CN113827485A - Root canal filling material containing bioactive glass and preparation method thereof - Google Patents
Root canal filling material containing bioactive glass and preparation method thereof Download PDFInfo
- Publication number
- CN113827485A CN113827485A CN202111144472.0A CN202111144472A CN113827485A CN 113827485 A CN113827485 A CN 113827485A CN 202111144472 A CN202111144472 A CN 202111144472A CN 113827485 A CN113827485 A CN 113827485A
- Authority
- CN
- China
- Prior art keywords
- bioactive glass
- root canal
- bioactive
- powder
- filling material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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- 230000000975 bioactive effect Effects 0.000 claims abstract description 32
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Images
Classifications
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- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
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- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
- A61K6/818—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising zirconium oxide
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- 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
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Landscapes
- Health & Medical Sciences (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Plastic & Reconstructive Surgery (AREA)
- Ceramic Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Dental Preparations (AREA)
Abstract
The invention discloses a root canal filling material containing bioactive glass, which comprises raw material components of powder and solvent, wherein the mass ratio of the powder to the solvent is 1.0-3.0; the powder is prepared from the following raw materials: bioactive glass, X-ray radiation-blockingAn agent, a thickener and/or a bioactive component, wherein the X-ray blocking agent is selected from ZrO2、Bi2O3、CHI3One or more of; the raw material component of the bioactive glass comprises SiO2And P2O5And at least one member selected from Na2O、CaO、SrO、MgO、K2O、CaF2、SrF2、LaF3、SrCl2、NaF、CaCl2、KCl、CuO、ZnO、B2O3、H3BO3CoO and hydrates thereof.
Description
Technical Field
The invention belongs to the technical field of oral cavity materials, and particularly relates to a root canal filling material containing bioactive glass and a preparation method thereof.
Background
A root canal filling material is used for filling and sealing a pulp cavity and a root canal gap in a root canal treatment process. An ideal root canal filling material should have the following properties: (1) the root canal is easy to fill; (2) after solidification, the material does not shrink and is impermeable to water, and the sealing property is good; (3) has antibacterial activity; (4) can be stored in the root canal for a long time without being absorbed; (5) has X-ray radiation blocking; (6) does not discolor teeth; (7) if necessary, can be removed from the root canal. The root canal filling material used clinically includes solid filling material, root canal sealer, pulp capping agent, root canal plasticizing liquid, etc.
Root canal sealers are one of the most important materials in root canal filling, and are very important for the close filling of root canals and for exerting antibacterial action. The current research uses more include: resins, calcium hydroxides, and glass ionomer cement. 1. Resins: AH26 and AHplus are the main representatives of resin root canal sealer, and the main components of the sealer are: diphenol α -diglycidyl ether and Hexamethylenetetramine (HMT). HMT is composed of formaldehyde and ammonia, the mixed HMT can be decomposed into formaldehyde and ammonia in aqueous solution or acid environment, and as representatives of resin root canal sealers, AH26 and AHplus, the antibacterial property and the biocompatibility of the HMT depend on the existence of the formaldehyde, and the two contradict with each other, so that the problem cannot be solved at present. 2. Calcium hydroxides: calcium hydroxide has been conventionally used for the pole tip induced formation of young permanent teeth in which the apical foramen has not been formed, and also has a good therapeutic effect for permanent teeth in which the apical foramen has been formed due to its excellent antibacterial property and biocompatibility, Ca (OH)2The antibacterial action of (A) is currently believed to be mainly due to OH-The result is obtained; high concentration of OH-Can destroy phospholipid on bacterial cell membrane by enzyme interfering peroxidation and saponification of fat, and inhibit bacterial growth and bacterial finenessCell division; thus, the calcium hydroxide exerts the antibacterial action at a high speed and maintains OH-The concentration of (b) is directly related, but the enzyme inactivation may be either irreversible or reversible. Ca (OH)2: all of them should have insolubility as a root canal sealer and can seal the root canal for a long period of time, but this contradicts with antibacterial property, and it is considered that when antibacterial is performed, the sealer is partially dissolved by releasing antibacterial ions, and the sealing property is lowered, and there is no solution to this problem at present, and further improvement is required for further improving the sealing property of the material. 3. Glass ion cement: the glass ions have good physical and chemical properties, biocompatibility and good adhesion. It is adhered to the surface of dentin by the chain action of the superfine structure, wherein the polyacrylate ion can generate replacement reaction with the phosphate ion in the hydroxyapatite, the reaction is irreversible, the adhesion property of the glass ion is further increased, and the adhesion property of the glass ion can be influenced by the root canal flushing agent. 4. Zinc oxide clove oil sealant: zinc oxide clove oil occlusion is a traditional root canal sealer that is often used as a control in new material testing. Mainly comprises zinc oxide, rosin and eugenol. The zinc oxide has an astringent effect, the rosin is added to increase the adhesive property of the material, and the eugenol can enable mycoprotein to agglutinate and precipitate by penetrating cell walls; inactivating bacterial endoenzymes; reducing surface tension, increasing cell permeability and the like, and playing antibacterial role; the study found that zinc oxide clove oil in the bacterial culture dish has antibacterial effect on white coccoid, staphylococcus aureus and streptococcus mutans, but within 3 days of the beginning of the experiment, the effect is not obvious, and the release of eugenol is considered to be possible to take a longer time.
By the introduction, zinc oxide clove oil, resin, calcium hydroxide, silicone and nano biological materials in the currently common root canal sealer types have the limitations of the materials:
zinc oxide clove oil sealant such as Pulp Canal Sealer has certain fluidity and consistency, is one of the first sealants applied to clinic, but has low strength, weak bonding force with root Canal wall, high dissolution rate, and inflammatory property due to free clove oil and zinc oxide.
Calcium hydroxide type sealing agents such as Sealapex are mainly characterized by forming a high-alkaline environment and exerting antibacterial performance, but have correspondingly high cytotoxicity and high dissolution rate, and can influence the root tip sealing effect.
Silicone-based root canal sealers such as Roeko Seal, Gutta Flow, have good biocompatibility, but have weak chemical bonding with the dentinal wall and large bonding force affected by residual substances on the root canal wall.
The resin-based root canal sealer mainly includes two types, i.e., polymethacrylic resin such as Epiphony SE and EndoRez and epoxy resin such as AH Plus, which have a low dissolution rate and a high adhesion to the root canal wall, but have a long curing time, and exhibit antibacterial properties mainly by releasing formaldehyde and the like before curing, and do not have antibacterial properties after curing.
The nano biomaterial root canal Sealer is a newer Sealer type, such as Endosequence BC Sealer and iRoot SP, which are bonded with dentin by forming a hydroxyapatite layer, has good root tip sealing performance, and is superior to other sealers in biocompatibility and antibacterial property, but can be completely cured in a humid environment and cannot be easily removed during root canal retreatment.
Therefore, the market needs a root canal filling material which can meet the clinical requirements and has good biological safety and antibacterial property.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the limitations of root canal filling materials such as zinc oxide clove oil, resin, calcium hydroxide, silicone, nano biological materials and the like commonly used in the prior art, and provides a root canal filling material containing bioactive glass and a preparation method thereof, which can be used for oral root canal treatment and have good sealing effect, biological safety and excellent antibacterial property.
The purpose of the invention is realized by the following technical scheme:
a root canal filling material containing bioactive glass comprises raw material components of powder and solvent, wherein the mass ratio of the powder to the solvent is 1.0-3.0; the powder is prepared from the following raw materials: bioactive glass, an X-ray radiation-blocking agent and a thickening agent.
Further, the X-ray blocking agent is selected from ZrO2、Bi2O3、CHI3One or more of; the raw material component of the bioactive glass comprises SiO2And P2O5And at least one member selected from Na2O、CaO、SrO、MgO、K2O、CaF2、SrF2、LaF3、SrCl2、NaF、CaCl2、KCl、CuO、ZnO、B2O3、H3BO3At least one of, CoO and hydrates thereof; and when the bioactive glass raw material components simultaneously comprise SiO2And P2O5The content of the components ensures that the connectivity NC of the bioactive glass meets the following conditions: NC is more than or equal to 1.5 and less than or equal to 3.2, wherein the calculation formula of NC is as follows:
in the formula:
is SiO in medical bioactive glass2The molar percentage of (A); mMOIs the mol percentage content of the alkaline earth metal oxide in the medical bioactive glass;
is the mol percentage content of alkali metal oxide in the medical bioactive glass;
is P in medical bioactive glass2O5The molar percentage of (A); the bioactive glass is prepared by a high-temperature melting and cold quenching method.
Further, when the stationThe raw material components of the bioactive glass simultaneously comprise SiO2And P2O5The content of the components ensures that the connectivity NC of the bioactive glass meets the following conditions: NC is more than or equal to 1.5 and less than or equal to 3.0, and P2O5The content of the bioactive glass is more than 3.5mol percent; and when at least one of metal fluoride, CuO, ZnO and CoO is contained, the content of the metal fluoride, or the CuO, or the ZnO or the CoO in the bioactive glass component is less than 5.0mol percent.
Further, the powder comprises the following components in percentage by mass: 30-70 wt% of bioactive glass, 15-65 wt% of X-ray radiation inhibitor and 1-15 wt% of thickener; and when the X-ray blocking agent consists of ZrO2And Bi2O3When composed, ZrO2The content of Bi accounts for 5.0 to 60 weight percent of the total weight of the powder2O3Is 0.5 to 9.5 weight percent of the total weight of the powder; when the X-ray-blocking agent contains ZrO together2、Bi2O3、CHI3The three are mixed according to any proportion.
Further, the powder also comprises a bioactive component, wherein the bioactive component is selected from one or more of amorphous calcium phosphate, casein phosphopeptide calcium phosphate complex, octacalcium phosphate, beta-calcium phosphate and apatite-like substances, and when mixed, the bioactive component is in any proportion; wherein the apatite-like substance is one or more of hydroxyapatite, fluorapatite, chlorapatite and composite apatite.
Further, the powder comprises the following components in percentage by mass:
10-70 wt% of bioactive glass, 0.1-35 wt% of bioactive component, 10-65 wt% of X-ray radiation inhibitor and 1-10 wt% of thickening agent;
and when the X-ray blocking agent consists of ZrO2And Bi2O3When composed, ZrO2The content of Bi accounts for 5.0 to 60 weight percent of the total weight of the powder2O3Is 0.5 to 9.5 weight percent of the total weight of the powder; when the X-ray-blocking agent contains ZrO together2、Bi2O3、CHI3The three are mixed according to any proportion.
Further, the thickening agent is selected from one or more of sodium alginate or sodium polyacrylate, cellulose, N-vinyl amide polymer, carbomer, lauryl alcohol and the like, and is in any proportion when mixed; the solvent is selected from one or more of deionized water, glycerol and ethanol, and is in any proportion when mixed.
Further, the root canal filling material is a root canal sealer, a root canal filler, or a pulp capping agent used for oral root canal treatment.
The invention also provides a preparation method of the root canal filling material containing the bioactive glass, which comprises the following steps:
1) weighing bioactive glass, an X-ray radiation resisting agent and a thickening agent according to the formula and the mass ratio of each component in the formula, and grinding the bioactive glass, the X-ray radiation resisting agent and the thickening agent by using a grinding instrument until the bioactive glass, the X-ray radiation resisting agent and the thickening agent are uniformly mixed;
2) and (3) uniformly mixing the uniform powder obtained in the previous step with a solvent according to a mass ratio, and forming uniform paste at normal temperature to obtain the root canal filling material containing the bioactive glass.
Further, the step 1) also comprises the steps of weighing the bioactive components, mixing the bioactive components with the bioactive glass, the X-ray radiation inhibitor and the thickening agent, and grinding; the particle size of the bioactive glass particles in the step 1) is less than 100 mu m; grinding to be uniformly mixed in the step 1), wherein the grinding is carried out for 5min-10min to be uniform; and 2) uniformly mixing in the step 2), namely uniformly stirring on a glass plate for 2-5 min by using a stirring knife.
Compared with the prior art, the invention has the following advantages:
1. the root canal filling material containing the bioactive glass is prepared by taking the bioactive glass with controllable degradability as a main component of a novel root canal filling material, taking the bioactive glass as an additive of a root canal sealing agent and containing SiO2、P2O5、Na2O、CaO、SrO、MgO、K2O、CaF2、SrF2、NaF、LaF3、CaCl2、SrCl2、CuO、ZnO、B2O3、H3BO3And CoO, etc., can controllably and slowly release Si, Sr, Zn, Na, Mg, Ca, P, F and Cu and Cl, which raise the pH of the surrounding environment, exhibit the potential to form apatites (e.g., hydroxyapatite, fluorapatite, etc.).
2. The root canal filling material containing the bioactive glass is the bioactive glass with amorphous shape or the bioactive glass ceramic with partial crystalline phase, and the obtained sealing agent has reasonable curing time, flowability and radiation resistance.
3. The root canal filling material containing the bioactive glass has good biological safety and excellent antibacterial property.
4. The root canal filling material containing the bioactive glass has good root tip sealing performance.
Drawings
These and/or other aspects and advantages of the present invention will become more apparent and more readily appreciated from the following detailed description of the embodiments of the invention, taken in conjunction with the accompanying drawings of which:
FIG. 1 is an XRD diffraction pattern of a bioactive glass and a bioactive glass-ceramic according to the present invention.
Fig. 2 is a graph showing the radioopacity of the root canal sealer containing bioactive glass according to the present invention.
FIG. 3 is a Fourier infrared spectrum of the root canal sealer containing bioactive glass of the present invention after being soaked in SBF solution for 0d, 3d, 7d and 14 d.
FIG. 4 is a graph showing the release of different ions at 1h, 4h, 1d, 3d, 7d, and 14d after the root canal sealer containing bioactive glass according to the present invention is soaked in Tris solution.
Fig. 5 is a graph showing the penetration ability of a dye into a transparent tooth filled with the root canal sealer containing bioactive glass according to the present invention and the root canal sealers obtained in comparative examples 1 to 2.
FIG. 6 is a graph showing the relative proliferation rate of cells after coculture of a root canal sealer containing bioactive glass according to the present invention with fibroblasts for various periods of time.
FIG. 7 is a graph showing the agar plate count-the inhibitory effect of the root canal sealer containing bioactive glass of the present invention on enterococcus faecalis.
Detailed Description
The present invention is described in further detail below by way of examples, which should not be construed as limiting the invention thereto.
Example 1:
a root canal sealer containing bioactive glass is prepared from powder and a solvent, wherein the powder-liquid ratio is 1.0, and the powder is prepared from the following components in parts by mass:
70 percent of bioactive glass,
0 percent of other bioactive components,
20 percent of X-ray radiation-resistant agent,
10% of a thickening agent;
the bioactive glass is amorphous bioactive glass and is made of SiO2、P2O5、CaO、K 20、MgO、CaCl2SrO, prepared according to 2.3 NC of glass component, and P2O5The content of the bioactive glass is 5mol percent; CaCl2The content of the bioactive glass is 10 mol%;
the X-ray radiation-blocking agent is selected from ZrO2；
The thickening agent is selected from sodium alginate;
the solvent is selected from deionized water and glycerol according to the volume ratio of 1: 2.
The preparation method of the root canal sealer containing the bioactive glass comprises the following steps:
1) weighing bioactive glass with particle size less than 38 μm, bioactive components, X-ray radiation inhibitor and thickener according to mass ratio, and grinding for 5min to uniformity;
2) and (3) uniformly mixing the uniform powder and the solvent obtained in the previous step on a glass plate for 2min by using a mixing knife according to the mass ratio, and forming uniform paste at normal temperature to obtain the product.
Example 2:
a root canal sealer containing bioactive glass is prepared from powder and a solvent, wherein the powder-liquid ratio is 2.0, and the powder is prepared from the following components in parts by mass:
48 percent of bioactive glass,
0 percent of other bioactive components,
50% of X-ray radiation-resistant agent,
2% of a thickening agent;
the bioactive glass is amorphous bioactive glass and is made of SiO2、P2O5、Na2O、CaO、CuO、CaF2Prepared according to the glass component NC being 2.1, and P2O5The content of the bioactive glass is 3.5mol percent; the content of CuO in the bioactive glass is 2mol percent; CaF2The content of the bioactive glass is 5mol percent;
the X-ray radiation-blocking agent is selected from ZrO2And Bi2O3In which ZrO245.0 wt%, Bi2O35.0 wt%;
the thickening agent is selected from sodium alginate;
the solvent is selected from deionized water.
The preparation method of the root canal sealer containing the bioactive glass is the same as that of example 1.
The root canal sealer containing bioactive glass obtained in example 2 is hereinafter referred to as NRCS 1.
Example 3:
a root canal sealer containing bioactive glass is prepared from powder and a solvent, wherein the powder-liquid ratio is 2.0, and the powder is prepared from the following components in parts by mass:
37 percent of bioactive glass,
35 percent of other bioactive components,
20 percent of X-ray radiation-resistant agent,
8% of a thickening agent;
the bioactive glass is bioactive glass ceramic with partial crystalline phase and is made of SiO2、P2O5、CaO、SrO、CaF2、CaCl2、B2O3Prepared according to the glass component NC being 3.1, and P2O5The content of the bioactive glass is 4mol percent; CaF2The content of the bioactive glass is 5mol percent; CaCl2The content of the bioactive glass is 20 mol%; b is2O3The content of the bioactive glass is 3mol percent;
the other bioactive components are amorphous calcium phosphate;
the X-ray radiation-resistant agent is selected from Bi2O3；
The thickening agent is selected from sodium polyacrylate;
the solvent is selected from deionized water and ethanol according to the volume ratio of 1: 1.
The preparation method of the root canal sealer containing the bioactive glass is the same as that of example 1.
Example 4:
a root canal filling agent containing bioactive glass is prepared from powder and a solvent, wherein the powder-liquid ratio is 3.0, and the powder is prepared from the following components in percentage by mass:
59 percent of bioactive glass,
25 percent of other bioactive components,
15% of X-ray radiation-resistant agent,
1% of a thickening agent;
the bioactive glass is amorphous bioactive glass and is made of SiO2、P2O5、SrO、MgO、K2O、CaF2、SrF2、NaF、CaCl2CuO, ZnO, prepared according to a glass composition NC of 2.9, and P2O5The content of the bioactive glass is 2mol percent; CaF2、SrF2The total content of NaF in the bioactive glass is 6 mol%, and the molar mass ratio of the NaF to the bioactive glass is 1:1: 1; CaCl2The content of the bioactive glass is 15mol percent; the content of CuO and ZnO in the bioactive glass is respectively 2mol percent;
the other bioactive components are amorphous calcium phosphate, octacalcium phosphate, beta-calcium phosphate and apatite-like substances (hydroxyapatite, fluorapatite, chlorapatite and the like) which are mixed according to equal weight ratio;
the X-ray radiation-blocking agent is selected from ZrO2；
The thickening agent is selected from cellulose and N-vinyl amide polymers which are mixed in equal weight ratio;
the solvent is selected from deionized water, glycerol and ethanol according to the volume ratio of 1:1: 1.
The preparation method of the root canal filling agent containing the bioactive glass comprises the following steps:
1) weighing bioactive glass with particle size less than 45 μm, bioactive components, X-ray radiation inhibitor and thickener according to mass ratio, and grinding for 10min to uniformity;
2) and (3) uniformly mixing the uniform powder and the solvent obtained in the step (a) on a glass plate for 5min by using a mixing knife according to the mass ratio, and forming uniform paste at normal temperature to obtain the root canal filler containing the bioactive glass.
Example 5:
a root canal filling agent containing bioactive glass is prepared from powder and a solvent, wherein the powder-liquid ratio is 1.0, and the powder is prepared from the following components in percentage by mass:
35 percent of bioactive glass,
30 percent of other bioactive components,
25% of X-ray radiation-resistant agent,
10% of a thickening agent;
the bioactive glass is bioactive glass ceramic with partial crystalline phase and is made of SiO2、CaO、SrO、K2O、SrCl2、H3BO3Prepared according to the NC of the glass component being 2.6, and P2O5The content of the bioactive glass is 2.8 mol%; SrCl2The content of the bioactive glass is 8mol percent; h3BO3The content of the bioactive glass is 5mol percent;
the other bioactive components are amorphous calcium phosphate, octacalcium phosphate and beta-calcium phosphate which are mixed according to equal weight ratio;
the X-ray radiation-blocking agent is selected from ZrO2And Bi2O3In which ZrO20.5 wt% of Bi2O324.5 wt%;
the thickening agent is selected from carbomer and lauryl alcohol which are mixed according to equal weight ratio;
the solvent is selected from deionized water and glycerol according to the volume ratio of 1: 3.
The preparation method of the root canal filling agent containing the bioactive glass is the same as that of the example 4.
Example 6:
a pulp capping agent containing bioactive glass is prepared from powder and a solvent, wherein the powder-liquid ratio is 1.5, and the powder is prepared from the following components in percentage by mass:
70 percent of bioactive glass,
0.1 percent of other bioactive components,
15% of X-ray radiation-resistant agent,
14.9% of a thickening agent;
the bioactive glass is bioactive glass ceramic with partial crystalline phase and is formed by P2O5、CaO、SrO、MgO、SrF2、SrCl2CuO, ZnO, prepared according to a glass composition NC of 2.0, and P2O5The content of the bioactive glass is 35mol percent; SrF2And SrCl2The content of the bioactive glass is 4mol percent; the content of both CuO and ZnO in the bioactive glass is 1mol percent;
the other bioactive components are amorphous calcium phosphate and octacalcium phosphate which are mixed according to the weight ratio of 1: 2;
the X-ray radiation-blocking agent is selected from ZrO2And Bi2O3In which ZrO214.0 wt%, Bi2O30.5 wt% of iodoform (CHI)3) 0.5 wt%;
the thickening agent is selected from cellulose and N-vinyl amide polymers which are mixed in equal weight ratio;
the solvent is selected from deionized water, glycerol and ethanol according to the volume ratio of 1:1: 2.
The preparation method of the pulp capping agent containing the bioactive glass is the same as that of the pulp capping agent in the example 1.
Example 7:
a root canal sealer containing bioactive glass is prepared from powder and a solvent, wherein the powder-liquid ratio is 2.5, and the powder is prepared from the following components in parts by mass:
38 percent of bioactive glass,
0 percent of other bioactive components,
60 percent of X-ray radiation-resistant agent,
2% of a thickening agent;
the bioactive glass is amorphous bioactive glass and bioactive glass ceramic with partial crystalline phase and is prepared with SiO2、P2O5、CaO、SrO、MgO、K2O, KCl, CoO, prepared with NC of glass component of 1.9, and P2O5The content of the bioactive glass is 4.5 mol%; the content of KCl in the bioactive glass is 10 mol%; the content of CoO in the bioactive glass is 1.5mol percent;
the X-ray radiation-blocking agent is selected from ZrO2And Bi2O3In which ZrO255.0 wt%, Bi2O35.0 wt%;
the thickening agent is selected from N-vinyl amide polymers, carbomer and lauryl alcohol which are mixed according to equal weight ratio;
the solvent is selected from deionized water and glycerol according to the volume ratio of 3: 1.
The preparation method of the root canal sealer containing the bioactive glass is the same as that of example 1.
Example 8:
a root canal sealer containing bioactive glass is prepared from powder and a solvent, wherein the powder-liquid ratio is 1.8, and the powder is prepared from the following components in parts by mass:
70 percent of bioactive glass,
0 percent of other bioactive components,
15% of X-ray radiation-resistant agent,
15% of a thickening agent;
the bioactive glass is bioactive glass ceramic with partial crystalline phase and is made of SiO2、P2O5、CaO、SrO、MgO、K2O、LaF3、CaCl2CuO, prepared according to a glass composition NC of 1.7, and P2O5The content of the bioactive glass is 4.5 mol%; LaF3The content of the bioactive glass is 3mol percent; CaCl2The content of the bioactive glass is 6mol percent; the content of CuO in the bioactive glass is 0.5mol percent;
the X-ray radiation-blocking agent is selected from ZrO2And Bi2O3In which ZrO210.0 wt%, Bi2O35.0 wt%;
the thickening agent is selected from N-vinyl amide polymers and lauryl alcohol polymers which are mixed according to equal weight ratio;
the solvent is selected from deionized water and ethanol according to the volume ratio of 1: 4.
The preparation method of the root canal sealer containing the bioactive glass is the same as that of example 1.
Example 9:
a root canal sealer containing bioactive glass is prepared from powder and a solvent, wherein the powder-liquid ratio is 1.5, and the powder is prepared from the following components in parts by mass:
60 percent of bioactive glass,
0 percent of other bioactive components,
30 percent of X-ray radiation-resistant agent,
10% of a thickening agent;
the bioactive glass is amorphous bioactive glass and is made of SiO2、P2O5、CaO、SrO、MgO、CaCl2Prepared according to the glass component NC being 1.5 and P2O5The content of the bioactive glass is 4.5 mol%; CaCl2The content of the bioactive glass is 9mol percent;
the X-ray radiation-blocking agent is selected from ZrO2、Bi2O3And CHI3In which ZrO210.0 wt%, Bi2O319.5 wt% and 0.5 wt% of iodoform;
the thickening agent is selected from N-vinyl amide polymers and carbomer, and is mixed according to the weight ratio of 1: 3;
the solvent is selected from deionized water and ethanol according to the volume ratio of 1: 2.
The preparation method of the root canal sealer containing the bioactive glass is the same as that of example 1.
Comparative example 1:
currently, the most clinically used root canal sealer:
SP, IBC, manufactured in canada (hereinafter NRCS 2).
Comparative example 2:
root canal sealer currently used clinically: AHPlus, Dentsply, manufactured in the United states (hereinafter referred to as NRCS 3).
Comparative example 3:
compared with example 2, when the content of the bioactive glass is O, the prepared material (hereinafter, referred to as NRCS 4) is prepared.
Comparative example 4:
compared with example 2, the composition of the bioactive glass is different (SiO is not included)2) The same procedure as in example 1 was repeated except that a material (hereinafter referred to as NRCS 5) was prepared.
Comparative example 5:
compared with example 2, the composition of the bioactive glass is different (P is not included)2O5) The same procedure as in example 1 was repeated except that a material (hereinafter referred to as NRCS 6) was prepared.
Comparative example 6:
the composition of the bioactive glass was different from that of example 1 (NC: 3.5), and the material (hereinafter, referred to as NRCS 7) was prepared in the same manner as in example 1.
Comparative example 7:
the composition of the bioactive glass was different from that of example 1 (NC: 1.4), and the material (hereinafter, referred to as NRCS 8) was prepared in the same manner as in example 1.
The experimental results are as follows:
table 1: setting time (unit: min) of root canal sealer containing bioactive glass (hereinafter, referred to as NRCS 1) obtained in example 2
The setting time of the root canal sealer containing bioactive glass obtained in example 2 was about 45.3 minutes.
Table 2: dissolution rate (unit%) of root canal sealer containing bioactive glass obtained in example 2
The dissolution rate of the root canal sealer containing the bioactive glass obtained in example 2 was 2.61, and the root canal sealer satisfied the international standard (not more than 3.0%).
Table 3: setting time (unit: min) of root canal sealer containing bioactive glass obtained in example 2 and root canal sealer obtained in comparative examples 1 to 3
The root canal sealer containing bioactive glass obtained in example 2 had a setting time of about 45.3 minutes, which is significantly shorter than that of the currently most clinically used root canal sealer.
Table 4: dissolution rates (unit%)
The dissolution rate of the root canal sealer containing the bioactive glass obtained in the example 2 is 2.61, has a dissolution rate which is comparable to the dissolution rate of the most common root canal sealer clinically used at present, and meets the international standard of the root canal sealer (not more than 3.0%). The dissolution rate of the root canal sealer NRCS8 obtained in comparative example 7 was 6.95, and the dissolution rate was high and did not meet the international standards for sealers.
Experimental example:
fig. 1 XRD diffraction patterns of bioactive glasses and bioactive glass-ceramics:
(a) XRD diffraction pattern of bioactive glass a;
(b) XRD diffraction pattern of bioactive glass-ceramic B;
the bioactive glass of the invention is amorphous bioactive glass (i.e. the material has only glass phase and no other crystal phase, and its XRD pattern is shown in figure 1 (a)) or bioactive glass ceramic with partial crystal phase (i.e. the material has not only glass phase but also crystal phase, and its XRD pattern is shown in figure 1 (b)).
The XRD diffraction pattern of the bioactive glass A has a typical amorphous structure broad peak at 25-32 degrees (2 theta), and no sharp diffraction peak appears at 15-60 degrees (2 theta), which indicates that the bioactive glass A does not contain crystalline phase. The XRD diffraction pattern of the bioactive glass ceramic B also has a typical wide peak of an amorphous structure at 25-32 degrees (2 theta), and a plurality of sharp diffraction peaks of apatite-like substances at 26.6 degrees, 28.0 degrees, 30.66 degrees, 31.87 degrees, 44.8 degrees, 49.85 degrees (2 theta) and the like can be seen, so that the material B not only contains a glass phase, but also contains an apatite-like crystalline phase, and the material is bioactive glass ceramic.
Fig. 2 radioopacity of root canal sealer NRCS1 containing bioactive glass obtained in example 2 and representative root canal sealer of comparative example:
(a) NRCS1(6.27 ± 0.04mm equivalent aluminum sheet thickness);
(b) NRCS2(6.07 ± 0.05mm equivalent aluminum sheet thickness);
(c) NRCS3(9.87 ± 0.05mm equivalent aluminum plate thickness);
(d) dentin disks (3.68 ± 0.06mm equivalent aluminum plate thickness);
(e) a stepped aluminum plate;
(f) NRCS5(8.23 ± 0.04mm equivalent aluminum plate thickness);
(g) NRCS6(7.45 + -0.06 mm equivalent aluminum plate thickness)
The quality of root canal filling, the efficacy of endodontic treatment, and the prognosis are often judged by means of X-ray examination, and thus the X-ray radiation resistance is one of the important properties for root canal sealers. FIG. 2 shows that the radiation opacity of NRCS1 is 6.27 + -0.04 mm equivalent aluminum plate thickness, which is greater than NRCS2(6.07 + -0.05 mm equivalent aluminum plate thickness), and although less than the X-ray opacity of NRCS3(9.87 + -0.05 mm equivalent aluminum plate thickness), much greater than the dentin (3.68 + -0.06 mm equivalent aluminum plate thickness), which can meet the requirement of clinical imaging examination. The bioactive glass component in the root canal sealer NRCS1 in example 2 was replaced with bioactive glass of other components, and the obtained root canal sealers NRCS5 and NRCS6 had radioopacity of 8.23 + -0.04 mm and equivalent aluminum plate thickness of 7.45 + -0.06 mm. These blocking agents are equally satisfactory for clinical imaging examinations.
Fig. 3 is a fourier infrared spectrum of the root canal sealer containing bioactive glass obtained in example 2 after being soaked in SBF solution for 0d, 3d, 7d and 14 d.
As can be seen from FIG. 3, the spectra before and after soaking did not change significantly, but the nonbridging oxygen Si-O-of the bioactive root canal sealer at 920cm-1 decreased in intensity after soaking and was 1035cm-1The characteristic peak of the apatite is shown. It is demonstrated that the bioactive glass root canal sealer of the present invention can undergo controlled material degradation in buffer (SBF, etc.) and can produce apatite-like but has good stability as a whole.
FIG. 4 release of different ions at 1h, 4h, 1d, 3d, 7d, 14d after soaking the root canal sealer containing bioactive glass obtained in example 2 in Tris solution: (a) calcium concentration; (b) the concentration of phosphorus; (c) the concentration of silicon; (d) the fluorine concentration.
As shown in fig. 4, after the root canal sealer containing bioactive glass obtained in example 2 was soaked in Tris solution, the material released Ca, P, Si, F, and the like, and the concentration of the material increased as a whole with time. The released ions can endow the material with certain antibacterial property. In comparative example 6, NRCS7 was obtained, since the bioactive glass having a composition of NC 3.5, the glass was not degraded and had no bioactivity, and thus no significant Ca, P, Si, F plasma could be detected after soaking it in Tris solution, and NRCS7 had no antibacterial property.
FIG. 5 is a graph showing the penetration ability of dye into a transparent tooth filled with a root canal sealer containing bioactive glass obtained in example 2 and a root canal sealer obtained in comparative examples 1 to 2: (a) NRCS1 sealant; (b) NRCS2 sealant; (c) NRCS3 sealant; (d) no blocking agent is used.
As shown in fig. 5, the penetration depth of the dye was significantly reduced in the transparent tooth using the root canal sealer containing bioactive glass obtained in example 2, as compared with the transparent tooth not using the sealer, and it was found that the bioactive glass root canal sealer according to the present item had excellent apical sealing performance.
FIG. 6 relative proliferation rates of cells after different time points of co-culture of the root canal sealer containing bioactive glass obtained in example 2 and the root canal sealer obtained in comparative examples 1 to 2 with fibroblasts: indicates a statistical difference, wherein indicates P <0.05, and indicates P < 0.01. The histograms for each time point represent, from left to right, NRCS1 blocker, NRCS2 blocker, NRCS3 blocker, negative control group and positive control group in order.
As shown in fig. 6, after the bioactive glass root canal sealer related to the present invention and the fibroblasts were co-cultured for different times, the relative proliferation rate of the cells was not statistically different from that of the root canal sealer and the negative control group commonly used in clinic and was significantly higher than that of the positive control group, so that the bioactive glass root canal sealer of the present invention has no significant cytotoxicity and good biological safety.
FIG. 7 agar plate count-schematic representation of the inhibitory effect on enterococcus faecalis of root canal sealer containing bioactive glass obtained in example 2: (a) the root canal sealer NRCS1 containing bioactive glass obtained in example 2; (b) the results were quantified in negative control groups (NC) and (c).
The incomplete pathogenic bacteria removal is an important reason for the failure of root canal treatment and the recurrence of periapical periodontitis. Enterococcus faecalis is a pathogenic bacterium existing in root canal system and having strong drug resistance. As shown in FIG. 7, the bioactive root canal sealer of the present invention showed significant growth inhibition of enterococcus faecalis after 20min of co-culture with enterococcus faecalis, compared to the agar plate without bioactive glass root canal sealer.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the inventive concept of the present invention, which falls into the protection scope of the present invention.
Claims (10)
1. A root canal filling material containing bioactive glass, which is characterized in that:
the raw material components comprise powder and solvent, and the mass ratio of the powder to the solvent is 1.0-3.0;
the powder is prepared from the following raw materials: bioactive glass, an X-ray radiation-blocking agent and a thickening agent.
2. The root canal filling material containing bioactive glass according to claim 1, wherein:
the X-ray radiation-blocking agent is selected from ZrO2、Bi2O3、CHI3One or more of;
the raw material component of the bioactive glass comprises SiO2And P2O5And at least one member selected from Na2O、CaO、SrO、MgO、K2O、CaF2、SrF2、LaF3、SrCl2、NaF、CaCl2、KCl、CuO、ZnO、B2O3、H3BO3At least one of, CoO and hydrates thereof;
and when the bioactive glass raw material components simultaneously comprise SiO2And P2O5When it is used, the contents of its components are such thatThe connectivity NC of the bioactive glass satisfies the following conditions: NC is more than or equal to 1.5 and less than or equal to 3.2, wherein the calculation formula of NC is as follows:
the bioactive glass is prepared by a high-temperature melting and cold quenching method.
3. The root canal filling material containing bioactive glass according to claim 2, wherein:
when the raw material components of the bioactive glass simultaneously comprise SiO2And P2O5The content of the components ensures that the connectivity NC of the bioactive glass meets the following conditions: NC is more than or equal to 1.5 and less than or equal to 3.0, and P2O5The content of the bioactive glass is more than 3.5mol percent;
and when at least one of metal fluoride, CuO, ZnO and CoO is contained, the content of the metal fluoride, or the CuO, or the ZnO or the CoO in the bioactive glass component is less than 5.0mol percent.
4. The root canal filling material containing bioactive glass according to claim 1, wherein:
the powder comprises the following components in percentage by mass:
30-70 wt% of bioactive glass, 15-65 wt% of X-ray radiation inhibitor and 1-15 wt% of thickener;
and when the X-ray blocking agent consists of ZrO2And Bi2O3When composed, ZrO2The content of Bi accounts for 5.0 to 60 weight percent of the total weight of the powder2O3Is 0.5 to 9.5 weight percent of the total weight of the powder; when the X-ray-blocking agent contains ZrO together2、Bi2O3、CHI3The three are mixed according to any proportion.
5. The root canal filling material containing bioactive glass according to claim 1, wherein:
the powder also comprises a bioactive component, wherein the bioactive component is selected from one or more of amorphous calcium phosphate, casein phosphopeptide calcium phosphate complex, octacalcium phosphate, beta-calcium phosphate and apatite-like substances, and is in any proportion when mixed; wherein the apatite-like substance is one or more of hydroxyapatite, fluorapatite, chlorapatite and composite apatite.
6. The root canal filling material containing bioactive glass according to claim 5, wherein: the powder comprises the following components in percentage by mass:
10-70 wt% of bioactive glass, 0.1-35 wt% of bioactive component, 10-65 wt% of X-ray radiation inhibitor and 1-10 wt% of thickening agent;
and when the X-ray blocking agent consists of ZrO2And Bi2O3When composed, ZrO2The content of Bi accounts for 5.0 to 60 weight percent of the total weight of the powder2O3Is 0.5 to 9.5 weight percent of the total weight of the powder; when the X-ray-blocking agent contains ZrO together2、Bi2O3、CHI3The three are mixed according to any proportion.
7. The root canal filling material of bioactive glass as claimed in claim 1, wherein:
the thickening agent is selected from one or more of sodium alginate or sodium polyacrylate, cellulose, N-vinyl amide polymers, carbomer, lauryl alcohol and the like, and is in any proportion when mixed;
the solvent is selected from one or more of deionized water, glycerol and ethanol, and is in any proportion when mixed.
8. The root canal filling material of bioactive glass as claimed in claim 1, wherein: the root canal filling material is a root canal sealer, a root canal filler or a pulp capping agent used in oral root canal treatment.
9. The method for producing a root canal filling material containing a bioactive glass according to any one of claims 1 to 8, wherein: the method comprises the following steps:
1) weighing bioactive glass, an X-ray radiation resisting agent and a thickening agent according to the formula and the mass ratio of each component in the formula, and grinding the bioactive glass, the X-ray radiation resisting agent and the thickening agent by using a grinding instrument until the bioactive glass, the X-ray radiation resisting agent and the thickening agent are uniformly mixed;
2) and (3) uniformly mixing the uniform powder obtained in the previous step with a solvent according to a mass ratio, and forming uniform paste at normal temperature to obtain the root canal filling material containing the bioactive glass.
10. The method for preparing a root canal filling material containing bioactive glass according to claim 9, wherein:
step 1) also comprises the steps of weighing bioactive components, mixing the bioactive components with bioactive glass, an X-ray radiation inhibitor and a thickening agent, and grinding;
the particle size of the bioactive glass particles in the step 1) is less than 100 mu m;
grinding to be uniformly mixed in the step 1), wherein the grinding is carried out for 5min-10min to be uniform;
and 2) uniformly mixing in the step 2), namely uniformly stirring on a glass plate for 2-5 min by using a stirring knife.
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| CN101596215A (en) * | 1998-09-10 | 2009-12-09 | 美国生物材料公司 | The application of bioactive glass compositions in anti-inflammatory and antimicrobial |
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| CN112057348A (en) * | 2019-05-23 | 2020-12-11 | 浙江大学 | Multiple composition for tooth sealing treatment |
| US20210186824A1 (en) * | 2018-06-07 | 2021-06-24 | Sonendo, Inc. | Material to fill dental spaces |
| CN113171306A (en) * | 2021-04-26 | 2021-07-27 | 北京大学口腔医学院 | Bioactive material for endodontic treatment, preparation method and application thereof |
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| CN101596215A (en) * | 1998-09-10 | 2009-12-09 | 美国生物材料公司 | The application of bioactive glass compositions in anti-inflammatory and antimicrobial |
| US20160051457A1 (en) * | 2013-03-28 | 2016-02-25 | Queen Mary And Westfield College University Of London | Chlorine-containing silicate glasses and glass ceramics |
| US20210186824A1 (en) * | 2018-06-07 | 2021-06-24 | Sonendo, Inc. | Material to fill dental spaces |
| CN112057348A (en) * | 2019-05-23 | 2020-12-11 | 浙江大学 | Multiple composition for tooth sealing treatment |
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Application publication date: 20211224 |