CN106377433A - Anti-microbial root canal filling material and preparation method thereof - Google Patents
Anti-microbial root canal filling material and preparation method thereof Download PDFInfo
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Abstract
The invention concretely relates to an anti-microbial root canal filling material containing nano-sized magnesium hydroxide, which comprises a solid-liquid dispersion system and a solid-phase component, wherein the weight ratio of nano-sized magnesium hydroxide to solid-phase component in the solid-liquid dispersion system is 0.1-0.3:1. The solid-liquid dispersion system is a fluid suspension obtained by uniformly dispersing the nano-sized magnesium hydroxide in a dispersant solution; the dispersant solution is a miscible solution of an aqueous solution with weight concentration of 0.1-3 wt% of the dispersant, or water and ethanol; and the dispersant is a mixer of one or more than two of polyvinyl alcohol, polyethylene glycol, polyacrylic acid, sodium polyacrylate, carboxymethylcellulose sodium, polyvinylpyrrolidone, sodium dodecyl sulfate and sodium hexametaphosphate. The antibiosis experiment shows that the killing rate of nano-sized magnesium hydroxide on gram-positive cocci and gram-negative bacillus can reach 100% in 7 h. The hemolysis test and cytotoxicity evaluate experiment show that the anti-microbial root canal filling material containing the nano-sized magnesium hydroxide has good biocompatibility.
Description
Technical field
The invention belongs to Medical oral cavity root canal filling material technical field is and in particular to a kind of anti-containing nano-sized magnesium hydroxide
Bacterium property tooth root canal filling material and preparation method thereof.
Background technology
Pulp vitality test is the common multiple odontopathy of clinical oral.Root canal is pulpitis and periapical periodontitis treatment
Most efficient method.The purpose of root-canal filling is closely to close root pipe for a long time with filler, prevents sending out of periapical lesion
Healing that is raw, promoting periapical lesion.However, tooth root canal filling material cannot be carried out to remaining or leaking into the bacterium in canalis radicis dentis
Persistently the main cause often leading to root canal treatment failure is killed in suppression.With the continuous progress of microbial identification research, people
Have been found that many canalis radicis dentis pathogenic bacteria, such as enterococcus faecalis, Candida albicans, Fusobacterium nucleatum etc., as enterococcus faecalis is as one kind
The simultaneous gram-positive cocci needing anaerobism, in root pipe, recall rate may be up to 40%, and in the case that root pipe is treated again, recall rate is high
Reach 24～77%.Moreover, this kind of canalis radicis dentis detects germ is also clinical common drug-fast bacteria, also often works in coordination with other bacteriums
Effect leads to mixed infection in canalis radicis dentis.
At present, domestic and international tooth root canal filling material, can be divided into calcium hydroxide kind, epoxy resin, many by its main component
Polyformaldehyde class, zinc-oxide-eugenol class etc., other are if hydroxyapatite, calcium phosphate, glass ionomer etc. are also continuous
Among research and application.These tooth root canal filling materials are to the many drug-fast bacterias in the infections of dental pulp of oral cavity（As enterococcus faecalis）Suppression
Kill ability all limited.For example, the sterilization capability of calcium hydroxide depends on the OH that root canal filling paste provides-Concentration, only
When pH value is maintained at a higher level, the calcium hydroxide in root pipe just has bactericidal activity.And many drug-fast bacterias are to strong
The tolerance of alkali environment is very strong.Isolated Tooth experiment display：Calcium hydroxide is to the enterococcus faecalis being present in dentinal tubule no
Effect.The enterococcus faecalis thus failing to be killed can be adhered to dentin collagen in tissue fluid environment, enters dentinal tubule shape
Become to infect again, lead to root canal failure.
Nano-sized magnesium hydroxide is a kind of new inorganic material with extensive use, can be used as Green Flammability agent, spent acidic
Thing nertralizer, adsorbent, food preservative, fertilizer additive, heavy metal removing, flue gas desulfurization, soil treatment with simulated acid rain and pH adjust
Section agent etc., is always the important source material of gastric acid inhibitory medicine in biomedical sector.
Studies have found that in recent years：Nano-sized magnesium hydroxide has broad spectrum antibacterial performance, document（Dong CX, Cairney
J, Sun QHi. Investigation of Mg(OH)2nanoparticles as an antibacterial agent.
J Nanopart Res, 2010, 12: 2101-2109）Provide nano-sized magnesium hydroxide to Escherichia coli, Staphylococcus aureus
Several difference such as bacterium and azophenlyene Burkholderia section purpose bacterium is respectively provided with the evidence of inhibitory or killing effect, and confirms this bactericidal property
With the OH in nano-sized magnesium hydroxide suspension-And Mg2+Unrelated.It is generally believed that the antibacterial mechanisms of nano-sized magnesium hydroxide are normal with other
The inorganic nano antibacterial material seen（As nano-ZnO, TiO2, Ag etc.）Similar, that is, the oxygen dissolving in the solution passes through single electron also
Former reaction generates peroxide O2-.Peroxide O2-There is in alkaline environment chemical stability, thus the O of high concentration2-Can
Exist on nano-sized magnesium hydroxide surface.This active oxygen is easily reacted with the peptide bond in bacterial cell wall proteins, thus
Destroy exine structure, reach the effect of quick sterilization.Moreover, the high nano-sized magnesium hydroxide of interfacial energy is acceptable
It is adsorbed onto bacterium surface and forms absorbing complex, reach suppression and kill effect by disturbing the normal physiological metabolism process such as the breathing of bacterium
Really.Therefore, nano-sized magnesium hydroxide can produce strong inhibitory or killing effect to all kinds of bacteriums of often detection in the infections of dental pulp of oral cavity, and carefully
Bacterium is not likely to produce drug resistance.
Magnesium is the macroelement of human body, and in normal human, 60%～65% magnesium is present in bone, in tooth, is only second in bone
Calcium, the content of phosphorus.Magnesium is element necessary to osteocyte 26S Proteasome Structure and Function, to promoting bone growing and osteanagenesis, maintain bone and
The intensity of tooth and density have important function.Research finds, in tooth enamel, content of magnesium is higher, and tooth is more difficult earlier
Decayed tooth and carious tooth occur；Magnesium replenishers may stop or delay periodontitis to develop.Nano-sized magnesium hydroxide can after being absorbed by the body
Generate Mg2+Become magnesium replenishers.Therefore, the Novel toothed root canal filling material containing nano-sized magnesium hydroxide that the present invention provides can not only
Play its unique anti-microbial property moreover it is possible to help human body to increase absorb magnesium elements, thus becoming the one kind being applied to oral environment
New type filling material.
Content of the invention
Present invention aim to overcome that prior art defect, provide a kind of root canal filling material that can persistently play antibiotic property
Material and preparation method thereof.
For achieving the above object, the present invention adopts the following technical scheme that：
A kind of antibiotic property tooth root canal filling material, including solid-liquid dispersing system and solid phase components, wherein, sends out in solid-liquid dispersing system
Wave the nano-sized magnesium hydroxide of different morphologies of antibacterial action and the weight of solid phase components than for 0.1 0.3：1.
Specifically, described solid-liquid dispersing system refers to nano-sized magnesium hydroxide is dispersed in obtained in dispersant solution
Suspension；Described dispersant solution is the aqueous solution of dispersant weight concentration 0.1wt% 3wt% or water and the dissolving each other of ethanol
Solution；The weight concentration of described dispersant refers to the percentage that dispersant weight is with respect to magnesium hydroxide weight and liquid phase weight sum
Than（Liquid phase refers to the solution that dispersant is with water composition or the solution of dispersant and water and ethanol composition）；Described dispersant is poly-
Vinyl alcohol, polyethylene glycol, polyacrylic acid, Sodium Polyacrylate, sodium carboxymethylcellulose, polyvinylpyrrolidone, dodecyl sulphur
One of sour sodium and calgon or two or more mixtures.Described suspension is to be uniformly dispersed and stability is high consolidates
Liquid dispersion.
Specifically, described solid phase components include calcium hydroxide, calcium chloride or magnesium chloride（As water reducer）, and dimethyl
Silicone oil or glycerine（Play lubrication）；Wherein, each raw material weight percentage of described solid phase components is：Calcium chloride or magnesium chloride
3% 6%, dimethicone or glycerine 3% 6%, balance of calcium hydroxide.
Above-mentioned antibiotic property tooth root canal filling material, the magnesium hydroxide playing antibacterial action is nanoscale, nanometer hydroxide
The specific surface area of magnesium is big, activity is high, and easy and root of the tooth pipe internal surface forms reliable and stable combination, makes in filler and canalis radicis dentis
Surface tight, product is more firm, antibacterial, anticorrosive, durable.
The preparation method of above-mentioned antibiotic property tooth root canal filling material, specially：Solid phase components are pressed 1 mg with solid-liquid dispersing system：
The ratio of 0.2 1.0ml is in harmonious proportion and uniformly obtains final product.Gained finished product is the preferable paste of mobility, directly uses.
In antibiotic property tooth root canal filling material of the present invention, play antibacterial action is nano-sized magnesium hydroxide, and it can be direct
Buy ordinary commercial products it is also possible to be prepared according to this area conventional method, or can also prepare as steps described below
Obtain：
Step one, molten with magnesium chloride, magnesium nitrate, magnesium sulfate or magnesium salts that magnesium acetate compound concentration is 0.01-1.5 mol/L
Liquid；
Step 2, under normal pressure and 50-80 DEG C of stirring condition, adjusts above-mentioned magnesium salt solution pH with NaOH or potassium hydroxide
It is worth to 10-13, continues stirring reaction 5-7h, add polyethylene glycol, Tween 80 or Sodium Polyacrylate during the course of the reaction, it adds
Enter the 1-8 wt% that amount is magnesium salts；
Step 3, reaction is cooled to room temperature after terminating, and then suspension is carried out separation of solid and liquid, and solid is scrubbed, be drying to obtain
Magnesium Hydroxide Nano-particles.Gained nano-sized magnesium hydroxide is needle-like, corynebacterium or hexagonal flake, and wherein corynebacterium major diameter is
100 300 nm, minor axis is 10 20 nm；Needle-like length 80 300 nm；Hexagonal flake diameter 20 100 nm.
Compared to the prior art, the antibiotic property tooth root canal filling material that the present invention provides has the advantage that：
1）Nano-sized magnesium hydroxide can cause a disease to multiple in root canal treatment and drug-fast bacteria plays and persistently excellent anti-kills performance；
2）The specific surface area of nano-sized magnesium hydroxide is big, activity is high, and easy and root of the tooth pipe internal surface forms reliable and stable combination, makes to fill out
Fill mixing material and root of the tooth pipe internal surface tight；
3）Magnesium is the macroelement in human body, and the nano-sized magnesium hydroxide in antibiotic property tooth root canal filling material can be used as magnesium replenishers
It is absorbed by the body, have no toxic side effect.
According to GBT 16886.5-2003 BiologicalEvaluationofMedicalDevice the 4th part：Interact with blood and test choosing
Select and the 5th part：The regulation of vitro cytotoxicity test carries out haemolysis to the antibiotic property tooth root canal filling material of the present invention respectively
Test and MTT cell toxicity test, test result indicate that：Antibiotic property tooth root canal filling material no hemolytic of the present invention, cell toxicant
Property be 0 grade, there is good biocompatibility.
Brief description
Fig. 1 is the X-ray diffractogram preparing gained nano-sized magnesium hydroxide using the inventive method（German Brooks D8
Advance x-ray diffractometer, with Cu-k α as radiation source, λ=1.54056）；As seen from Figure 1, all diffraction maximums all can be with
Hexagonal crystal system magnesium hydroxide（Space group P-3m1（164））Standard card JCPDS 00-044-1482 corresponding, and no other
The presence of crystalline phase diffraction maximum, illustrates that product is mainly hexagonal crystal system magnesium hydroxide；
Fig. 2 is the TEM electronic diffraction photo preparing gained nano-sized magnesium hydroxide using the inventive method（Hitachi H-800 type transmission
Electron microscope, England Oxford INCA energy disperse spectroscopy）；Knowable to the electronic diffraction photo of gained sample, this is hexagonal crystallographic texture.
Being further characterized by products obtained therefrom is magnesium hydrate hexagonal crystalline structure.
Fig. 3 is the TEM transmission electron microscope photo preparing gained nano-sized magnesium hydroxide using the inventive method（80000 times, Hitachi H-
800 type transmission electron microscopes, sample preparation drips on the copper mesh bearing carbon film using after absolute ethyl alcohol ultrasonic disperse, and in the air is done
Dry）, as seen from Figure 3, product be long 300nm about, dispersiveness preferably nano whiskers magnesium hydroxide（Hexagonal crystal system）；
Fig. 4 is the TEM transmission electron microscope photo preparing gained nano-sized magnesium hydroxide using the inventive method（80000 times, Hitachi H-800
Type transmission electron microscope, sample preparation drips on the copper mesh bearing carbon film using after absolute ethyl alcohol ultrasonic disperse, and in the air is done
Dry）, it can be seen that product be long 100nm about, dispersiveness preferably nano bar-shape magnesium hydroxide（Hexagonal crystal system）；
Fig. 5 is the TEM transmission electron microscope photo preparing gained nano-sized magnesium hydroxide using the inventive method（80000 times, Hitachi H-800
Type transmission electron microscope, sample preparation drips on the copper mesh bearing carbon film using after absolute ethyl alcohol ultrasonic disperse, and in the air is done
Dry）, it can be seen that product be 80nm about, dispersiveness preferably nano-hexagonal flake magnesium hydroxide（Hexagonal crystal system）；
For gained antibiotic property tooth root canal filling material of the present invention to colibacillary antibacterial effect, other Gram-negatives need Fig. 6
The antibacterial effect of oxygen bacterium or anaerobic bacteria is similar；
Fig. 7 is the antibacterial effect to staphylococcus aureus for the gained antibiotic property tooth root canal filling material of the present invention, other grams
The antibacterial effect of positive aerobic bacteria or anaerobic bacteria is similar.
Specific embodiment
With reference to embodiments technical scheme is further discussed in detail, but protection scope of the present invention
It is not limited thereto.
Embodiment 1
A kind of antibiotic property tooth root canal filling material, its preparation process is as follows：
One）The preparation of nano-sized magnesium hydroxide
Step one, the magnesium salt solution being 0.8 mol/L with magnesium chloride compound concentration；
Step 2, under normal pressure and 60 DEG C of stirring conditions, adjusts above-mentioned magnesium salt solution pH value to 10 with NaOH, continues stirring
Reaction 5h, adds Tween 80 during the course of the reaction, and the addition of Tween 80 is 1 wt% of magnesium salts；
Step 3, reaction is cooled to room temperature after terminating, and then gained suspension is carried out separation of solid and liquid, and solid is scrubbed, dry
Obtain final product Magnesium Hydroxide Nano-particles.Gained nano-sized magnesium hydroxide is in the long needle-like of 300 nm（Fig. 3）.
Two）The preparation of antibiotic property tooth root canal filling material
Weigh calcium hydroxide 9.2 g, magnesium chloride 0.5 g, dimethicone 0.3 g, nano-sized magnesium hydroxide 3 g respectively.With 0.2%
Polyvinyl alcohol water solution nano-sized magnesium hydroxide is made stable suspension（As can be using stirring or ultrasonic method by nanometer
Magnesium hydroxide is dispersed in the aqueous solution of 0.2% polyvinyl alcohol and obtains）.Then according to solid-to-liquid ratio 1 mg:0.2 ml, by hydrogen
Calcium oxide, magnesium chloride, dimethicone are added in the suspension of nano-sized magnesium hydroxide and are in harmonious proportion uniformly, obtain antibiotic property canalis radicis dentis
Filler.
Antibacterial experiment
Using nano-sized magnesium hydroxide in the suspension antisepsis test present invention to Escherichia coli（E coli）, staphylococcus aureus
（SAU）Anti- kill effect.
Prepare 0.8 mg/mL length 300 nm about acicular nanometer magnesium hydroxide physiological saline suspension, after sealing
0.103 MPa, high pressure steam sterilization 20 min under the conditions of 121 DEG C, standby.
Microbionation will be tested on plating medium, and after 37 DEG C of culture 24 h, take single bacterium colony to transfer in nutrient broth
In, cultivate 20 h at 37 DEG C.Bacterium solution concentration dilution will be tested to 10 using gradient dilution method-5.Take 1mL 10 respectively-5Reality
Test bacterium solution（Escherichia coli need anaerobic gram-negative bacteria representative, staphylococcus aureus to need anaerobic gram-positive for simultaneous for simultaneous
Bacterium represents）It is added dropwise in the normal saline solution containing nano-sized magnesium hydroxide, be placed on magnetic stirring apparatus and form it into suspension
（Simultaneously using the normal saline solution without nano-sized magnesium hydroxide as antibacterial experiment blank control group）.Extract 1mL sample respectively
Product drop in pushed away with spreading rod on sterilized plate count agar plate even, then by plate put in 37 DEG C of biochemical cultivation cases be inverted
Cultivate 24 h.Calculate sterilizing rate using the method for plate culture count.
Hemolytic test
According to GB/T 16886.4 2003. BiologicalEvaluationofMedicalDevice the 4th part:Interact to test with blood and select
Regulation and haemolysis pass judgment on require, hemolytic test is carried out to the antibiotic property tooth root canal filling material of the present invention.Wherein, part steps
It is listed below：
With physiological saline, red blood cell is made into 5% cell suspension, standby.Several test tubes are taken to be separately added into the red thin of 2.5ml 5%
Born of the same parents' suspension, adds 2.5ml sterile distilled water in positive control test tube, adds 2.5ml physiological saline, experiment in negative control test tube
The leaching liquor of the antibacterial tooth root canal filling material of 2.5ml is added in group test tube（Preparation can be found in GB/T 16886.4 2003）.
After incubating 1 hour in 37 DEG C, all examination liquid in pipe are taken out, centrifugation, supernatant is moved in cuvette, applies ultraviolet-visible
Light spectrophotometer mensuration absorbance (OD) value at 545nm wavelength, and calculate hemolysis rate.Every group of operation repetitive 3 is managed.Hemolysis rate
The computing formula of Z is：
Z(%) = (Dt- Dnc）/ (Dpc- Dnc) ×100%. （Formula 1）
In equation 1, DtFor sample absorbance value, DncFor the absorbance of negative control group, DpcSuction for positive controls
Shading value.Judgment criteria：During hemolysis rate ＜ 5%, can determine whether that this material does not have haemocylolysis.
Cytotoxicity test：
Prepare the leaching liquor of antibiotic property tooth root canal filling material using 10% calf serum and cell culture medium, specially：Weigh anti-
Bacterium property tooth root canal filling material l g, adds the DMEM culture medium l0 ml containing l0% calf serum after autoclaving.Vibration mixes
Afterwards in 5% CO2Place 3 days for 37 DEG C in cell culture incubator, then obtain supernatant through 3 000 r/min centrifugal treating, adopt
It is used for subsequent cell MTT test after filter EK.
Take the stable l cell L929 of growth, after 0.25% Trypsin Induced 3 min plus little containing l0%
The DMEM culture medium of cow's serum terminates digestion, so that attached cell is come off with sterilizing pasteur pipet piping and druming, is entered with blood cell counting plate
Row cell count, is made into 10 with DMEM culture medium on demand4/ ml cell suspension inoculation, in 96 well culture plates, every hole 100 μ l, is put
In 37 DEG C, 5%CO224 h are cultivated in incubator.The original fluid of in the hole and non-attached cell is discarded after cell attachment.Experiment
Group adds the leaching liquor 100 μ l of antibiotic property tooth root canal filling material, and blank control group adds the DMEM culture containing l0% calf serum
Base 100 μ l, positive controls add and contain 5% dimethyl sulfoxide (DMSO)（DMSO）The culture medium of DMEM containing serum 100 μ l.Every group sets 6 again
Culture is continued in hole.L, 3,5,7 day after dosing respectively, inhale and abandon original fluid, change fresh medium, finally simultaneously every
MTT is added in hole（5 mg / L）20 μ l, after continuing culture 4 h, reject extraction raffinate, every hole adds DMSO 150 μ l, micro oscillation 10
Min, surveys absorbance when wavelength is 570 nm on enzyme linked immunological instrument（OD）, record result.Do 3 Duplicate Samples（p<
0.05）.
Nano-sized magnesium hydroxide is through XRD test analysis and correlation computations and TEM electron diffraction analysis and grain morphology size
Test understands（See Fig. 1 to Fig. 3）：The nano-sized magnesium hydroxide of the present embodiment be in long 300 nm about needle-like, nano-sized magnesium hydroxide
Contact the sterilizing rate after 7 hours with Escherichia coli, staphylococcus aureus and all reach 100%（See Fig. 6 to Fig. 7）.
Detect hemolysis and the cell of the antibiotic property tooth root canal filling material that embodiment 1 is obtained using above-mentioned experimental technique
Toxicity, result is：No hemolytic, cytotoxicity is 0 grade, has good cell compatibility.
Embodiment 2
A kind of antibiotic property tooth root canal filling material, its preparation process is as follows：
One）The preparation of nano-sized magnesium hydroxide
Step one, the magnesium salt solution being 0. 01 mol/L with magnesium acetate compound concentration；
Step 2, under normal pressure and 80 DEG C of stirring conditions, adjusts above-mentioned magnesium salt solution pH value to 13 with NaOH, continues stirring
Reaction 7h, adds polyethylene glycol during the course of the reaction, and the addition of polyethylene glycol is 8 wt% of magnesium salts；
Step 3, reaction is cooled to room temperature after terminating, and then carries out separation of solid and liquid, solid is scrubbed, be drying to obtain a nanometer hydrogen-oxygen
Change magnesium powder body.
Two）The preparation of antibiotic property tooth root canal filling material
Weigh calcium hydroxide 8.8 g, magnesium chloride 0.6 g, dimethicone 0.6 g, nano-sized magnesium hydroxide 1 g respectively.With 0.1%
Aqueous Solutions of Polyethylene Glycol nano-sized magnesium hydroxide is made stable suspension.Then according to solid-to-liquid ratio 1 mg:0.5 ml, will
Calcium hydroxide, magnesium chloride, dimethicone are added in the suspension of nano-sized magnesium hydroxide and are in harmonious proportion uniformly, obtain antibiotic property root of the tooth
Pipe filler.
Nano-sized magnesium hydroxide is through XRD test analysis and correlation computations and TEM electron diffraction analysis and the test of grain morphology size
Understand：The nano magnesia of the present embodiment is corynebacterium, and major diameter is 100 nm, and minor axis is 10 nm（See Fig. 4）.Nanometer hydroxide
Magnesium is contacted the sterilizing rate after 7 hours and all reaches 100% with Escherichia coli, staphylococcus aureus.
Detect hemolysis and the cell of the antibiotic property tooth root canal filling material that embodiment 2 is obtained using above-mentioned experimental technique
Toxicity, result is：No hemolytic, cytotoxicity is 0 grade, has good cell compatibility.
Embodiment 3
A kind of antibiotic property tooth root canal filling material, its preparation process is as follows：
One）The preparation of nano-sized magnesium hydroxide
Step one, the magnesium salt solution being 0.6 mol/L with magnesium nitrate compound concentration；
Step 2, under normal pressure and 50 DEG C of stirring conditions, adjusts above-mentioned magnesium salt solution pH value to 12 with potassium hydroxide, continues stirring
React 6 h, add Sodium Polyacrylate during the course of the reaction, the addition of Sodium Polyacrylate is 7 wt% of magnesium salts；
Step 3, reaction is cooled to room temperature after terminating, and then suspension is carried out separation of solid and liquid, and solid is scrubbed, be drying to obtain
Magnesium Hydroxide Nano-particles.
Two）The preparation of antibiotic property tooth root canal filling material
Weigh calcium hydroxide 9 g, magnesium chloride 0.5 g, dimethicone 0.5 g, nano-sized magnesium hydroxide 2 g respectively.With concentration it is
The ethanol of 2% polyvinylpyrrolidone and water（Volume ratio 3:1）Nano-sized magnesium hydroxide is made stable suspension by mixed solution
Liquid.Then according to solid-to-liquid ratio 1 mg:0.6 ml, calcium hydroxide, magnesium chloride, dimethicone are added to nano-sized magnesium hydroxide
Suspension in be in harmonious proportion uniformly, obtain antibiotic property tooth root canal filling material.
Nano-sized magnesium hydroxide is through XRD test analysis and correlation computations and TEM electron diffraction analysis and grain morphology size
Test understands：The nano-sized magnesium hydroxide of the present embodiment is long 80 nm needle-likes.Nano-sized magnesium hydroxide and Escherichia coli, golden yellow Portugal
Sterilizing rate after grape coccus contacts 7 hours all reaches 100%.
Detect hemolysis and the cell of the antibiotic property tooth root canal filling material that embodiment 3 is obtained using above-mentioned experimental technique
Toxicity, result is：No hemolytic, cytotoxicity is 0 grade, has good cell compatibility.
Embodiment 4
A kind of antibiotic property tooth root canal filling material, its preparation process is as follows：
One）Nano-sized magnesium hydroxide, purchased from Beijing Deco Dao Jin Science and Technology Ltd..
Two）The preparation of antibiotic property tooth root canal filling material
Weigh calcium hydroxide 9 g, calcium chloride 0.4g, glycerine 0.6 g, nano-sized magnesium hydroxide 1.5 g respectively.It is 0.7 % with concentration
Sodium Polyacrylate and calgon（Weight compares 1:1）The aqueous solution nano-sized magnesium hydroxide is made stable suspension.So
Afterwards according to solid-to-liquid ratio 1 mg:0.4 ml, calcium hydroxide, calcium chloride, glycerine are added in the suspension of nano-sized magnesium hydroxide and adjust
With uniform, obtain antibiotic property tooth root canal filling material.
Nano-sized magnesium hydroxide is through XRD test analysis and correlation computations and TEM electron diffraction analysis and grain morphology size
Test understands：The nano magnesia of the present embodiment is hexagonal flake, a length of 20 nm about.Nano-sized magnesium hydroxide and Escherichia coli,
Sterilizing rate after staphylococcus aureus contacts 7 hours all reaches 100%.
Detect hemolysis and the cell of the antibiotic property tooth root canal filling material that embodiment 4 is obtained using above-mentioned experimental technique
Toxicity, result is：No hemolytic, MTT experiment shows that the cytotoxicity of material is 0 grade, has good cell compatibility.
Embodiment 5
A kind of antibiotic property tooth root canal filling material, its preparation process is as follows：
One）The preparation of nano-sized magnesium hydroxide
Step one, the magnesium salt solution being 1.5 mol/L with magnesium sulfate compound concentration；
Step 2, under normal pressure and 70 DEG C of stirring conditions, adjusts above-mentioned magnesium salt solution pH value to 11 with potassium hydroxide, continues to stir
Mix reaction 6h, add Tween 80 during the course of the reaction, the addition of Tween 80 is 2 wt% of magnesium salts；
Step 3, reaction is cooled to room temperature after terminating, and then suspension is carried out separation of solid and liquid, and solid is scrubbed, be drying to obtain
Magnesium Hydroxide Nano-particles.
Two）The preparation of antibiotic property tooth root canal filling material
Weigh calcium hydroxide 9 g, calcium chloride 0.5 g, glycerine 0.5 g, nano-sized magnesium hydroxide 2.5 g respectively.It is 1.5% with concentration
The polyacrylic acid aqueous solution nano-sized magnesium hydroxide is made stable suspension.Then according to solid-to-liquid ratio 1 mg:1 ml, by hydrogen
Calcium oxide, calcium chloride, glycerine are added in the suspension of nano-sized magnesium hydroxide and are in harmonious proportion uniformly, obtain antibiotic property root canal filling material
Material.
Nano-sized magnesium hydroxide is through XRD test analysis and correlation computations and TEM electron diffraction analysis and grain morphology size
Test understands：The nano-sized magnesium hydroxide of the present embodiment is corynebacterium, and major diameter is 300 nm, and minor axis is 20 nm.Nano-sized magnesium hydroxide
Contact the sterilizing rate after 7 hours with Escherichia coli, staphylococcus aureus and all reach 100%.
Detect hemolysis and the cell of the antibiotic property tooth root canal filling material that embodiment 5 is obtained using above-mentioned experimental technique
Toxicity, result is：No hemolytic, MTT experiment shows that the cytotoxicity of material is 0 grade, has good cell compatibility.
Embodiment 6
A kind of antibiotic property tooth root canal filling material, its preparation process is as follows：
One）The preparation of nano-sized magnesium hydroxide
Step one, the magnesium salt solution being 0.05 mol/L with magnesium acetate compound concentration；
Step 2, under normal pressure and 70 DEG C of stirring conditions, adjusts above-mentioned magnesium salt solution pH value to 11 with potassium hydroxide, continues stirring
Reaction 6h, adds polyethylene glycol during the course of the reaction, and the addition of polyethylene glycol is 6 wt% of magnesium salts；
Step 3, reaction is cooled to room temperature after terminating, and then suspension is carried out separation of solid and liquid, and solid is scrubbed, be drying to obtain
Magnesium Hydroxide Nano-particles.
Two）The preparation of antibiotic property tooth root canal filling material
Weigh calcium hydroxide 9 g, magnesium chloride 0.5 g, dimethicone 0.5 g, nano-sized magnesium hydroxide 3 g respectively.With concentration 1%
Sodium carboxymethyl cellulose solution nano-sized magnesium hydroxide is made stable suspension.Then according to solid-to-liquid ratio 1 mg: 0.3
Ml, calcium hydroxide, magnesium chloride, dimethicone is added in the suspension of nano-sized magnesium hydroxide and is in harmonious proportion uniformly, obtains antibacterial
Property tooth root canal filling material.
Nano-sized magnesium hydroxide is through XRD test analysis and correlation computations and TEM electron diffraction analysis and grain morphology size
Test understands：The nano-sized magnesium hydroxide of the present embodiment is hexagonal flake, long 80 nm about（See Fig. 5）.Nano-sized magnesium hydroxide with big
Sterilizing rate after enterobacteria, staphylococcus aureus contact 7 hours all reaches 100%.
Detect hemolysis and the cell of the antibiotic property tooth root canal filling material that embodiment 6 is obtained using above-mentioned experimental technique
Toxicity, result is：No hemolytic, MTT experiment shows that the cytotoxicity of material is 0 grade, has good cell compatibility.
Embodiment 7
A kind of antibiotic property tooth root canal filling material, its preparation process is as follows：
One）The preparation of nano-sized magnesium hydroxide
Step one, the magnesium salt solution being 0.6 mol/L with magnesium chloride compound concentration；
Step 2, under normal pressure and 70 DEG C of stirring conditions, adjusts above-mentioned magnesium salt solution pH value to 12 with potassium hydroxide, continues stirring
Reaction 6h, adds Sodium Polyacrylate during the course of the reaction, and the addition of Sodium Polyacrylate is 5 wt% of magnesium salts；
Step 3, reaction is cooled to room temperature after terminating, and then suspension is carried out separation of solid and liquid, and solid is scrubbed, be drying to obtain
Magnesium Hydroxide Nano-particles.
Two）The preparation of antibiotic property tooth root canal filling material
Weigh calcium hydroxide 9 g, magnesium chloride 0.5 g, glycerine 0.5 g, nano-sized magnesium hydroxide 1 g respectively.It is 0.5% with concentration
Calgon and polyethylene glycol（Weight compares 2:1）The aqueous solution nano-sized magnesium hydroxide is made stable suspension.Then press
According to solid-to-liquid ratio 1 mg:0.5 ml, calcium hydroxide, magnesium chloride, glycerine are added in the suspension of nano-sized magnesium hydroxide and are in harmonious proportion all
Even, obtain antibiotic property tooth root canal filling material.
Nano-sized magnesium hydroxide is through XRD test analysis and correlation computations and TEM electron diffraction analysis and grain morphology size
Test understands：The nano-sized magnesium hydroxide of the present embodiment is corynebacterium, and major diameter is 150 nm, and minor axis is 15 nm.Nano-sized magnesium hydroxide
Contact the sterilizing rate after 7 hours with Escherichia coli, staphylococcus aureus and all reach 100%.
Detect hemolysis and the cell of the antibiotic property tooth root canal filling material that embodiment 7 is obtained using above-mentioned experimental technique
Toxicity, result is：No hemolytic, MTT experiment shows that the cytotoxicity of material is 0 grade, has good cell compatibility.
Embodiment 8
A kind of antibiotic property tooth root canal filling material, its preparation process is as follows：
One）The preparation of nano-sized magnesium hydroxide
Step one, the magnesium salt solution being 0.2 mol/L with magnesium sulfate compound concentration；
Step 2, under normal pressure and 70 DEG C of stirring conditions, adjusts above-mentioned magnesium salt solution pH value to 13 with NaOH, continues to stir
Mix reaction 6h, add Tween 80 during the course of the reaction, the addition of Tween 80 is 1 wt% of magnesium salts；
Step 3, reaction is cooled to room temperature after terminating, and then suspension is carried out separation of solid and liquid, and solid is scrubbed, be drying to obtain
Magnesium Hydroxide Nano-particles.
Two）The preparation of antibiotic property tooth root canal filling material
Weigh calcium hydroxide 9 g, magnesium chloride 0.5 g, dimethicone 0.5 g, nano-sized magnesium hydroxide 3 g respectively.Dense with quality
Nano-sized magnesium hydroxide is made stable suspension by lauryl sodium sulfate (SDS) aqueous solution of degree 0.5%.Then according to solid-liquid
Than 1 mg:0.3 ml, calcium hydroxide, magnesium chloride, dimethicone are added in the suspension of nano-sized magnesium hydroxide and are in harmonious proportion all
Even, obtain antibiotic property tooth root canal filling material.
Nano-sized magnesium hydroxide is through XRD test analysis and correlation computations and TEM electron diffraction analysis and grain morphology size
Test understands：The nano-sized magnesium hydroxide of the present embodiment be about 80 nm about needle-like.Nano-sized magnesium hydroxide and Escherichia coli, gold
Sterilizing rate after staphylococcus aureus contact 7 hours all reaches 100%.
Detect hemolysis and the cell of the antibiotic property tooth root canal filling material that embodiment 8 is obtained using above-mentioned experimental technique
Toxicity, result is：No hemolytic, MTT experiment shows that the cytotoxicity of material is 0 grade, has good cell compatibility.
Embodiment 9
A kind of antibiotic property tooth root canal filling material, its preparation process is as follows：
One）The preparation of nano-sized magnesium hydroxide
Step one, the magnesium salt solution being 0. 6 mol/L with magnesium chloride compound concentration；
Step 2, under normal pressure and 80 DEG C of stirring conditions, adjusts above-mentioned magnesium salt solution pH value to 10 with potassium hydroxide, continues stirring
React 7 h, add polyethylene glycol during the course of the reaction, the addition of polyethylene glycol is 8 wt% of magnesium salts；
Step 3, reaction is cooled to room temperature after terminating, and then suspension is carried out separation of solid and liquid, and solid is scrubbed, be drying to obtain
Magnesium Hydroxide Nano-particles.
Two）The preparation of antibiotic property tooth root canal filling material
Weigh calcium hydroxide 9 g, calcium chloride 0.6 g, dimethicone 0.4g, nano-sized magnesium hydroxide 1.5 g respectively.Use 1.5 %
Polyethylene glycol and polyacrylic acid（Weight compares 1:4）Ethanol and water（Volume ratio 1:2）Mixed solution by nano-sized magnesium hydroxide
Make stable suspension.Then according to solid-to-liquid ratio 1 mg:0.5 ml, calcium hydroxide, calcium chloride, dimethicone are added
It is in harmonious proportion uniformly in the suspension of nano-sized magnesium hydroxide, obtain antibiotic property tooth root canal filling material.
Nano-sized magnesium hydroxide is through XRD test analysis and correlation computations and TEM electron diffraction analysis and the test of grain morphology size
Understand：The nano magnesia of the present embodiment is hexagonal flake, is about 100 nm.Nano-sized magnesium hydroxide and Escherichia coli, golden yellow
Sterilizing rate after staphylococcus contacts 7 hours all reaches 100%.
Detect hemolysis and the cell of the antibiotic property tooth root canal filling material that embodiment 9 is obtained using above-mentioned experimental technique
Toxicity, result is：No hemolytic, cytotoxicity is 0 grade, has good cell compatibility.
Claims (5)
1. a kind of antibiotic property tooth root canal filling material, including solid-liquid dispersing system and solid phase components it is characterised in that solid-liquid dispersing
The weight of the nano-sized magnesium hydroxide in system and solid phase components is than for 0.1 0.3：1.
2. antibiotic property tooth root canal filling material according to claim 1 is it is characterised in that described solid-liquid dispersing system refers to
Nano-sized magnesium hydroxide is dispersed in the suspension obtained in dispersant solution；Described dispersant solution is dispersant weight
The aqueous solution of concentration 0.1wt% 3wt% or the miscible solutions of water and ethanol；The weight concentration of described dispersant refers to dispersant
Weight is with respect to the percentage of magnesium hydroxide weight and liquid phase weight sum；Described dispersant is polyvinyl alcohol, polyethylene glycol, poly-
In acrylic acid, Sodium Polyacrylate, sodium carboxymethylcellulose, polyvinylpyrrolidone, lauryl sodium sulfate and calgon
One or more mixture.
3. antibiotic property tooth root canal filling material according to claim 1 is it is characterised in that described solid phase components include hydrogen-oxygen
Change calcium, calcium chloride or magnesium chloride, and dimethicone or glycerine；Wherein, each raw material weight percentage of described solid phase components
For：Calcium chloride or magnesium chloride 3% 6%, dimethicone or glycerine 3% 6%, balance of calcium hydroxide.
4. antibiotic property tooth root canal filling material according to claim 3 is it is characterised in that play the hydroxide of antibacterial action
Magnesium is nanoscale, and the specific surface area of nano-sized magnesium hydroxide is big, activity is high, and easy and root of the tooth pipe internal surface forms reliable and stable knot
Close, make filler and root of the tooth pipe internal surface tight, product is more firm, antibacterial, anticorrosive, durable.
5. the preparation method of antibiotic property tooth root canal filling material described in claim 1 is it is characterised in that by solid phase components and solid-liquid
Dispersion presses 1 mg：The ratio of 0.2 1.0ml is in harmonious proportion and uniformly obtains final product.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107982069A (en) * | 2017-12-04 | 2018-05-04 | 武汉大学 | A kind of canalis radicis dentis packing material and preparation method thereof |
| CN110934750A (en) * | 2019-12-27 | 2020-03-31 | 广州润虹医药科技股份有限公司 | Root canal filler for treating pulpitis or periapicalitis and preparation method thereof |
| CN113912822A (en) * | 2021-09-06 | 2022-01-11 | 上海抚佳精细化工有限公司 | Thermoplastic polyurethane elastomer and preparation method and application thereof |
| CN115460924A (en) * | 2021-05-06 | 2022-12-09 | 死海溴品有限公司 | Aqueous dispersions of magnesium compounds for preserving harvested products |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0464545B1 (en) * | 1990-06-26 | 1994-11-30 | Showa Yakuhin Kako Co., Ltd. | Paste composition and method for preparing the same |
| CN100998543A (en) * | 2007-01-15 | 2007-07-18 | 邓旭亮 | Oral cavity root canal sealant and its preparing method |
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- 2016-08-31 CN CN201610777530.6A patent/CN106377433B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0464545B1 (en) * | 1990-06-26 | 1994-11-30 | Showa Yakuhin Kako Co., Ltd. | Paste composition and method for preparing the same |
| CN100998543A (en) * | 2007-01-15 | 2007-07-18 | 邓旭亮 | Oral cavity root canal sealant and its preparing method |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107982069A (en) * | 2017-12-04 | 2018-05-04 | 武汉大学 | A kind of canalis radicis dentis packing material and preparation method thereof |
| CN110934750A (en) * | 2019-12-27 | 2020-03-31 | 广州润虹医药科技股份有限公司 | Root canal filler for treating pulpitis or periapicalitis and preparation method thereof |
| CN115460924A (en) * | 2021-05-06 | 2022-12-09 | 死海溴品有限公司 | Aqueous dispersions of magnesium compounds for preserving harvested products |
| CN113912822A (en) * | 2021-09-06 | 2022-01-11 | 上海抚佳精细化工有限公司 | Thermoplastic polyurethane elastomer and preparation method and application thereof |
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| CN106377433B (en) | 2019-04-05 |
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