CN107997972B - Material for in-situ generation of calcium phytate to seal dentinal lumen and application thereof - Google Patents

Material for in-situ generation of calcium phytate to seal dentinal lumen and application thereof Download PDF

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CN107997972B
CN107997972B CN201711261804.7A CN201711261804A CN107997972B CN 107997972 B CN107997972 B CN 107997972B CN 201711261804 A CN201711261804 A CN 201711261804A CN 107997972 B CN107997972 B CN 107997972B
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reagent
calcium
root canal
dentin
lumen
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张祖太
李永梅
丁宁
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Huazhi Medical Equipment Beijing Co ltd
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Beijing Stomatological Hospital
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00Preparations for dentistry
    • A61K6/50Preparations specially adapted for dental root treatment
    • A61K6/54Filling; Sealing
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00Preparations for dentistry
    • A61K6/80Preparations for artificial teeth, for filling teeth or for capping teeth

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Abstract

A material for sealing dentinal lumen by in-situ generation of calcium phytate and application thereof, belonging to the technical field of dental materials. Comprises an acid solution of calcium phytate as a reagent A. The reagent B is alkaline solution of calcium hydroxide, potassium hydroxide, sodium hydroxide, etc. The reagent A is coated on the surface of exposed dentin or placed in a root canal, the reagent A enters the inside of a dentin tubule, a lateral branch root canal and the like and can reach an apical pore along the root canal, and then the reagent B is coated, so that calcium phytate precipitate can be generated in an acidic solution of calcium phytate in the dentin tubule, the lateral branch root canal or the apical pore along with the increase of the pH value, and the dentin tubule, the lateral branch root canal or the apical pore is blocked. Hydrophilic components such as ethanol, ethylene glycol and acetone can be added into the reagent A or the reagent B to improve the permeability of the reagent A or the reagent B and further seal dentinal tubules, collateral roots and apical pores. Elements such as silicon-containing compounds and the like can also be added into the reagent B to assist in inducing calcium salt deposition in oral cavities and tissues, and further seal dentinal tubules, collateral roots and apical pores.

Description

Material for in-situ generation of calcium phytate to seal dentinal lumen and application thereof
Technical Field
The invention belongs to the technical field of oral cavity dental restoration, and relates to a material for blocking dentinal tubules, lateral branch root canals or apical foramens by generating calcium phytate precipitates in the dentinal tubules, the lateral branch root canals or the apical foramens and an application method thereof.
Background
Exposed dentin is associated with dentin hypersensitivity, the occurrence of pulpitis, dentin adhesion, and the like. With the continuous development of science and technology, new dentin sealing materials are continuously made available. Although numerous techniques disclose the use of combinations of various materials for treating dentinal hypersensitivity, improving cavity filling, etc., there remains a need to provide more effective materials and methods.
Recent approaches to sealing dentin have focused on the use of physicochemical methods to seal open dentinal tubules by remineralization of inorganic precipitates, solidification of organic materials, or laser surface melting. At present, most of the sealing agents form a protective barrier on the exposed dentin surface or are solidified after being infiltrated by organic resin and other materials, the long-term effect of the sealing agents is not ideal, and complex environmental factors in the oral cavity such as large temperature difference in the oral cavity, salivary enzyme, mechanical friction during tooth brushing and chewing and the like can act on the sealing layer along with the prolonging of time, so that the long-term curative effect of sealing is influenced.
The root canal system is composed of a main root canal and a lateral branch root canal, and also comprises a root apex bifurcation, a root canal traffic branch, a bent root canal and the like, and the structure of the root canal system is very complex. It is reported that the existence of collateral root canals, root canal branches and the like is one of the important factors influencing the success of the root canal treatment, so whether the root canal system can be strictly and completely closed is the key of the success of the root canal treatment, and the root canal filling material directly influences the perfection of the root canal filling. A good root canal filling material should have the ability to seal the canal walls and apical pores, adapting to the different shapes and contours of each root canal. The traditional root canal filling material is mainly gutta-percha material, gaps exist among the gutta-percha, the sealant and the canal wall after the root canal is filled, and the generated micro-leakage is a main factor influencing the success of the root canal treatment. The cold gutta-percha lateral pressure filling technology has the defects of uneven texture, poorer adaptability with the root canal wall, incapability of tightly sealing the whole root canal system and the like, and can generate larger wedge force in the lateral pressurizing process, thereby easily causing the longitudinal crack of the root canal. The existing hot gutta-percha root canal filling technology still has the defect that the entering length of the gutta-percha tip cannot be accurately controlled like the cold gutta-percha filling technology, and in addition, the gutta-percha and the paste easily exceed the apical foramen due to the fluidity of the hot gutta-percha.
Phytic acid (also known as phytic acid (IP 6)) is a naturally occurring organic compound containing phosphorus, has 6 negatively charged phosphate groups (shown in structural formula a) in the molecule, which can be complexed with metals, has a strong chelating ability, and when combined with a calcium source, calcium phytate (shown in structural formula B) is easily formed, which has been widely used in the medical field and can promote metabolism of the human body. It is reported that taking calcium phytate can build up body, and has the effects of nourishing brain, treating neurasthenia, improving sleep, preventing and treating child building restraint, strengthening liver, protecting liver, promoting growth, preventing aging, etc. In addition, phytic acid can also generate insoluble compounds with metal ions such as calcium, iron, magnesium, zinc and the like, so that the effectiveness of the metal ions is reduced, the degradation of collagen fibers in dentin can be prevented, and the stability of the dentin is enhanced. Can be effectively matched with protein molecules, thereby reducing the digestibility of the protein and being effectively combined with the dentin collagen fibers. Phytic acid, metal ions and proteins form ternary complexes with very low solubility, which facilitates the binding of calcium phytate to dentin.
Figure BDA0001493717540000021
The technology of the invention adopts a solution method, the calcium phytate solution can effectively permeate into dentinal tubules, lateral branch root canals, apical foramen and the like, and precipitates such as calcium phytate and the like are generated by adjusting the pH value, so that the in-situ sealing of the lumen is realized. In addition, calcium phytate can provide a large amount of calcium and phosphorus ions, induce calcium salt deposition and further seal the lumen.
Disclosure of Invention
The invention adopts the technology that the calcium phytate solution is infiltrated into dentin tubules, root canals, apical foramen, lateral branch root canals, root canal traffic branches and the like, and then calcium phytate precipitate is formed along with the change of the pH value to realize in-situ sealing.
The invention provides a material for in-situ formation of mineral deposits in a dentin lumen, which is characterized by comprising an independent reagent A and an independent reagent B; the reagent A is 1-70% calcium phytate acidic aqueous solution by mass, the reagent B is alkaline solution, preferably alkaline aqueous solution of calcium hydroxide, potassium hydroxide, sodium hydroxide and the like, and the pH value of the alkaline aqueous solution is more than 7 and less than or equal to 12.
Generally, calcium phytate is dissolved in water when the pH value is less than 4. The acidity of the calcium phytate acidic aqueous solution is to dissolve calcium phytate in water, and the calcium phytate acidic aqueous solution is harmless to human bodies or has as low acidity as possible.
Furthermore, one or more hydrophilic components such as ethanol, ethylene glycol and acetone can be added into the reagent A or the reagent B to improve the permeability of the reagent A or the reagent B, so as to further seal dentinal tubules, collateral roots and apical pores. The hydrophilic component accounts for not more than 5 percent by volume.
Further, a silicon-containing compound may be added to the reagent B, for example, the silicon-containing mass fraction is 0.5X 10-6Na of (2)2SiO3And) inducing calcium salt deposition in the oral cavity and tissues to further seal dentinal tubules, collateral roots and apical pores.
The preparation method of the material for in-situ formation of mineral deposits in the dentin lumen comprises the following steps: (1) the preparation of the reagent A comprises the following steps: placing calcium phytate in deionized water, and adjusting the pH value with hydrochloric acid; or dissolving calcium salt such as calcium chloride or calcium carbonate in phytic acid to fully dissolve; (2) the preparation of the reagent B comprises the following steps: dissolving alkaline substances such as calcium hydroxide, potassium hydroxide and sodium hydroxide in deionized water to prepare alkaline solution.
When the reagent A is used, the reagent A is directly coated or placed on the exposed dentin surface or in a root canal, can dissolve a contamination layer on the dentin surface and flows into the inner part or a deep layer of a dentin tubule, a root canal, a apical pore, a lateral branch root canal, a root canal traffic branch and the like, and then the reagent B is coated, so that the pH value of the reagent A is increased, calcium phytate precipitate is generated, and the dentin tubule, the root canal, the apical pore, the lateral branch root canal and the root canal traffic branch are blocked. Before use, the dentin sample can be subjected to acid etching cleaning treatment, so that dentin tubules are fully exposed.
The time for coating the agent A on the dentin surface is 5-300 seconds, and the agent A can be coated for multiple times.
The time for coating the agent B on the dentin surface is 5-300 seconds, and the agent B can be coated for multiple times.
In multiple applications, reagent A and reagent B may be coated alternately to allow more complete precipitation.
Applying agent A directly to the tooth surface of the exposed dentin, which dissolves the stained layer on the surface of the dentin and flows into the inside or deep layer of the dentin tubules; before use, the exposed dentin can be subjected to acid etching cleaning treatment to fully expose the dentin tubules, and the reagent A is coated on the tooth surface of the exposed dentin tubules to smoothly flow into the inside or deep layer of the dentin tubules. Then alkaline solution B is coated on the surface of dentin, the PH value of reagent A is increased, calcium phytate is precipitated, and dentin tubules are blocked.
The reagent A is put into the tooth root canal, so that the reagent A smoothly flows into the apical foramen, the lateral branch root canal, the root canal traffic branch and the like, and then the alkaline reagent B is added into the root canal, so that the pH value of the reagent A is changed, calcium phytate is precipitated, and the lateral branch root canal, the root canal traffic branch and the apical foramen are blocked.
The invention is based on the fact that the pH value of the system changes to cause the calcium phytate to precipitate, the solution of the reagent A smoothly permeates into the cavity of the tooth dentin, and the calcium phytate and other precipitates are formed after the reagent B is coated to block the cavity. And the calcium phytate precipitate is blocked in the dentinal lumen, so that falling and damage caused by external mechanical friction are avoided, remineralization can be induced in vivo, and the lumen is further sealed. The method for sealing dentinal tubules, collateral root canals and apical foramen can be used for treating dentin hypersensitivity, improving adhesion, and improving root canal therapy.
Drawings
FIG. 1 SEM image of a dentin sample acid etched before using the reagent in example 1;
FIG. 2 SEM image of coated agents after dentin acid etching of example 1;
FIG. 3 SEM photograph of dentinal tubules after application of the agent in example 1;
FIG. 4 SEM photograph of dentin of example 1 after 7 days using the coating agent
Wherein the left and right figures in fig. 1-4 are all of different scale dimensions.
Fig. 5 is an optical microscope (left) SEM (right) view of the agent embedded in the root canal of example 2.
Specific examples of the experiments
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1: dentinal tubule occlusion (tubules invisible to the naked eye)
The method comprises the following steps: 6 human premolars (6 teeth are milled) which are complete in dental crowns, free of caries and cracks and are freshly extracted due to orthodontics in oral cavity and maxillofacial surgery of institute of medical sciences, university of capital medical science and university of capital (patients agree with the consent, root surface soft tissue residues are removed by a curette after extraction, 4 ℃ physiological saline is stored for later use, the time is not more than 4 weeks), tooth roots are embedded by self-setting resin, occlusal surface enamel is milled, and dentin slices which are perpendicular to a long axis of teeth and are cut into 1.5mm in thickness are used as test pieces for later use.
Equipment: scanning electron microscopy (Phenom proX, Phenom-World B.V., the Netherlands), metallographic specimen pre-mill (YM-2A, Shanghai metallographical mechanical equipment Co., Ltd.), low speed cutter (Isomet 4000line Precision Saw, Buehler, USA);
materials: self-setting methyl methacrylate-based resin (dental materials factory, Shanghai medical instruments GmbH; self-setting resin for short), acid etching agent (Gruma, Germany);
preparing a reagent A: dissolving calcium phytate in deionized water, adjusting the pH value to 3.5-4 by hydrochloric acid, and preparing a reagent B: dissolving sodium hydroxide in deionized water to prepare sodium hydroxide solution, and adjusting the pH value to 8-10.
Before use, the dentin sample is subjected to 37% phosphoric acid etching for 30s, washed for 15 s and then naturally dried, dentin tubules are fully exposed, and the observation is carried out by an electron microscope. Coating the reagent A on the surface of a dentin sample, naturally drying for 1min, then coating the reagent B, naturally drying for 10 min, cleaning the tooth surface with deionized water, removing redundant substances and the like, and observing by using an electron microscope. Soaking artificial saliva for 7 days, and observing by an electron microscope.
The results are shown in FIGS. 1-4.
As can be seen from fig. 1: fully exposing dentinal tubules after acid etching; as can be seen from fig. 2: high-density substance deposition exists in the dentinal tubules, and the occlusion rate of the dentinal tubules in the visual field reaches 99 percent; as can be seen from fig. 3: the section shows that calcium salt substance deposits in the dentinal tubules and can reach the deep layer, and the dentinal tubules are fully sealed; as can be seen from fig. 4: the artificial saliva is soaked for 7 days, and dentin tubules are basically sealed.
Example 2: closed root tip hole (tube visible to the naked eye)
The method comprises the following steps: 3 human premolars (which are complete in dental crowns, free of caries and cracks and are freshly extracted in oral and maxillofacial surgery of oral medical college of capital medical university) due to orthodontics are selected (patients agree with the consent, the residues of root surface soft tissues are removed by a curette after extraction, and physiological saline at 4 ℃ is stored for standby, and the time is not more than 4 weeks), and the dental crowns are used as test pieces for standby.
Equipment: scanning electron microscopy (Phenom proX, Phenom-World B.V., the Netherlands), metallographic specimen pre-mill (YM-2A, Shanghai metallographical mechanical equipment Co., Ltd.), low speed cutter (Isomet 4000line Precision Saw, Buehler, USA);
materials: self-setting methyl methacrylate-based resin (dental materials factory, Shanghai medical instruments GmbH; self-setting resin for short), acid etching agent (Gruma, Germany);
preparing a reagent A: dissolving calcium phytate in deionized water, adjusting the pH value to 3.5-4 by hydrochloric acid, and preparing a reagent B: dissolving sodium hydroxide in deionized water to prepare sodium hydroxide solution, and adjusting the pH value to 8-10.
Before use, the root canal is dredged by a nickel-titanium instrument Protaper, the dental pulp and other substances in the root canal are removed, and the root canal is washed by deionized water for 15 seconds and then dried. Placing 10 μ L of the reagent A in the root canal, placing 10 μ L of the reagent B in the root canal after 1min, and naturally drying for 10 min. Self-solidifying and embedding the tooth root, longitudinally cutting the tooth root perpendicular to the long axis of the tooth under a low-speed cutting machine, and observing the section by an electron microscope.
As a result, the calcium phytate precipitate blocked the apical pores, as can be seen in FIG. 5.
EXAMPLE 3 dentinal tubule occlusion by adding ethanol to reagent A
Preparing a reagent A: dissolving calcium phytate in deionized water, adjusting pH value to 3.5-4 with hydrochloric acid, and simultaneously adding 95% ethanol with volume percentage content of 0.5%; preparing a reagent B: dissolving sodium hydroxide in deionized water to prepare sodium hydroxide solution, adjusting pH value to 8-10, and simultaneously adding 95% ethanol with volume percentage content of 0.5%.
Before use, the dentin sample is subjected to 37% phosphoric acid etching for 30s, washed for 10 s and then naturally dried, dentin tubules are fully exposed, and the observation is carried out by an electron microscope. Coating the reagent A on the surface of a dentin sample, naturally drying for 1min, then coating the reagent B, naturally drying for 10 min, cleaning the tooth surface with deionized water, removing redundant substances and the like, and observing by using an electron microscope. Soaking artificial saliva for 7 days, and observing by an electron microscope.
The results were substantially the same as in example 1.

Claims (6)

1. A material for the in situ formation of mineral deposits within the lumen of a dentin lumen comprising a separate agent a and a separate agent B; the reagent A is 1-70% calcium phytate acidic aqueous solution by mass, the reagent B is alkaline solution which is alkaline aqueous solution of calcium hydroxide, potassium hydroxide or sodium hydroxide, and the pH value of the alkaline aqueous solution is 8-10; the pH value of the reagent A is 3.5-4.
2. A material for the in situ formation of mineral deposits in the lumen of dentinal tubes according to claim 1, wherein the acidity of the acidic aqueous solution of calcium phytate is such that the calcium phytate dissolves in water and is not harmful to the human body or as less acidic as possible.
3. The material for in situ formation of mineral deposits in dentinal lumens as claimed in claim 1, wherein one or more of hydrophilic components ethanol, ethylene glycol and acetone are added to agent a or agent B to increase permeability;
the content of the hydrophilic component in percentage by volume is not more than 0.05 percent.
4. A material for the in situ formation of mineral deposits in the lumen of dentin tubes according to claim 1, wherein a silicon-containing compound is added to agent B in a silicon-containing mass fraction of 0.5 x 10-6Na of (2)2SiO3To induce calcium salt deposition in the oral cavity and tissues.
5. A method of preparing a material for the in situ formation of a mineral deposit within a dentinal lumen as claimed in any one of claims 1 to 4 comprising the steps of:
(1) the preparation of the reagent A comprises the following steps: placing calcium phytate in deionized water, and adjusting the pH value with hydrochloric acid; or dissolving calcium chloride or calcium carbonate in phytic acid to fully dissolve; (2) the preparation of the reagent B comprises the following steps: dissolving one or more of alkaline substances of calcium hydroxide, potassium hydroxide and sodium hydroxide in deionized water to prepare alkaline solution.
6. The method according to claim 5, wherein the agent A is applied directly to the exposed dentinal surface or the exposed dentinal surface of the root canal, or the exposed dentinal surface.
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CN112494340B (en) * 2020-11-02 2021-12-10 浙江大学 A kind of dental bonding pretreatment material and use
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CN101869534A (en) * 2009-04-22 2010-10-27 日进齿科材料(昆山)有限公司 Lubricant for root canal therapy
CN106974834A (en) * 2017-04-01 2017-07-25 首都医科大学附属北京口腔医院 A kind of utilization deferred reaction forms material and its application of mineral matter in dentinal tubule

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