CN113041161A - Precursor solution and method for repairing demineralized dentin and sealing dentin tubule - Google Patents
Precursor solution and method for repairing demineralized dentin and sealing dentin tubule Download PDFInfo
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- CN113041161A CN113041161A CN202110346408.4A CN202110346408A CN113041161A CN 113041161 A CN113041161 A CN 113041161A CN 202110346408 A CN202110346408 A CN 202110346408A CN 113041161 A CN113041161 A CN 113041161A
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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
- A61K6/884—Preparations for artificial teeth, for filling teeth or for capping teeth comprising natural or synthetic resins
- A61K6/887—Compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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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
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/884—Preparations for artificial teeth, for filling teeth or for capping teeth comprising natural or synthetic resins
- A61K6/891—Compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention discloses a precursor solution and a method for repairing demineralized dentin and sealing dentin tubules, belonging to the technical field of biological materials. The invention can repair demineralized dentin and seal dentinal tubules, takes overgrowth mineralization based on collagen internal mineralization as a strategy, is a polymer-induced calcium phosphate liquid-phase mineralization precursor, and comprises the components of polymer, calcium phosphate and sodium chloride. The preparation method of the liquid-phase mineralized precursor comprises the following steps: respectively preparing a calcium-containing mother liquor and a phosphorus-containing mother liquor, dropwise adding a certain amount of polyaspartic acid solution into the calcium-containing solution, gently mixing uniformly, adding a phosphorus-containing solution with the same volume as the calcium-containing solution, and mixing uniformly. The invention has the advantages of easily obtained raw materials and simple and convenient process, and can repair demineralized dentin and deeply seal dentinal tubules.
Description
Technical Field
The invention belongs to the technical field of biological materials, and particularly relates to a precursor solution and a method for repairing demineralized dentin and sealing dentin tubules.
Background
Dentinal hypersensitivity is a common clinical symptom. Its prevalence varies from 3% to 98% of the global population. It is a transient and sharp pain caused by exposure of dentinal tubules to temperature, tactile, osmotic or chemical stimuli and may even seriously affect the quality of life of the patient. According to the hydrodynamics, reducing the diameter of dentinal tubules, occluding the dentinal tubules, is an effective treatment for dentinal hypersensitivity.
The traditional desensitizer widely used in clinic at present is difficult to obtain lasting and effective treatment effect. For example, the mouth of the tubule and the surface of the dentin are only covered with a thin layer of the dolefluoride and the grulmar, and although the noriflamine and the nano-hydroxyapatite can enter the dentin tubule with a certain depth, the binding force between the noriflamine and the dentin is poor, so the dolefluoride and the grulmar are easy to fall off under the action of mechanical force such as tooth brushing and the like. Thus, deep, firm occlusion of dentinal tubules is a method of long-lasting treatment of dentinal hypersensitivity. In addition, the patent granted so far has been an invention for achieving occlusion of dentinal tubules by simple inorganic mineral deposition or oligomer surface modification. These inventions all have the same disadvantage of loose bonding between the intra-tubular occlusion and the dentinal collagen fibers.
The polymer-induced liquid phase precursor is an amorphous liquid phase mineral precursor stabilized by a charged polymer, such as polyaspartic acid, polyallylamine hydrochloride, or polyacrylic acid, which can sequester ions to induce or stabilize nanodroplets. The fluid nature of this amorphous precursor phase enables it to be drawn into the nano-scale interstices and grooves of collagen fibrils by capillary action or the Gibbs-Donnan effect. The precursor solidifies into amorphous calcium phosphate and crystallizes into hydroxyapatite, thereby producing a large amount of ordered intrafiber minerals.
Therefore, it is desirable to provide a polymer-induced liquid phase precursor that is capable of repairing demineralized dentin and occluding dentinal tubules.
Disclosure of Invention
The invention aims to solve the problems of dentinal desensitization in the prior art and provides a precursor solution and a method for repairing demineralized dentin and sealing dentinal tubules. The invention simulates natural mineralization, utilizes a polymerization non-induction liquid-phase precursor to induce the overgrowth of ordered minerals by mineralization in collagen, and finally realizes the tubule closure, and the mineral which extends out from the collagen and grows in order is tightly combined with the collagen, so that the tubule closure is firmer and more stable.
In order to achieve the purpose, the invention adopts the following specific technical scheme:
in one aspect, the invention provides a method for preparing a precursor solution for repairing demineralized dentin and sealing dentin tubules, which comprises the following steps:
s1: respectively preparing a polymer solution, a calcium-containing mother liquor and a phosphorus-containing mother liquor; the calcium-containing mother liquor is a calcium chloride aqueous solution, and the phosphorus-containing mother liquor is a mixed aqueous solution of disodium hydrogen phosphate and sodium chloride;
s2: and adding the polymer solution into the calcium-containing mother liquor, uniformly mixing, adding the phosphorus-containing mother liquor, and uniformly mixing to obtain a precursor solution for repairing demineralized dentin and sealing dentin tubules.
Preferably, the polymer solution is an aqueous solution of polyaspartic acid, polyallylamine, or polyacrylic acid.
Preferably, the polymer solution is an aqueous polyaspartic acid solution.
Preferably, the concentration ratio of the disodium hydrogen phosphate to the sodium chloride is 3: 50-2: 3.
Preferably, in the precursor solution for repairing demineralized dentin and sealing dentin tubules, the concentration of the polymer is 10-600 mu g/mL, and Ca is contained2+In a concentration of 1 to 10mM, PO4 3-The concentration of (B) is 5 to 15 mM.
In another aspect, the present invention provides a precursor solution for repairing demineralized dentin and occluding dentinal tubules, prepared according to any one of the above-described preparation methods.
Compared with the prior art, the invention has the following beneficial effects:
1) the invention uses polyaspartic acid in calcium phosphate solution to stabilize amorphous calcium phosphate precursor phase, promotes amorphous calcium phosphate to infiltrate collagen fibril, promotes collagen mineralization in vivo, and thereby restores demineralized dentin.
2) The precursor solution of the invention has simple system, easily obtained raw materials, simple preparation method and batch production.
3) The precursor solution can enter the deep part of a small tube due to the flow state characteristic, can be drawn into nano-scale gaps and grooves of collagen fibrils through the capillary action or the Gibbs-Donnan effect, and then is crystallized into hydroxyapatite to generate a large amount of orderly-arranged intrafiber minerals so as to realize collagen mineralization; the collagen inner mineral is further deduced to be collagen over-mineralization, and the mineralization result obtained by the mineralization process is bionic and ordered.
Drawings
FIG. 1 is an SEM image (x 2000) of the surface topography of a dentin demineralization desensitization model after immersion in the precursor solution of example 1 for days 0 and 14.
Fig. 2 is a longitudinal sectional SEM image (x 3000) of a dentin demineralization desensitization model after immersion in the precursor solution of example 1 for days 0 and 14.
Fig. 3 shows xrd (a) and atr (b) results of healthy Dentin (Dentin), Dentin demineralization desensitization model (Acid-unreacted Dentin), and Dentin demineralization desensitization model after 14 days immersion in the precursor solution of example 1 (Remineralization).
Fig. 4 shows the nanoindentation hardness (a) and the elastic modulus (b) of the surface of healthy Dentin (Dentin), Dentin demineralization desensitization model (Acid-unreacted Dentin), and Dentin demineralization desensitization model after being immersed in the precursor solution in example 1 for 14 days (Remineralization).
Fig. 5 is an SEM image (x 2000) of the surface topography of the dentin demineralization desensitization model after 14 days immersion in the precursor solution of example 1, before (a) and after (b) sonication.
Detailed Description
The invention will be further elucidated and described with reference to the drawings and the detailed description. The technical features of the embodiments of the present invention can be combined correspondingly without mutual conflict.
The invention provides a liquid-phase mineralized precursor (precursor solution) for repairing demineralized dentin and sealing dentin tubules, and the preparation method of the precursor solution comprises the following steps:
s1: respectively preparing a polymer solution, a calcium-containing mother liquor and a phosphorus-containing mother liquor. In practical application, the polymer solution can adopt an aqueous solution of polyaspartic acid, polyallylamine or polyacrylic acid, and preferably an aqueous solution of polyaspartic acid; the calcium-containing mother liquor can adopt calcium chloride aqueous solution, and the phosphorus-containing mother liquor can adopt mixed aqueous solution of disodium hydrogen phosphate and sodium chloride.
S2: adding the prepared polymer solution into the obtained calcium-containing mother liquor, uniformly mixing the calcium-containing mother liquor and the polymer solution, then adding the phosphorus-containing mother liquor, and uniformly mixing the three to obtain the precursor solution capable of repairing demineralized dentin and sealing dentin tubules.
The precursor solution contains polymer with concentration of 10-600 mu g/mL and Ca2+In a concentration of 1 to 10mM, PO4 3-The concentration of (B) is 5 to 15 mM.
Example 1
(1) Anhydrous calcium chloride is used as a solute, deionized water is used as a solvent, and a calcium chloride solution with the concentration of 3.34mM is prepared to be used as a calcium-containing mother solution.
(2) Disodium hydrogen phosphate and sodium chloride are used as solutes, and deionized water is used as a solvent to prepare the phosphorus-containing mother liquor. In the phosphorus-containing mother liquor, the concentration of disodium hydrogen phosphate was 19mM and the concentration of sodium chloride was 300 mM.
(3) Polyaspartic acid solution with the concentration of 10mg/mL is prepared by using polyaspartic acid as solute and deionized water as solvent.
(4) Adding the prepared polymer solution into the obtained calcium-containing mother liquor, uniformly mixing the calcium-containing mother liquor and the polymer solution, then adding the phosphorus-containing mother liquor, and uniformly mixing the three to obtain a precursor solution (a calcium phosphate liquid-phase precursor induced by polyaspartic acid) capable of repairing demineralized dentin and sealing dentin tubules. Wherein, the calcium-containing mother liquor, the polyaspartic acid solution and the phosphorus-containing mother liquor are mixed in a ratio of 125: 6: 125, are mixed.
(5) Collecting non-carious in-vitro teeth, cutting dentin slices (without enamel and pulp tissues) with the pulp chamber top thickness of 0.8-1.2 mm by using a slow-speed slicer perpendicular to the long axis of the teeth, and polishing by using 1200-mesh silicon carbide abrasive paper to generate a uniform stain layer. And then soaking the obtained dentin sheet in 6% citric acid solution for 2min, washing with a large amount of deionized water, and then carrying out ultrasonic treatment for 15min to obtain a dentin demineralization desensitization model.
(6) Taking 10mL of the precursor solution obtained in step (4) into an incubator, and then placing the dentin demineralization desensitization model prepared in step (5) into the incubator.
(7) And (3) placing the culture bottle filled with the precursor solution and the dentin demineralization desensitization model in the step (6) in a constant temperature box at 37 ℃, taking out the culture bottle at days 1, 4, 7 and 14 respectively, and carrying out observation, data detection and data acquisition, wherein the results are as follows:
as shown in fig. 1, is an SEM image (x 2000) of the surface topography of the dentinal demineralization desensitization model after 0 and 14 days immersion in the precursor solution of example 1, from which it can be seen that the dentinal tubules at day 14 have been completely enclosed by dense minerals.
As shown in fig. 2, which is a longitudinal sectional SEM image (x 3000) of the dentin demineralization desensitization model after soaking in the precursor solution of example 1 for 0 th and 14 th days, it can be seen that the dentin surface of 14 th day is covered by a dense mineral protective layer with a thickness of about 1.5-4 microns, and the tubules are also completely enclosed by deposited mineral crystals to a depth of 20 microns; the boundaries between the dentin surface and the mineral deposited in the tube and dentin were unclear, indicating that the bond between the two was strong.
As shown in FIG. 3, XRD (a) and ATR (b) results of healthy Dentin (Dentin), Dentin demineralization desensitization model (Acid-unreacted Dentin) and Dentin demineralization desensitization model after soaking in the precursor solution of example 1 for 14 days (Remineralization), it can be seen that the XRD results show characteristic diffraction peaks of the mineralized layer at 002, 211 and 300, and the ATR results show that typical O-P-O oscillation peaks at 556cm-1And P-O stretching vibration at 1017cm-1The mineral protective layer on the dentinal surface at day 14 was shown to be HAp.
As shown in fig. 4, after the precursor solution in example 1 is soaked for 14 days, the nano indentation hardness (a) and the elastic modulus (b) of the surface of the precursor solution are statistically analyzed, and the Dentin hardness and the elastic modulus of the precursor solution at day 14 are both restored to the level of healthy Dentin, which is significantly higher than that of desensitized demineralized Dentin (Dentin demineralization desensitization model).
(8) And (3) carrying out ultrasonic treatment on the remineralized dentin sheet (obtained after soaking the dentin demineralization desensitization model in the precursor solution for 14 days) obtained in the step (7) for 15min, and carrying out observation, data detection and data acquisition, wherein the result is shown in figure 5.
As shown in fig. 5, which is an SEM image (x 2000) of the surface topography of the dentin demineralization desensitization model before (a) and after (b) the ultrasonic treatment after soaking in the precursor solution of example 1 for 14 days, it can be seen that the mineral protective layer on the dentin surface could not be removed by the ultrasonic treatment, indicating that the bonding force between the precursor solution of the present invention and the dentin surface is strong.
The experiments and data show that the precursor solution can penetrate into the deep layer of the dentinal tubule due to the flow state characteristic, and hydroxyapatite crystals are orderly deposited by performing the deduction from mineralization in collagen to overgrowth mineralization, so that the dentinal tubule is more firmly sealed, and the stability is better.
The above-described embodiments are merely preferred embodiments of the present invention, which should not be construed as limiting the invention. Various changes and modifications may be made by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present invention. Therefore, the technical scheme obtained by adopting the mode of equivalent replacement or equivalent transformation is within the protection scope of the invention.
Claims (6)
1. A preparation method of a precursor solution for repairing demineralized dentin and sealing dentin tubules is characterized by comprising the following steps:
s1: respectively preparing a polymer solution, a calcium-containing mother liquor and a phosphorus-containing mother liquor; the calcium-containing mother liquor is a calcium chloride aqueous solution, and the phosphorus-containing mother liquor is a mixed aqueous solution of disodium hydrogen phosphate and sodium chloride;
s2: and adding the polymer solution into the calcium-containing mother liquor, uniformly mixing, adding the phosphorus-containing mother liquor, and uniformly mixing to obtain a precursor solution for repairing demineralized dentin and sealing dentin tubules.
2. The method of claim 1, wherein the polymer solution is an aqueous solution of polyaspartic acid, polyallylamine, or polyacrylic acid.
3. The method of claim 1, wherein the polymer solution is an aqueous polyaspartic acid solution.
4. The method for preparing the precursor solution according to claim 1, wherein the concentration ratio of the disodium hydrogen phosphate to the sodium chloride is 3: 50 to 2: 3.
5. The method for preparing the precursor solution according to claim 1, wherein the concentration of the polymer in the precursor solution for repairing demineralized dentin and sealing dentinal tubules is 10-600 μ g/mL, Ca2+In a concentration of 1 to 10mM, PO4 3-The concentration of (B) is 5 to 15 mM.
6. A precursor solution for repairing demineralized dentin and sealing dentinal tubules prepared according to the preparation method of any one of claims 1 to 5.
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Cited By (2)
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| CN115300398A (en) * | 2022-08-10 | 2022-11-08 | 北京大学口腔医学院 | Method for promoting remineralization of demineralized dentin |
| CN116999335A (en) * | 2023-08-08 | 2023-11-07 | 南昌大学附属口腔医院(江西省口腔医院) | Nanometer hybrid material for dental hard tissue repair and preparation method and application thereof |
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Application publication date: 20210629 |