CN110882166A - Stable calcium phosphate root canal filler - Google Patents
Stable calcium phosphate root canal filler Download PDFInfo
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- CN110882166A CN110882166A CN201911259376.3A CN201911259376A CN110882166A CN 110882166 A CN110882166 A CN 110882166A CN 201911259376 A CN201911259376 A CN 201911259376A CN 110882166 A CN110882166 A CN 110882166A
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Abstract
The invention belongs to the field of medical materials, and relates to a root filling agent, in particular to a root filling agent capable of being stably stored and a preparation method thereof, wherein the root filling agent consists of solid-phase powder and liquid-phase components, and is characterized by comprising the solid-phase powder and the liquid-phase components, wherein the solid-phase powder comprises, by mass, 60-90 parts of calcium phosphate powder, 10-20 parts of β -cyclodextrin, 10-20 parts of chitosan bentonite and 20-40 parts of a developing agent, and the liquid-phase components comprise, by mass, 40-120 parts of an organic solvent.
Description
Technical Field
The invention belongs to the field of medical materials, relates to a root canal filler, and particularly relates to a root canal filler capable of being stably stored and a preparation method thereof.
Background
Root canal filling is the most commonly used method for treating pulpitis and periapical periodontitis, and a root canal filling material is one of important factors affecting the efficacy of root canal treatment. The root canal fillers currently used clinically mainly include three types, i.e., solid, paste and liquid.
The solid root canal filling material (such as gutta-percha point, titanium-nickel alloy point, silver point, plastic point and the like) has no adhesiveness, can not be adhered with the internal structure of the root canal, can not enter the bent root canal and the side auxiliary root canal, can not form tight sealing, and the gutta-percha point must be matched with root canal paste for use. Paste root filling materials (such as zinc oxide clove oil, calcium hydroxide, iodoform, resins, glass ionomer cement and other pastes) can shrink in volume during the curing process, are dissolved in water or tissue fluid, and have micro-gaps with the root canal wall to cause micro-leakage, so that the apical foramen cannot be completely sealed. Although the paste has a certain improvement effect when used together with the gutta-percha point, the problem is difficult to solve fundamentally, and the clinical operation time is long. Liquid underfill materials (such as FR novolac) tend to penetrate into dentinal tubules and cause discoloration of teeth, affecting aesthetics, and are irritating and cytotoxic to tissue during polymerization. Although the gutta-percha point and paste root filling material is the most common root canal filling method in clinic, the biocompatibility is poor, if the gutta-percha point and the root filling material are carelessly beyond the root tip, long-term foreign body stimulation is formed, and some materials have stimulation and corrosiveness on tissues and even cause enamel development defects of inherited permanent teeth and the like.
The calcium phosphate cement is an orthopedic material and can be self-solidified under physiological condition to obtain solidified product similar to human bone tissue. The calcium phosphate bone cement has good biocompatibility and can be arbitrarily shaped according to the defect part. After being hydrated, the calcium phosphate cement is converted into hydroxyapatite which can guide bone growth. The self-curing performance and biocompatibility of the calcium hydroxide paste are obviously superior to those of calcium hydroxide paste, and the calcium hydroxide paste also has potential dentin reconstruction function. The product after solidification is hydroxyapatite which is similar to inorganic components of human hard tissues, but calcium phosphate bone cement has degradability and is easily dispersed by blood or body fluid after filling, so that the volume of the material is reduced, bacteria easily enter the root canal again for reproduction, inflammation is recurrent, and treatment fails, and the traditional calcium phosphate bone cement needs to be prepared by a doctor on site, so that the defects exist: firstly, the doctor can influence the performance of the bone cement by on-site blending; secondly, tools prepared on site need to be disinfected in advance; third, physician scheduling increases working time.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a calcium phosphate root canal filler which can be stably stored for more than 1 year, is not easy to separate solid from liquid, and can not be dispersed when the root canal filler is implanted into a root apex.
In order to achieve the purpose, the invention adopts the technical scheme that:
the stable calcium phosphate root canal filler consists of solid phase powder and liquid phase component, and features that the solid phase powder consists of calcium phosphate powder 60-90 weight portions, β -cyclodextrin 10-20 weight portions, chitosan bentonite 10-20 weight portions and developer 20-40 weight portions, and the liquid phase component consists of organic solvent 20-90 weight portions.
Further, the solid phase powder comprises, by mass, 80 parts of a-tricalcium phosphate powder, 15 parts of β -cyclodextrin, 15 parts of chitosan bentonite and 30 parts of a developer, wherein the developer is iodoform, a solvent in the liquid phase component is glycerol, and the liquid phase component comprises, by mass, 50 parts of an organic solvent.
Further, the preparation method of the chitosan bentonite comprises the following steps:
(1) adding sodium bentonite with the granularity of 100-400 meshes into water with the mass 10-30 times of that of the bentonite, stirring and dispersing for 0.5-3 hours to obtain bentonite suspension;
(2) dissolving chitosan with the mass being 0.5-3 times of that of bentonite in an acetic acid solution with the mass concentration of 1% to prepare a chitosan solution with the mass concentration of 2-8% and the pH value of 3-6;
(3) uniformly adding the bentonite suspension into the chitosan solution within 6-12 hours at 50-100 ℃ under stirring, and continuing to react for 20-50 hours after the bentonite suspension is added to obtain a reaction completion solution;
(4) and filtering, washing and drying the reaction finished liquid to obtain the chitosan bentonite.
Still further, the preparation method of the chitosan bentonite comprises the following steps:
(1) adding sodium bentonite with the granularity of 250 meshes into water with the mass 20 times of that of the bentonite, stirring and dispersing for 2 hours to obtain bentonite suspension;
(2) dissolving chitosan with the mass 2 times of that of bentonite in an acetic acid solution with the mass concentration of 1% to prepare a chitosan solution with the mass concentration of 5% and the pH value of 4.5;
(3) uniformly adding the bentonite suspension into the chitosan solution within 8 hours under the stirring at the temperature of 80 ℃, and continuing to react for 35 hours after the bentonite suspension is added to obtain a reaction completion solution;
(4) and filtering, washing and drying the reaction finished liquid to obtain the chitosan bentonite.
Still further, the mass ratio of the solid-phase powder to the liquid phase is 1 (0.4-0.7).
Still further, the calcium phosphate in the solid phase powder is selected from one or more of tricalcium phosphate, tetracalcium phosphate, octacalcium phosphate, anhydrous calcium hydrophosphate, calcium hydrophosphate dihydrate, monocalcium phosphate, calcium pyrophosphate, hydroxyapatite, fluorapatite, strontium apatite and apatite carbonate.
Still further, in the liquid phase component, the organic solvent is glycerol or polyethylene glycol.
Still further, the solid phase powder also comprises the following components in parts by mass: 2-5 parts of an antibacterial agent selected from: one or more of metronidazole, tinidazole, tylenol and tobramycin, preferably, the solid phase powder further comprises the following components in parts by mass: 4 parts of antibacterial agent.
Still further, the developer is selected from: at least one of iodoform, barium sulfate, strontium chloride and zirconium dioxide, and preferably, the developer is iodoform.
The properties of bentonite are strongly related to the kind of exchangeable cations between the layers. Bentonite is generally classified into calcium bentonite and sodium bentonite according to the kind of cation mainly exchangeable between layers.
The bentonite has adsorbability and cation exchange performance, and can be used for removing edible oil toxin, purifying gasoline and kerosene, and treating wastewater; the fire-retardant coating has good water swelling property, dispersion, suspension and slurry making property, so that the fire-retardant coating is used for drilling mud and flame retardance (suspension fire extinguishing); can also be used as filler in paper industry to optimize the properties of coating, such as adhesion, covering power, water resistance, washing resistance, etc
And performing cation exchange on the chitosan and the bentonite to form chitosan bentonite.
β -cyclodextrin is widely used for separating organic compounds and organic synthesis, and also used as pharmaceutical adjuvant, food additive, etc. at present, people prepare natural cyclodextrin and modified cyclodextrin with some drug molecules without biocompatibility to prepare inclusion compound.
The root canal filler of the invention is not solidified under the anhydrous condition, and the solid-liquid separation can not occur after long-term storage, probably because the chitosan bentonite and β -cyclodextrin are added into the solid phase powder, the chitosan bentonite, β -cyclodextrin and organic solvent are wrapped around the calcium phosphate powder through the cross-linking reaction or the van der Waals force winding effect, the calcium phosphate particles of the root canal filler do not settle, the system is kept stable, and the solid-liquid separation does not occur.
Although the calcium phosphate solid phase powder can delay the time of the solidification reaction by adding the organic solvent, CPC particles in the solid phase powder can be settled to cause solid-liquid separation, and after various methods are tried by the inventor of the application, chitosan bentonite and β -cyclodextrin are added into the solid phase powder, and the chitosan bentonite and β -cyclodextrin surround the calcium phosphate powder by a cross-linking reaction or van der Waals force winding action with the organic solvent, so that the stability of the system is improved.
The root canal filling agent is stored in a container at 4-50 ℃, the root canal filling agent can be stored at normal temperature, is convenient to store, is prepared into paste in advance, and is directly injected or filled into a tooth root. The paste can be stored in a container because the paste does not contain water, the paste can not be hydrated in the storage process, the storage time can reach more than 1 year, the commercial popularization and application of the product are facilitated, and the dental root filling agent is cured and reacts with water to generate hydroxyapatite after being extruded into a dental root canal.
The invention also provides the application of the root canal filler, which is directly injected and filled by a filling mode or a syringe.
Compared with the prior art, the invention has the beneficial effects that:
1) the tooth root filling agent prepared by the invention is simple to operate, the sample is placed in the container and is injected or filled when in use, the solid phase and the liquid phase do not need to be mixed on site, and the operation time and the risk of introducing bacteria are reduced.
2) The added chitosan bentonite, β -cyclodextrin and organic solvent can lead the root filling agent to be stored in a container in a sealing way and be stored stably for a long time at room temperature without solid-liquid separation, the root filling agent has good fluidity and injection performance, the filling agent is stable paste in the container, after being filled into the root canal, the filling agent is gradually solidified by the liquid in the environment, the solidification time is greatly shortened, and the patient can conveniently eat.
3) The root filling agent does not contain water and is stored in the container, and the root filling agent is cured when meeting water after being added into the root canal, can resist the washing of body fluid, is not dispersed in the initial filling stage, can ensure that the filling material is tightly combined with the root canal, and prevents the generation of gaps.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
250 mesh sodium bentonite (Changtai bentonite Co., Ltd.)
Example 1
Preparing chitosan bentonite:
(1) adding sodium bentonite with the granularity of 250 meshes into water with the mass 20 times of that of the bentonite, stirring and dispersing for 2 hours to obtain bentonite suspension;
(2) dissolving chitosan with the mass 2 times of that of bentonite in an acetic acid solution with the mass concentration of 1% to prepare a chitosan solution with the mass concentration of 5% and the pH value of 4.5;
(3) uniformly adding the bentonite suspension into the chitosan solution within 8 hours under the stirring at the temperature of 80 ℃, and continuing to react for 35 hours after the bentonite suspension is added to obtain a reaction completion solution;
(4) and filtering, washing and drying the reaction finished liquid to obtain the chitosan bentonite.
Example 2
In one embodiment of the calcium phosphate root canal filler of the present invention, the root canal filler comprises a solid-phase powder and a liquid-phase component;
the solid phase powder comprises, by mass, 60 parts of a-tricalcium phosphate powder, 10 parts of β -cyclodextrin, 10 parts of chitosan bentonite and 20 parts of iodoform, and the liquid phase comprises, by mass, 40 parts of glycerol.
Example 3
In one embodiment of the calcium phosphate root canal filler of the present invention, the root canal filler comprises a solid-phase powder and a liquid-phase component;
the solid phase powder comprises, by mass, 75 parts of a-tricalcium phosphate powder, 15 parts of β -cyclodextrin, 15 parts of chitosan bentonite and 30 parts of iodoform, and the liquid phase comprises, by mass, 80 parts of glycerol.
Example 4
In one embodiment of the calcium phosphate root canal filler of the present invention, the root canal filler comprises a solid-phase powder and a liquid-phase component;
the solid phase powder comprises, by mass, 90 parts of a-tricalcium phosphate powder, 20 parts of β -cyclodextrin, 20 parts of chitosan bentonite and 40 parts of iodoform, and the liquid phase comprises, by mass, 119 parts of glycerol.
Comparative example 1
A calcium phosphate root canal filler comprises solid phase powder and liquid phase component;
the solid phase powder comprises 75 parts by mass of a-tricalcium phosphate powder, 30 parts by mass of β -cyclodextrin and 30 parts by mass of iodoform, and the liquid phase component comprises 80 parts by mass of glycerol.
This comparative example is substantially the same as example 3 except that chitosan bentonite is not included.
Comparative example 2
A calcium phosphate root canal filler comprises solid phase powder and liquid phase component;
the solid-phase powder comprises the following components in parts by mass: 75 parts of a-tricalcium phosphate powder, 30 parts of chitosan bentonite and 30 parts of iodoform; the liquid phase component comprises the following components in parts by mass: 35 parts of glycerol.
This comparative example is the same as example 3 except that β -cyclodextrin was not included.
Comparative example 3
A calcium phosphate root canal filler comprises solid phase powder and liquid phase component;
the solid-phase powder comprises the following components in parts by mass: 75 parts of a-tricalcium phosphate powder and 30 parts of iodoform; the liquid phase component comprises the following components in parts by mass: 35 parts of glycerol.
This comparative example is the same as example 3 except that β -cyclodextrin, chitosan bentonite, were not included.
Comparative example 4
A calcium phosphate root canal filler comprises solid phase powder and liquid phase component;
the solid phase powder comprises, by mass, 75 parts of a-tricalcium phosphate powder, 15 parts of β -cyclodextrin, 15 parts of bentonite and 30 parts of iodoform, and the liquid phase powder comprises, by mass, 35 parts of glycerol.
This comparative example is substantially the same as example 3 except that bentonite is used in place of chitosan bentonite.
The following performance tests were performed on the fillers prepared in examples 2-4, comparative examples 1-4.
1. Fluidity of the resin
According to the 7.2 test in the standard YY0717-2009 of the people's republic of china medical practice, a graduated syringe was used to deliver 0.05ml of the filler, which was placed in the center of one glass plate, and 180s after tempering, the second glass plate was placed in the middle of the top of the filler, followed by the weight block, giving a total applied mass of 120 g. The weight was removed in 10min and the maximum and minimum diameters of the filler were measured.
As shown in Table 1, the products of examples 2 to 4 had good fluidity, and the maximum diameter of the disks of the fluidity test tests of the samples of examples 2 to 4 was 26mm and the minimum diameter was 24mm, and the fluidity was remarkably improved by adding the thickener in conformity with the specification of iso6876, and the diameters of the samples were all larger than 20 mm. The filler can reach the root canal apex, so when the filler of examples 2-4 is used for filling the tooth, the gutta percha apex is not needed, and the problem that the gutta percha apex root filling material exceeds the root apex to form foreign body stimulation can be avoided.
2. Curing time
According to the test of 7.4 in the national medical and pharmaceutical industry standard YY0717-2009, a stainless steel die is placed on a flat glass sheet, the blended sealing material is filled in the stainless steel die, after the blending is finished for 120s, the materials of the examples 2-4 and the comparative examples 1-4 are placed on a metal block in a constant temperature and humidity box, then the metal block is placed in SBF body fluid, the pressure head of a penetrometer is lightly and vertically placed on the horizontal plane of the sealing material every 60s, the operation is repeated until no indentation appears by naked eyes, and the curing time is recorded.
The results are shown in Table 1, the addition of chitosan bentonite does not affect the setting time, which should not be too fast due to the time required for the physician to manipulate the root filling material, considering that the working time is within 30min, the setting time should exceed 30min, and too long a setting time may affect the patient's food intake.
3. Dimensional change after curing
According to the 7.6 test in the standard YY0717-2009 of the people's republic of China, a mold was placed on a glass plate covered with a polyethylene film, the solid phase powder in examples 2-4 and comparative examples 1-4 was blended with a liquid phase, and the blended material was slightly super-filled in the mold. Another glass sheet coated with a polyethylene film was placed on top of the filler. The mold is secured to the C-clamp along with the glass sheet. 5min after the start of the mixing, the material and the C-shaped clamp are put into the SBF body fluid for 3h and then taken out. The mold was rubbed back and forth on a wet sandpaper of P600 to flatten both ends of the sample, the sample was taken out of the mold, the height of the sample was measured, and the sample was stored in distilled water at 37 ℃ for 30 days to measure the height of the sample again. The change in specimen length and the percent of original length were calculated and the results are shown in table 1, with the sample size remaining unchanged in the examples of the invention.
TABLE 1
4. Dissolution rate
The test was carried out according to 7.7 of the national standards for the pharmaceutical industry, YY0717-2009, by placing the mold on a glass plate, blending the solid powder with the liquid phase in examples 2-4 and comparative examples 1-4, respectively, and slightly overfilling the blend in the mold. The top of the filler was covered with a polyethylene film coated glass plate. The above materials were placed in a constant temperature and humidity cabinet for 24 hours, the specimens were removed from the molds, and the quality was measured after carefully trimming the burrs.
The 7 samples were placed in a tray and were not allowed to touch and interfere with each other. Adding 50ml of water, covering the tray cover and putting the tray cover into a constant temperature and humidity box for 24 hours, then taking out the sample, washing the sample in a shallow tray by using 2ml-3ml of clean water, checking the washing in the tray, and indicating that the material is decomposed if particles appear. The sample was removed, the water in the tray was evaporated, the water did not boil, and the tray was then oven dried in an oven at 110 ℃ until the tray had a constant weight. The trays were cooled to room temperature in a desiccator before each weighing. The difference of the mass of the final tray from the initial tray mass was calculated, dissolution = difference of mass of final tray from initial tray mass/initial mass of sample. The results are shown in Table 2.
5. Compressive strength
Compressive strength was determined according to the classical mechanics in iso 9917: 1991.
The results are shown in Table 2.
TABLE 2
As shown in Table 2, the dissolution rate of example 2 is the lowest, the degradation rate of example 2-4 is reduced by adding chitosan bentonite and β -cyclodextrin to the solid powder, and the compressive strength of the root filler is significantly improved by adding bentonite to example 2-4
6. X-ray opacity
According to the test of 7.8 in the Chinese people's republic of China medical industry standard YY0717-2009, YY0717-2009 specifies that the X-ray radiation resistance of the sealing material is not lower than the equivalent radiation resistance of an aluminum plate with the thickness of 3 mm. The prepared filler of examples 2 to 4 was filled into a mold, and the top and bottom of the mold were covered with cover plates to mold the filler to a thickness of 1 mm. The mold is placed in the center of the dental X-ray occlusal splint, a wedge-shaped stepped aluminum plate is placed beside the dental X-ray occlusal splint, and a same cover plate is placed below the wedge-shaped stepped aluminum plate. The sample, wedge-shaped stepped aluminum plate and film were irradiated using 65kV X-rays at a distance of about 300mm from the film for a time sufficient to provide an optical density value of between 0.5 and 2.5 for the 1mm thick aluminum wedge and the film beneath it. After film development, fixing and drying, the optical densities of the samples and the images of the wedge-shaped stepped aluminum plate were compared using a densitometer. The X-ray opacity of the sample is expressed in millimeters of equivalent aluminum plate thickness. The results show that the formulated fillers of examples 2-4 have a radiopacity equivalent to a 7.1mm thick aluminum plate, and are satisfactory for clinical use.
7. Storage time:
the samples of examples 24-comparative examples 1 to 4 were placed in a sealed container and stored at room temperature for 30 days, 2 months, 6 months, and 12 months, and the phases of the samples were observed. The products of examples 2 to 4 can be stored for 12 months, the product performance is the same as that of the product just prepared, and the products of comparative examples 1 to 4 can cause solid-liquid separation when being placed for more than 2 months.
TABLE 3
| Group of | 30 days | 2 month | 6 month | 12 month |
| Practice of Example 2 | The product is not solidified, is fluid and can be handled Consistent with the product prepared on site | The product is not solidified, is fluid and can be handled Consistent with the product prepared on site | The product is not solidified, is fluid and can be handled Consistent with the product prepared on site | The product is not solidified, is fluid and can be handled Consistent with the product prepared on site |
| Practice of Example 3 | The product is not solidified, is fluid and can be handled Consistent with the product prepared on site | The product is not solidified, is fluid and can be handled Consistent with the product prepared on site | The product is not solidified, is fluid and can be handled Consistent with the product prepared on site | The product is not solidified, is fluid and can be handled Consistent with the product prepared on site |
| Practice of Example 4 | Product(s)Non-setting, flowable, when handled Consistent with the product prepared on site | The product is not solidified, is fluid and can be handled Consistent with the product prepared on site | The product is not solidified, is fluid and can be handled Consistent with the product prepared on site | The product is not solidified, is fluid and can be handled Consistent with the product prepared on site |
| Comparison of Example 1 | The product is not solidified, is fluid and can be handled Consistent with the product prepared on site | The product is not solidified and is separated from solid and liquid | The product is not solidified and is separated from solid and liquid | The product is not solidified and is separated from solid and liquid |
| Comparison of Example 2 | The product is not solidified, is fluid and can be handled Consistent with the product prepared on site | The product is not solidified and is separated from solid and liquid | The product is not solidified and is separated from solid and liquid | The product is not solidified and is separated from solid and liquid |
| Comparison of Example 3 | The product is not solidified, is fluid and can be handled Consistent with the product prepared on site | The product is not solidified and is separated from solid and liquid | The product is not solidified and is separated from solid and liquid | The product is not solidified and is separated from solid and liquid |
| Comparison of Example 4 | The product is not solidified, is fluid and can be handled Consistent with the product prepared on site | The product is not solidified and is separated from solid and liquid | The product is not solidified and is separated from solid and liquid | The product is not solidified and is separated from solid and liquid |
In conclusion, the root canal filler prepared by the invention is simple to operate, the added chitosan bentonite and β -cyclodextrin can prevent the root canal filler from being dispersed when being placed in body fluid, the root canal filler prepared by the invention has good fluidity and injection performance, solid and liquid are not separated, the filler is stable paste in a container, after being filled into a root canal, the filler is gradually solidified by the liquid in the environment, the solidification time is greatly shortened, and a patient can take food after being filled for 2 hours.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. The stable calcium phosphate root canal filler consists of solid phase powder and liquid phase component, and features that the solid phase powder consists of calcium phosphate powder 60-90 weight portions, β -cyclodextrin 10-20 weight portions, chitosan bentonite 10-20 weight portions and developer 20-40 weight portions, and the liquid phase component consists of organic solvent 40-120 weight portions.
2. The calcium phosphate root canal filler according to claim 1, wherein the solid phase powder comprises 80 parts by mass of a-tricalcium phosphate powder, 15 parts by mass of β -cyclodextrin, 15 parts by mass of chitosan bentonite, and 30 parts by mass of a developing agent, the developing agent is iodoform, the solvent in the liquid phase component is glycerol, and the liquid phase component comprises 50 parts by mass of an organic solvent.
3. The calcium phosphate endodontic filler according to claim 1, wherein said chitosan bentonite is prepared by the following method:
(1) adding sodium bentonite with the granularity of 100-400 meshes into water with the mass 10-30 times of that of the bentonite, stirring and dispersing for 0.5-3 hours to obtain bentonite suspension;
(2) dissolving chitosan with the mass being 0.5-3 times of that of bentonite in an acetic acid solution with the mass concentration of 1% to prepare a chitosan solution with the mass concentration of 2-8% and the pH value of 3-6;
(3) uniformly adding the bentonite suspension into the chitosan solution within 6-12 hours at 50-100 ℃ under stirring, and continuing to react for 20-50 hours after the bentonite suspension is added to obtain a reaction completion solution;
(4) and filtering, washing and drying the reaction finished liquid to obtain the chitosan bentonite.
4. The calcium phosphate endodontic filler according to claim 3, wherein said chitosan bentonite is prepared by the following method:
(1) adding sodium bentonite with the granularity of 250 meshes into water with the mass 20 times of that of the bentonite, stirring and dispersing for 2 hours to obtain bentonite suspension;
(2) dissolving chitosan with the mass 2 times of that of bentonite in an acetic acid solution with the mass concentration of 1% to prepare a chitosan solution with the mass concentration of 5% and the pH value of 4.5;
(3) uniformly adding the bentonite suspension into the chitosan solution within 8 hours under the stirring at the temperature of 80 ℃, and continuing to react for 35 hours after the bentonite suspension is added to obtain a reaction completion solution;
(4) and filtering, washing and drying the reaction finished liquid to obtain the chitosan bentonite.
5. The calcium phosphate endodontic filler according to claim 1, wherein the mass ratio of the solid phase powder to the liquid phase is 1 (0.4-0.7).
6. The calcium phosphate root canal filler of claim 1, wherein the calcium phosphate in the solid phase powder is selected from one or more of tricalcium phosphate, tetracalcium phosphate, octacalcium phosphate, calcium hydrogen phosphate anhydrous, calcium hydrogen phosphate dihydrate, calcium dihydrogen phosphate, calcium pyrophosphate, hydroxyapatite, fluorapatite, strontium apatite, and carbonate-containing apatite.
7. The calcium phosphate root canal filler according to claim 1, wherein the organic solvent in the liquid-phase component is glycerin or polyethylene glycol.
8. The calcium phosphate endodontic filler according to claim 1, wherein said solid phase powder further comprises the following components in parts by mass: 2-5 parts of an antibacterial agent selected from: one or more of metronidazole, tinidazole, tylenol and tobramycin, preferably, the solid phase powder further comprises the following components in parts by mass: 4 parts of antibacterial agent.
9. The calcium phosphate endodontic filler of claim 1, wherein said imaging agent is selected from the group consisting of: at least one of iodoform, barium sulfate, strontium chloride and zirconium dioxide, and preferably, the developer is iodoform.
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| CN113480181A (en) * | 2021-08-17 | 2021-10-08 | 辽宁瑞晟新材料科技有限公司 | Preparation method of antibacterial glass particles |
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| DE2211128A1 (en) * | 1972-03-08 | 1973-09-13 | Erich Kopp | Dental prostheses - cast from compsn contg acrylamide and methylene-bisacrylamide, initiator activator and opt fillers |
| EA200100908A1 (en) * | 2001-07-25 | 2003-04-24 | Инсомуддин Садыкович Соатов | FILLING MATERIAL FOR ROOT CHANNELS OF TEETH |
| CN1446530A (en) * | 2003-01-29 | 2003-10-08 | 华东理工大学 | Self-solidifying calcium phosphate filling material for canalis radicis dentis |
| CN1857190A (en) * | 2006-03-03 | 2006-11-08 | 厦门大学 | Root canal filling paste capable of being stored and injected |
| CN101475187A (en) * | 2009-01-16 | 2009-07-08 | 广西大学 | Chitosan bentonite and preparation thereof |
| CN103462814A (en) * | 2013-08-20 | 2013-12-25 | 青岛华新华义齿技术有限公司 | Denture adhesive |
| CN105853238A (en) * | 2016-04-25 | 2016-08-17 | 于金华 | Dental composition for detecting and removing dentin caries tissue and preventing carious lesion |
| CN107949378A (en) * | 2016-06-30 | 2018-04-20 | 泰合生技药品股份有限公司 | For bestowing the molten film of quick-acting mouths of local anaesthesia |
| CN109982680A (en) * | 2016-11-21 | 2019-07-05 | 玛汝奇公司 | Oxpara composition |
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| CN113480181A (en) * | 2021-08-17 | 2021-10-08 | 辽宁瑞晟新材料科技有限公司 | Preparation method of antibacterial glass particles |
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