An oral intracanal medicament, a preparation method thereof and application thereof

By preparing an intracanal medication containing polyelectrolytes, nano-cerium oxide particles, and other components, the problems of poor inhibition of Enterococcus faecalis and diffusion of nano-cerium oxide in existing root canal medications have been solved. This has achieved remineralization and long-lasting antibacterial effect on the root canal system, thus improving the long-term success rate of root canal treatment.

CN117100620BActive Publication Date: 2026-04-17ZHEJIANG UNIV
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
ZHEJIANG UNIV
Filing Date
2023-06-27
Publication Date
2026-04-17

AI Technical Summary

Technical Problem

Existing root canal medications have limited inhibitory effects on refractory periapical periodontitis caused by Enterococcus faecalis and other bacteria, and may reduce the mechanical strength of the tooth root and affect the apical sealing. Nano-cerium oxide diffuses rapidly within the root canal, leading to a decrease in its effective concentration.

Method used

The oral root canal medication is made by using a polyelectrolyte, nano-cerium oxide particles, hydrogen peroxide, doped metal ion agent and thickener. By adjusting the solution pH and controlling the component concentration, the nano-cerium oxide is mineralized in an orderly manner within the collagen fibers, forming a cerium oxide remineralized layer, which enhances antibacterial properties and biocompatibility.

Benefits of technology

It effectively inhibits various bacteria, including Escherichia coli and Enterococcus faecalis, improves the remineralization effect of the root canal system surface, seals accessory root canals and dentinal tubules, achieves long-lasting antibacterial effect, and enhances the long-term efficacy of root canal treatment.

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Abstract

The application discloses an oral root canal medicine, a preparation method thereof and application thereof. The oral root canal medicine comprises the following raw materials: a polyelectrolyte, cerium nitrate, nano cerium oxide particles, an oxidizing agent, a metal ion doped agent and a thickening agent, and the pH is adjusted to 7-10. The root canal medicine of the application should be used after tooth root canal preparation and before root canal filling, and is temporarily sealed for one to two weeks after being placed in the root canal. The oral root canal medicine of the application is used for realizing the biomimetic remineralization of the inner wall of the root canal, so that the long-term antibacterial effect in the root canal is achieved. The root canal medicine of the application can realize the complete sealing of the microcavity of the root canal system and the persistent release of the antibacterial component by using the biomimetic mineralization method, and solves the problem that residual microorganisms cannot be completely removed in modern root canal treatment.
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Description

Technical Field

[0001] This invention relates to an intracanal medication in the field of oral treatment technology, specifically to an intracanal medication, its preparation method, and its application. Background Technology

[0002] Root canal treatment, also known as endodontic treatment, is the preferred method for treating common oral diseases such as pulpitis and periapical periodontitis. Its core principle is to thoroughly remove the source of infection through mechanical preparation, root canal irrigation, root canal medication, and meticulous root canal filling. However, due to the extreme complexity of the human root canal system, achieving this goal with current technology still faces significant challenges.

[0003] Currently, the only strategy for dealing with residual microorganisms is passive filling with artificial materials. To improve infection control, many researchers have attempted to add antibacterial components (such as ampicillin, metronidazole, and nano-silver ions) to root canal sealants. However, with the rapid release of these antibacterial components, the long-term effectiveness of these root canal filling materials is significantly reduced, and their biocompatibility may be affected. Furthermore, in many cases, the filling material cannot adequately seal the apical foramen, allowing glycoprotein-rich tissue fluid to seep into the root canal, providing nutrients for residual microorganisms, enabling them to proliferate and reach sufficient numbers, thereby causing or maintaining periapical lesions. The persistent presence of infectious microorganisms is a major cause of root canal treatment failure.

[0004] To compensate for the shortcomings of mechanical and chemical preparation, intracanal medications are often used in clinical practice to further reduce the number of bacteria. Among them, calcium hydroxide is the most commonly used intracanal medication in clinical practice. It has broad-spectrum antibacterial activity, but its inhibitory effect on Enterococcus faecalis is limited, and it has problems such as reducing the mechanical strength of the tooth root and affecting the apical sealing. Therefore, it is not an ideal root canal disinfectant.

[0005] Nano-cerium oxide is a newly emerging material with antibacterial and anti-inflammatory functions in recent years. It not only has good biocompatibility but also possesses multiple functions such as anti-oxidation, inhibition of cell apoptosis, and promotion of angiogenesis. However, in practical applications, nano-cerium oxide can rapidly diffuse from the adsorption or encapsulation area, leading to a rapid decrease in the effective concentration at the site of action and affecting its function. Summary of the Invention

[0006] To address the problems existing in the background art, the present invention provides an intracanal medication for oral cavity, its preparation method and its application, which can effectively form a cerium oxide remineralization layer and play an antibacterial role.

[0007] At least one objective of this invention is to provide a root canal sealing agent that can remineralize the demineralized dentin on the surface of the root canal system, thereby achieving the purpose of sealing lateral canals and dentinal tubules and providing long-lasting antibacterial effects.

[0008] At least one objective of this invention is to provide a method for preparing and applying such intracanal medication.

[0009] The purpose of this invention is to overcome the limitations of current root canal medications in inhibiting microorganisms closely related to refractory periapical periodontitis, such as Enterococcus faecalis, and to address issues such as reduced root mechanical strength and impaired apical sealing. This invention provides an oral root canal medication and its preparation method.

[0010] To achieve the above objectives, the present invention provides the following technical solution:

[0011] I. A type of oral root canal medication

[0012] The oral root canal medication contains the following ingredients: polyelectrolyte, cerium nitrate (Ce(NO3)4), nano-cerium oxide particles (CeO2 NPs), hydrogen peroxide (H2O2), doped metal ion agent, deionized water, and thickener, wherein deionized water is used as a solvent.

[0013] The polyelectrolyte includes one of dextran, polyaspartic acid, and O-carboxymethyl chitosan.

[0014] The particle size of the cerium oxide nanoparticles is 1-100 nm.

[0015] The doped metal ion agent is a mixture of Sm(NO3)3, La(NO3)3, Er(NO3)3 and Cu(NO3)2.

[0016] The thickener mentioned therein is a cellulose derivative.

[0017] The oral root canal sealing medication contains a polyelectrolyte concentration of 0.1-5000 mg / mL, a cerium nitrate concentration of 1 mM-6 M, a hydrogen peroxide concentration of 0-100 mg / mL, a cerium oxide nanoparticle concentration of 0.01-100 mg / mL, a doped metal ion concentration of 0.01-100 mg / mL, and a thickener mass fraction of 0.1-5%. The use of dextran, O-carboxymethyl chitosan, and polyaspartic acid stabilizes the amorphous state of the cerium oxide nanoparticles, inhibits cerium oxide precipitation, and maintains a clear solution for an extended period, thereby achieving ordered mineralization of the cerium oxide nanoparticles within collagen fibers. Controlling the H2O2 concentration to 0-100 mg / mL aims to increase the Ce content in the cerium oxide nanoparticles through the oxidizing effect of H2O2. 4+ The proportion of [a specific ingredient] is adjusted to increase the antibacterial properties of the material. Doping with metal ions is used to modulate the surface chemical properties of cerium oxide nanoparticles, improving antibacterial properties and biocompatibility. Thickeners are used to reduce the flowability of intracanal medications and increase the degree of remineralization of the intracanal wall.

[0018] II. A method for preparing oral root canal sealing medication

[0019] Based on the concentration ratio of the oral root canal sealing agent, polyelectrolyte, cerium nitrate (Ce(NO3)4), nano-cerium oxide particles (CeO2 NPs), hydrogen peroxide (H2O2), doped metal ion agents (Sm(NO3)3, La(NO3)3, Er(NO3)3, Cu(NO3)2) and thickener are dissolved in deionized water. Then, the pH of the solution is adjusted to 7-10 using NaOH to obtain the oral root canal sealing agent.

[0020] III. Application of a type of intracanal medication in oral cavity

[0021] The aforementioned oral root canal medication is used for the application of oral products for root canal medication disinfection or dressing changes.

[0022] IV. A method for applying intracanal medication in oral cavity

[0023] During root canal preparation for dental root canal treatment, the root canal is treated with ethylenediaminetetraacetic acid solution (specifically, commercially available 17% EDTA), then rinsed with water, dried with absorbent paper points, and then intracanal medication is injected into the root canal and temporarily sealed for 1 to 2 weeks, thereby achieving root canal medication sealing.

[0024] Compared with the prior art, the present invention has the following advantages:

[0025] The method for preparing intracanal oral medication of the present invention is simple, and the prepared intracanal oral medication has a better inhibitory effect on a variety of bacteria such as Escherichia coli and Enterococcus faecalis. It has good biocompatibility and can remineralize the demineralized dentin on the surface of the root canal system to achieve the purpose of sealing lateral canals and dentinal tubules and providing long-lasting antibacterial effect. Attached Figure Description

[0026] Figure 1 These are TEM images of two-dimensional collagen processed at 7 days and demineralized dentin at 14 days, as per the present invention. Figure 1 (a) is a TEM image of two-dimensional collagen processed by the present invention after 7 days. Figure 1 (b) is a TEM image of demineralized dentin treated with the present invention for 14 days.

[0027] Figure 2 This invention processes micro-CT images of tooth root canals prepared with a mechanical root canal file and demineralized with EDTA, wherein... Figure 2 (a) is a micro-CT image of the apical lateral branch canal closure of a tooth after processing according to the present invention. Figure 2 (b) is a micro-CT image of the inner wall of the tooth root canal after being processed by the present invention.

[0028] Figure 3This is a comparison image of live and dead staining of dentin cultured with Enterococcus faecalis 14 days after demineralized dentin treatment according to the present invention. Figure 3 Image (a) is a live / dead staining image of dentin cultured with Enterococcus faecalis 14 days after treatment with intracanal medication of the present invention. Figure 3 (b) is a live / dead staining image of dentin cultured with Enterococcus faecalis 14 days after oral root canal treatment with intracanal medication without the present invention. Detailed Implementation

[0029] The present invention will now be clearly and completely described in conjunction with the accompanying drawings and specific embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0030] Example 1

[0031] A polyelectrolyte and Ce(NO3)4 were dissolved in 100 ml of deionized water, with the polyelectrolyte concentration being 1 mg / mL and the Ce(NO3)4 concentration being 10 mM. 20 mg / ml H2O2 and 20 mg / ml doping metal ion agent were added, along with 3% sodium carboxymethyl cellulose. The pH of the solution was adjusted to 7 using NaOH, and the mixture was thoroughly stirred to obtain the intracanal medication. The polyelectrolyte was dextran.

[0032] Example 2

[0033] Polyelectrolyte and Ce(NO3)4 were dissolved in 100 ml of deionized water, with the polyelectrolyte concentration being 1 g / mL and the Ce(NO3)4 concentration being 2 M. 30 mg / ml H2O2 and 30 mg / ml doping metal ion agent were added, along with 5% sodium carboxymethyl cellulose. The pH of the solution was adjusted to 8 using NaOH, and the mixture was thoroughly stirred to obtain the intracanal medication. The polyelectrolyte is O-carboxymethyl chitosan.

[0034] Example 3

[0035] Polyelectrolyte and Ce(NO3)4 were dissolved in 100 ml of deionized water, with the polyelectrolyte concentration being 500 mg / mL and the Ce(NO3)4 concentration being 1 M. 50 mg / mL H2O2 and 50 mg / mL doping metal ion agent were added, along with 0.5% sodium carboxymethyl cellulose. The pH of the solution was adjusted to 10 using NaOH, and the mixture was thoroughly stirred to obtain the oral root canal medication. The polyelectrolyte was polyaspartic acid.

[0036] The intracanal medications used in Examples 1-3 of this paper are applied to patient treatment, and the specific usage methods are as follows:

[0037] 1) For teeth with pulpitis or periapical periodontitis, open the pulp chamber, uncover the pulp apex, remove the pulp, and prepare the root canal for root canal medication.

[0038] 2) Use a syringe to inject the root canal sealing agent of the present invention into the root canal, temporarily seal with zinc oxide, and seal for 1-2 weeks.

[0039] 3) Remove zinc oxide, i.e., release the temporary sealant. Use a syringe needle to thoroughly flush and clean the root canal. After completely removing the medication from the root canal, perform root canal filling.

[0040] During root canal treatment, the intracanal medication of this invention can mineralize the collagen fibers of the dentin lining the root canal wall, which have been treated with EDTA clinically, both internally and externally. Figure 1 (a) and Figure 1 As shown in (b), and fully deposited on the inner wall and sides of the root canal, as shown in (b). Figure 2 (a) and Figure 2 As shown in (b). The intracanal medication of the present invention also has an antibacterial effect, such as... Figure 3 (a) and Figure 3 As shown in (b). Therefore, the intracanal medication proposed in this invention can provide a basis for the long-term efficacy of root canal treatment.

[0041] The above embodiments illustrate the basic principles and preparation method of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention and are not intended to limit the scope of the invention in any way. Various changes and modifications can be made to the present invention without departing from its scope. Therefore, all technical solutions obtained by equivalent substitution are within the protection scope of the present invention.

Claims

1. A type of intracanal medication for oral cavity, characterized in that, The product contains the following ingredients: polyelectrolyte, cerium nitrate, hydrogen peroxide, dopant metal ions, deionized water, and thickener. The polyelectrolyte content ranges from 0.1 to 5000 mg / mL, the cerium nitrate concentration is 1 mM to 3.5 M, the hydrogen peroxide concentration is 0 to 100 mg / mL, the dopant metal ion concentration is 0.01 to 100 mg / mL, and the thickener mass fraction is 0.1% to 5%. The polyelectrolyte is used to stabilize the amorphous state of nano-cerium oxide, inhibit the formation of cerium oxide precipitates, and maintain the solution in a clear state for a long time, thereby achieving ordered mineralization of nano-cerium oxide within collagen fibers. Hydrogen peroxide is used to increase the Ce content in the nano-cerium oxide crystals. 4+ The ratio; doping with metal ions is used to adjust the surface chemical properties of cerium oxide nanoparticles, thereby improving their antibacterial properties and biocompatibility.

2. The endodontic medicament according to claim 1, wherein The polyelectrolyte mentioned therein includes one of dextran, polyaspartic acid, and O-carboxymethyl chitosan.

3. The endodontic medicament of claim 1, wherein the at least one active ingredient is selected from the group consisting of: chlorhexidine, cetylpyridinium chloride, and combinations thereof. The doped metal ion agent is a mixture of Sm(NO3)3, La(NO3)3, Er(NO3)3 and Cu(NO3)2.

4. The endodontic medicament of claim 1, wherein the medicament is a powder. The thickener mentioned therein is a cellulose derivative.

5. A method for preparing an intracanal medication according to any one of claims 1-4, characterized in that, The polyelectrolyte, cerium nitrate, nano-cerium oxide particles, hydrogen peroxide, doped metal ion agent, and thickener are all dissolved in deionized water. Then, the pH of the solution is adjusted to 7-10 using NaOH to obtain intracanal medication.

6. Use of a medicament for the preparation of an oral product according to any of claims 1-4, characterized in that, The aforementioned oral root canal medication is used in the preparation of oral products for root canal medication disinfection or dressing changes.

Citation Information

Patent Citations

  • Preparation method of temperature-sensitive injectable moldable mineralized material

    CN116211714A

  • Metal-modified nanoparticle enabled dental resins for prevention of dental caries

    US20230138286A1