium ions in the solution A is 0.01-2 mol/L.
The phosphoric acid compound is one or more of phosphoric acid, sodium hydrogen phosphate, potassium hydrogen phosphate, ammonium hydrogen phosphate and the like, the concentration of the phosphoric acid in the solution B is 0.02-5 mol/L, and the concentration of triethylamine is 0.6-15 mol/L.
Preferably, the concentration of the calcium salt in the solution A is 5-20 g/L; the concentration of the phosphoric acid compound in the solution B is 2.5-6 g/L, and the concentration of triethylamine is 25-240 g/L.
In the step (3), the concentration of the calcium phosphate ion oligomer solution is 5-200 g/L.
In the step (4), the concentration of the aqueous calcium phosphate oligomer solution is 0.1-50 g/L. The reason for setting this concentration range is that the tubule blocking material in this range has fluidity.
The invention also discloses a dental tubule plugging material prepared by the preparation method.
The invention also discloses application of the dental tubule plugging material in dental tubule plugging and dentin repair.
The application method comprises the following steps:
(1) coating the aqueous calcium phosphate oligomer solution D on the pretreated dentin surface, and drying to obtain a calcium phosphate repair layer which covers the dentin surface and partially permeates dentin tubules;
(2) further curing the calcium phosphate repairing layer by the action of saliva or further curing the calcium phosphate repairing layer by coating mineralized liquid.
Wherein, the calcium phosphate repairing layer is further cured to enhance the mechanical property of the dentin.
In the step (2), the mineralized liquid is a hydroxyapatite saturated solution.
Specifically, in the step (1), the application method of the dental tubule plugging material of the invention is as follows: the dentin surface was uniformly coated with a cotton swab and air dried for 5 minutes.
The dental tubule plugging material provided by the invention is a water-phase calcium phosphate oligomer solution with fluidity, the main component is calcium phosphate, and the dental tubule plugging material has good biocompatibility; the continuous plugging layer can be quickly formed on the surface of the acid-etched dentin by means of smearing and the like, the mechanical property of the acid-etched dentin can be improved by the plugging material, and the formed continuous plugging layer can be firmly combined on the dentin substrate in a simulated oral cavity environment and a real oral cavity environment, so that quick and effective dentin desensitization is realized.
The invention has the following beneficial effects:
1. the invention has simple preparation and good controllability, and the main component of the invention is calcium phosphate which is the same as the tooth, thus having good biocompatibility.
2. The dental tubule plugging material is simple in use method, and can achieve a desensitization effect by being simply smeared.
3. The tubule plugging material can improve the mechanical property of dentin and help teeth resist external stress.
4. The tubule plugging material can be firmly combined on the surface of dentin, and has good use effect.
Drawings
Fig. 1 is a scanning electron microscope image of the coated tubule blocking material prepared in example 1 of the present invention on the surface of a tubule, wherein a is an acid-etched dentin surface and b is a coated dentin surface.
Fig. 2 is a scanning electron microscope image of the dentin surface coated with the tubule blocking material prepared in example 1 of the present invention after further aging for 2 days, in which a is the surface of the untreated dentin after being soaked in the phase change liquid for 2 days, and b is the surface of the dentin after being coated with the tubule blocking material and soaked in the phase change liquid for 2 days.
FIG. 3 is a load-displacement curve of the surface plugging layer after the dental tubule plugging material prepared in example 1 of the present invention is used for dental tubule plugging.
Fig. 4 is a scanning electron microscope image of the tubule blocking material prepared in example 1 of the present invention for testing the tubule blocking performance in an animal experiment, wherein a is the incisor teeth of a mouse ground to dentin, b is the surface of an untreated tooth after 2 days, c is the cross section of an untreated tooth after 2 days, d is the surface of a tubule blocked after 2 days, and e is the cross section blocked after 2 days.
Detailed Description
The invention will be further described with reference to the following figures and examples, to which, however, the scope of the invention is not limited.
Collecting non-carious in-vitro teeth, cutting off enamel and tooth roots by using a slow diamond slicer to be vertical to a long axis of the teeth to obtain dentin slices with the thickness of 0.5-1 mm, gradually polishing by using abrasive paper of No. 360-No. 3000, and cleaning by using deionized water; and (3) etching the obtained dentin sheet for 10-15 seconds by 37% phosphoric acid, washing with deionized water, and drying for later use.
Example 1
Preparing 1L of 2g/L calcium chloride ethanol solution as solution A; preparing 0.5L of ethanol solution containing 0.8g/L of phosphoric acid and 40g/L of triethylamine to be used as solution B; the solution A and the solution B were mixed at a volume ratio of 2:1 to obtain a calcium phosphate oligomer solution C. The calcium phosphate oligomer solution C was re-dispersed in 200mL of water after high speed centrifugation (10000rcf,5min) to obtain about 10g/L of an aqueous calcium phosphate oligomer solution as a dental tubule plugging material. Coating a layer of the obtained material on the surface of the acid-etched dentin by using a dental cotton swab, and drying to obtain a continuous calcium phosphate blocking layer. And then soaking the blocked dentin sample in artificial simulated saliva, putting the sample in a water bath box at 37 ℃ for mineralization for 2 days, taking the sample out, putting the sample in clear water for ultrasonic cleaning for 5 minutes, and drying the sample for scanning electron microscope observation and nano indentation test.
Example 2
Preparing 1L of 5g/L calcium chloride ethanol solution as solution A; preparing 0.5L of ethanol solution containing 2g/L of phosphoric acid and 100g/L of triethylamine to be used as solution B; the solution A and the solution B were mixed at a volume ratio of 2:1 to obtain a calcium phosphate oligomer solution C. The calcium phosphate oligomer solution C was re-dispersed in 200mL of water after high speed centrifugation (10000rcf,5min) to obtain about 25g/L of an aqueous calcium phosphate oligomer solution as a dental tubule plugging material. Coating a layer of the obtained material on the surface of the acid-etched dentin by using a dental cotton swab, and drying to obtain a continuous calcium phosphate blocking layer. And then soaking the blocked dentin sample in artificial simulated saliva, putting the sample in a water bath box at 37 ℃ for mineralization for 2 days, taking the sample out, putting the sample in clear water for ultrasonic cleaning for 5 minutes, and drying the sample for scanning electron microscope observation and nano indentation test.
Example 3
Preparing 1L of 10g/L calcium chloride ethanol solution as solution A; preparing 0.5L of ethanol solution containing 4g/L of phosphoric acid and 200g/L of triethylamine to be used as solution B; the solution A and the solution B were mixed at a volume ratio of 2:1 to obtain a calcium phosphate oligomer solution C. The calcium phosphate oligomer solution C was re-dispersed in 200mL of water after high speed centrifugation (10000rcf,5min) to obtain about 50g/L of an aqueous calcium phosphate oligomer solution as a dental tubule plugging material. Coating a layer of the obtained material on the surface of the acid-etched dentin by using a dental cotton swab, and drying to obtain a continuous calcium phosphate blocking layer. And then soaking the blocked dentin sample in artificial simulated saliva, putting the sample in a water bath box at 37 ℃ for mineralization for 2 days, taking the sample out, putting the sample in clear water for ultrasonic cleaning for 5 minutes, and drying the sample for scanning electron microscope observation and nano indentation test.
Mineralization in examples 1-3 aboveThe solution contained 1.67mM CaCl2,9.5mM Na2PO4150mM NaCl and 20mM 4-hydroxyethylpiperazine ethanesulfonic acid, and the pH of the solution was maintained at around 7.0.
According to the chemical components of the mineralized liquid, calcium salt and phosphate with other concentrations can be adopted to prepare the mineralized liquid.
In order to verify the beneficial effects of the present invention, the inventor performed various performance tests on the dental tubule plugging material prepared in example 1, the specific tests are as follows:
in example 1, the acid etched dentin surface was as shown in fig. 1a, exposing a small dentinal hole; dentin after application of an aqueous calcium phosphate oligomer solution and drying thereof is shown in fig. 1b, it can be seen that the continuous blocking layer formed covers most of the dentinal pores.
In example 1, the dentin surface after immersion of untreated, acid-etched dentin in a mineralized solution for 2 days is shown in fig. 2a, and the dentin surface after treatment with a tubule plugging material for 2 days and further aging is shown in fig. 2b, and it can be seen that after ultrasonic treatment, the calcium phosphate plugging layer is still firmly bonded to the dentin surface, indicating the reliability of the plugging material.
The mechanical characterization of the dentin subjected to plugging in example 1 was performed, and the load-displacement curve of the prepared tubule plugging material used for the surface plugging layer after the tubule plugging is shown in fig. 3, wherein the curve "natural" refers to natural dentin, the curve "acid etching" refers to dentin subjected to acid etching, and the curve "treatment" refers to dentin treated by the method. The hardness of natural dentin is calculated
1.02 +/-0.12 GPa and the elastic modulus of 30.86 +/-3.55 GPa; the hardness of the dentin after acid etching is 0.07 +/-0.01 GPa, the elastic modulus is 3.89 +/-0.56 GPa, and the mechanical property is greatly reduced; the hardness of the processed dentin is 0.58 +/-0.04 GPa, and the elastic modulus is 23.95 +/-3.65 GPa. Therefore, the used tubule plugging material can greatly improve the mechanical property of dentin.
The tubule blocking material prepared in example 1 was used in animal experiments, coated on exposed dentin of rats (fig. 4a), and taken out for observation after 2 days. And untreated acid-etched dentin groups were used as control experiments. From fig. 4b, it can be seen that the untreated dentinal surface is not significantly altered, while the sectional view of fig. 4c also shows that the tubules are still exposed; whereas from the dentin surface view of fig. 4d it can be seen that the occluding layer covers most of the tubules and from the cross-sectional view of fig. 4e it can be seen that the occluding layer is continuous. Animal experiments further prove that the dental tubule plugging material can realize continuous plugging of dental tubules and does not fall off in a daily chewing environment, so that a desensitizing effect is realized.
Claims (9)
1. A preparation method of a dental tubule plugging material is characterized by comprising the following steps:
(1) preparing an ethanol solution of calcium salt with the concentration of 2-50 g/L as a solution A;
(2) preparing an ethanol solution containing 0.5-15 g/L of phosphoric acid compound and 10-600 g/L of triethylamine to be used as a solution B;
(3) mixing the solution A and the solution B, and standing to obtain a calcium phosphate ion oligomer solution C, wherein the mixing volume ratio of the solution A to the solution B is 2-10: 1;
(4) and (4) centrifuging the calcium phosphate oligomer solution C obtained in the step (3) and then re-dispersing the calcium phosphate oligomer solution C in water to obtain an aqueous calcium phosphate oligomer solution D serving as a dental tubule plugging material.
2. The method for preparing a dental tubule blocking material according to claim 1, wherein in step (1), the calcium salt is selected from one or more of calcium chloride, calcium nitrate or calcium citrate, and the concentration of calcium ion in solution A is 0.01-2 mol/L.
3. The method for preparing a dental tubule blocking material according to claim 1, wherein in the step (2), the phosphoric acid compound is selected from any one or more of phosphoric acid, sodium hydrogen phosphate, potassium hydrogen phosphate and ammonium hydrogen phosphate, the concentration of phosphoric acid in the solution B is 0.02 to 5mol/L, and the concentration of triethylamine is 0.6 to 15 mol/L.
4. The method for preparing a dental tubule blocking material according to claim 1, wherein the concentration of the calcium phosphate ionic oligomer solution in step (3) is 5 to 200 g/L.
5. The method for preparing a dental tubule blocking material according to claim 1, wherein the concentration of the aqueous calcium phosphate oligomer solution in step (4) is 0.1 to 50 g/L.
6. A dental tubule blocking material obtained by the production method according to any one of claims 1 to 5.
7. Use of a dental tubule blocking material according to claim 6 for tubule blocking and dentin restoration.
8. Use of a dental tubule blocking material according to claim 7 for tubule blocking and dentin restoration, characterized in that the method of application comprises:
(1) coating the aqueous calcium phosphate oligomer solution D on the pretreated dentin surface, and drying to obtain a calcium phosphate repair layer which covers the dentin surface and partially permeates dentin tubules;
(2) further curing the calcium phosphate repairing layer by the action of saliva or further curing the calcium phosphate repairing layer by coating mineralized liquid.
9. The use of a dental tubule blocking material according to claim 8 for tubule blocking and dentin restoration, wherein in step (2) the mineralized solution is a saturated solution of hydroxyapatite.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113995682A (en) * | 2021-11-04 | 2022-02-01 | 浙江大学 | Application of tooth restoration composition in tooth restoration |
| CN114795974A (en) * | 2022-01-21 | 2022-07-29 | 武汉大学 | Composition for repairing demineralized dentin and preparation method and application thereof |
| CN115120775A (en) * | 2022-07-07 | 2022-09-30 | 中国人民解放军国防科技大学 | Bone repair scaffold material and preparation method and application thereof |
| CN115414527A (en) * | 2022-05-16 | 2022-12-02 | 浙江大学 | Bionic bone-like composite scaffold, preparation method and application of bionic bone-like composite scaffold in rapid repair of bone defects |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113995682A (en) * | 2021-11-04 | 2022-02-01 | 浙江大学 | Application of tooth restoration composition in tooth restoration |
| CN114795974A (en) * | 2022-01-21 | 2022-07-29 | 武汉大学 | Composition for repairing demineralized dentin and preparation method and application thereof |
| CN115414527A (en) * | 2022-05-16 | 2022-12-02 | 浙江大学 | Bionic bone-like composite scaffold, preparation method and application of bionic bone-like composite scaffold in rapid repair of bone defects |
| CN115120775A (en) * | 2022-07-07 | 2022-09-30 | 中国人民解放军国防科技大学 | Bone repair scaffold material and preparation method and application thereof |
| CN115120775B (en) * | 2022-07-07 | 2023-12-22 | 中国人民解放军国防科技大学 | Bone repair stent material and preparation method thereof |
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Application publication date: 20210806 |