CN106377433B - A kind of antibiotic property tooth root canal filling material and preparation method thereof - Google Patents
A kind of antibiotic property tooth root canal filling material and preparation method thereof Download PDFInfo
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Abstract
Present invention relates particularly to a kind of antibiotic property root canal filling material containing nano-sized magnesium hydroxide comprising the weight ratio of solid-liquid dispersing system and solid phase components, nano-sized magnesium hydroxide and solid phase components in solid-liquid dispersing system is 0.1-0.3:1.The solid-liquid dispersing system, which refers to, is dispersed in suspension obtained in dispersant solution for nano-sized magnesium hydroxide；The dispersant solution is the aqueous solution of dispersant weight concentration 0.1wt% -3wt% or the miscible solutions of water and ethyl alcohol；The dispersing agent is the mixture of one or more of polyvinyl alcohol, polyethylene glycol, polyacrylic acid, Sodium Polyacrylate, sodium carboxymethylcellulose, polyvinylpyrrolidone, lauryl sodium sulfate and calgon.Antibacterial experiment shows；Nano-sized magnesium hydroxide can reach 100% to the suppression rate of killing of gram-positive cocci and gram-Negative bacillus in 7h.Hemolytic test, Cytotoxic evaluation experiment show: the antibiotic property tooth root canal filling material biocompatibility containing nano-sized magnesium hydroxide is good.
Description
Technical field
The invention belongs to Medical oral cavity root canal filling material technical fields, 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 technique
Pulp vitality test is the common multiple odontopathy of clinical oral.Root canal treatment is pulpitis and periapical periodontitis treatment
Most efficient method.The purpose of root-canal filling is closely to close root canal for a long time with filler, prevents the hair of periapical lesion
Healing that is raw, promoting periapical lesion.However, tooth root canal filling material can not carry out the bacterium for remaining or leaking into canalis radicis dentis
The main reason for often root canal treatment being caused to fail, is killed in lasting suppression.With being constantly progressive for microbial identification research, people
Many canalis radicis dentis pathogenic bacteria, such as enterococcus faecalis, Candida albicans, Fusobacterium nucleatum are had found, as enterococcus faecalis is as a kind of
The simultaneous gram-positive cocci for needing anaerobism, recall rate may be up to 40% in root canal, and recall rate is high in the case of root canal re-treatment
Up to 24~77%.Moreover, this kind of canalis radicis dentis detection germ is also clinical common drug-fast bacteria, is also often cooperateed with other bacteriums
Effect leads to mixed infection in canalis radicis dentis.
Currently, domestic and international tooth root canal filling material, calcium hydroxide kind, epoxy resin, more can be divided by its main component
Polyformaldehyde class, zinc-oxide-eugenol class etc., other such as hydroxyapatite, calcium phosphate, glass ionomers are also continuous
Among research and application.Suppression of these tooth root canal filling materials to many drug-fast bacterias (such as enterococcus faecalis) in the infections of dental pulp of oral cavity
It is limited to kill ability.For example, the OH that the sterilization capability of calcium hydroxide depends on root canal filling paste to provide-Concentration, only
When pH value is maintained at a higher level, the calcium hydroxide in root canal 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 to the enterococcus faecalis being present in dentinal tubule without
Effect.Therefore dentin collagen can be adhered in tissue fluid environment by failing the enterococcus faecalis being killed, into dentinal tubule shape
At infecting again, root canal treatment is caused to fail.
Nano-sized magnesium hydroxide is a kind of new inorganic material with extensive use, can be used as Green Flammability agent, spent acidic
Object neutralizer, adsorbent, food preservative, fertilizer additive, heavy metal removing, flue gas desulfurization, soil treatment with simulated acid rain and pH tune
Agent etc. is saved, is always the important source material of gastric acid inhibitory drug in field of biomedicine.
In recent years studies have found that: nano-sized magnesium hydroxide have broad spectrum antibacterial performance, document (Dong CX, Cairney
J, Sun QHi. Investigation of Mg(OH)2 nanoparticles as an antibacterial agent.
J Nanopart Res, 2010,12:2101-2109) nano-sized magnesium hydroxide is provided to Escherichia coli, Staphylococcus aureus
Several different sections purpose bacteriums such as bacterium and azophenlyene Burkholderia all have the evidence of inhibitory or killing effect, and confirm this bactericidal property
With the OH in nano-sized magnesium hydroxide suspension-And Mg2+It is unrelated.It is generally believed that the antibacterial mechanisms of nano-sized magnesium hydroxide are normal with other
Inorganic nano antibacterial material (such as nano-ZnO, TiO seen2, Ag etc.) it is similar, that is, dissolve oxygen in the solution by single electron also
Original reaction generates peroxide O2-.Peroxide O2-There is chemical stability, thus the O of high concentration in alkaline environment2-It can
Exist on nano-sized magnesium hydroxide surface.This active oxygen easily reacts with the peptide bond in bacterial cell wall proteins, thus
Exine structure is destroyed, has the function that quick sterilization.Moreover, the high nano-sized magnesium hydroxide of interfacial energy can be with
It is adsorbed onto bacterium surface and forms absorbing complex, reach suppression by normal physiological metabolism process such as the breathings of interference bacterium and kill effect
Fruit.Therefore, nano-sized magnesium hydroxide can generate strong inhibitory or killing effect to all kinds of bacteriums often detected in the infections of dental pulp of oral cavity, and thin
Bacterium is not likely to produce drug resistance.
Magnesium is the macroelement of human body, and 60%~65% magnesium is present in bone, in tooth in normal human, is only second in bone
The content of calcium, phosphorus.Magnesium is osteocyte structure and function necessary element, to promoting bone growing and osteanagenesis, maintain bone and
The intensity and density of tooth play a significant role.Earlier the study found that content of magnesium is higher in tooth enamel, tooth is more not easy
Appearance decays tooth and saprodontia；Magnesium replenishers may prevent or periodontitis is delayed to develop.Nano-sized magnesium hydroxide can after being absorbed by the body
Generate Mg2+As magnesium replenishers.Therefore, the Novel toothed root canal filling material provided by the invention containing nano-sized magnesium hydroxide can not only
Play its unique anti-microbial property, moreover it is possible to help human body to increase and absorb magnesium elements, to become one kind applied to oral environment
New type filling material.
Summary of the invention
Present invention aims to overcome that prior art defect, provides a kind of root canal filling material that can persistently play antibiotic property
Material and preparation method thereof.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of antibiotic property tooth root canal filling material, including solid-liquid dispersing system and solid phase components, wherein solid-liquid dispersing system
The nano-sized magnesium hydroxide of the middle different morphologies for playing antibacterial action and the weight ratio of solid phase components are 0.1-0.3:1.
Nano-sized magnesium hydroxide is dispersed in obtained in dispersant solution specifically, the solid-liquid dispersing system refers to
Suspension；The dispersant solution is the aqueous solution or water of dispersant weight concentration 0.1wt% -3wt% and dissolving each other for ethyl alcohol
Solution；The weight concentration of the dispersing agent refers to percentage of the dispersant weight relative to the sum of magnesium hydroxide weight and liquid phase weight
Than (liquid phase refers to the solution that the solution of dispersing agent and water composition or dispersing agent and water and ethyl alcohol form)；The dispersing agent is poly-
Vinyl alcohol, polyethylene glycol, polyacrylic acid, Sodium Polyacrylate, sodium carboxymethylcellulose, polyvinylpyrrolidone, dodecyl sulphur
The mixture of one or more of sour sodium and calgon.The suspension is to be uniformly dispersed and what stability was high consolidates
Liquid dispersion.
Specifically, the solid phase components include calcium hydroxide, calcium chloride or magnesium chloride (being used as water-reducing agent) and dimethyl
Silicone oil or glycerol (playing lubricating action)；Wherein, each raw material weight percentage of the solid phase components are as follows: calcium chloride or magnesium chloride
3% -6%, dimethicone or glycerol 3% -6%, surplus are calcium hydroxide.
Above-mentioned antibiotic property tooth root canal filling material, the magnesium hydroxide for playing antibacterial action is nanoscale, nanometer hydroxide
Large specific surface area, the activity of magnesium are high, and easily 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, specifically: solid phase components and solid-liquid dispersing system are pressed 1
The ratio of mg:0.2-1.0ml reconciles uniformly to obtain the final product.Gained finished product is the preferable paste of mobility, direct use.
In antibiotic property tooth root canal filling material of the present invention, play antibacterial action is nano-sized magnesium hydroxide, can be direct
Ordinary commercial products are bought, can also be prepared according to conventional method in that art, or can also prepare as steps described below
It obtains:
Step 1, the magnesium salts for being 0.01-1.5 mol/L with magnesium chloride, magnesium nitrate, magnesium sulfate or magnesium acetate compound concentration
Solution；
It is molten to adjust above-mentioned magnesium salts with sodium hydroxide or potassium hydroxide under normal pressure and 50-80 DEG C of stirring condition for step 2
Liquid pH value continues to be stirred to react 5-7h to 10-13, and polyethylene glycol, Tween 80 or Sodium Polyacrylate are added during the reaction,
Its additional amount is the 1-8 wt% of magnesium salts；
Step 3 is cooled to room temperature after reaction, is then separated by solid-liquid separation suspension, and solid is washed, dry
Up to Magnesium Hydroxide Nano-particles.Gained nano-sized magnesium hydroxide be needle-shaped, corynebacterium or hexagonal flake, wherein corynebacterium major diameter be
100-300 nm, minor axis are 10-20 nm；Needle-shaped 80-300 nm of length；20-100 nm of hexagonal flake diameter.
Compared to the prior art, antibiotic property tooth root canal filling material provided by the invention has the advantages that
1) nano-sized magnesium hydroxide can be to a variety of anti-killing property caused a disease and drug-fast bacteria performance is persistently excellent in root canal treatment
Energy；
2) large specific surface area of nano-sized magnesium hydroxide, activity are high, and easily and root of the tooth pipe internal surface forms reliable and stable combination,
Make to 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 benefit
It fills agent to be absorbed by the body, have no toxic side effect.
According to the 4th part of GBT 16886.5-2003 BiologicalEvaluationofMedicalDevice: interacting with blood and test choosing
Select and the 5th part: the regulation of vitro cytotoxicity test carries out haemolysis to antibiotic property tooth root canal filling material of the invention respectively
Test and MTT cell toxicity test, the results showed that antibiotic property tooth root canal filling material of the present invention is without hemolytic, cell toxicant
Property be 0 grade, have good biocompatibility.
Detailed description of the invention
Fig. 1 is X-ray diffractogram (the German Brooks D8 that gained nano-sized magnesium hydroxide is prepared using the method for the present invention
Advance x-ray diffractometer, using Cu-k α as radiation source, the à of λ=1.54056)；As seen from Figure 1, all diffraction maximums can be with
Hexagonal crystal system magnesium hydroxide (space group P-3m1(164)) standard card JCPDS 00-044-1482 it is corresponding, and without other
The presence of crystal phase diffraction maximum illustrates that product is mainly hexagonal crystal system magnesium hydroxide；
Fig. 2 is TEM electronic diffraction photo (Hitachi's H-800 type that gained nano-sized magnesium hydroxide is prepared using the method for the present invention
Transmission electron microscope, England Oxford INCA energy disperse spectroscopy)；From the electronic diffraction photo of gained sample it is found that this is hexagonal
Structure.Further confirm that products obtained therefrom is magnesium hydrate hexagonal crystalline structure.
Fig. 3 be using the method for the present invention prepare gained nano-sized magnesium hydroxide TEM transmission electron microscope photo (80,000 times, Hitachi H-
800 type transmission electron microscopes, sample preparation are added dropwise on the copper mesh for bearing carbon film after using dehydrated alcohol ultrasonic disperse, do in air
It is dry), as seen from Figure 3, product is long 300nm or so, the preferable nano whiskers magnesium hydroxide (hexagonal crystal system) of dispersibility；
Fig. 4 be using the method for the present invention prepare gained nano-sized magnesium hydroxide TEM transmission electron microscope photo (80,000 times, Hitachi H-
800 type transmission electron microscopes, sample preparation are added dropwise on the copper mesh for bearing carbon film after using dehydrated alcohol ultrasonic disperse, do in air
It is dry), it can be seen from the figure that product is long 100nm or so, the preferable nano bar-shape magnesium hydroxide (hexagonal crystal system) of dispersibility；
Fig. 5 be using the method for the present invention prepare gained nano-sized magnesium hydroxide TEM transmission electron microscope photo (80,000 times, Hitachi H-
800 type transmission electron microscopes, sample preparation are added dropwise on the copper mesh for bearing carbon film after using dehydrated alcohol ultrasonic disperse, do in air
It is dry), it can be seen from the figure that product is 80nm or so, the preferable nano-hexagonal flake magnesium hydroxide (hexagonal crystal system) of dispersibility；
Fig. 6 is antibacterial effect of the present invention gained antibiotic property tooth root canal filling material to Escherichia coli, other gram-negatives
The antibacterial effect of property aerobic bacteria or anaerobic bacteria is similar；
Fig. 7 is antibacterial effect of the present invention gained antibiotic property tooth root canal filling material to staphylococcus aureus, other leather
Lan Shi positive aerobic bacteria or the antibacterial effect of anaerobic bacteria are similar.
Specific embodiment
Technical solution of the present invention is further discussed in detail with reference to embodiments, but protection scope of the present invention
It is not limited thereto.
Embodiment 1
A kind of antibiotic property tooth root canal filling material, preparation step are as follows:
One) preparation of nano-sized magnesium hydroxide
Step 1, the magnesium salt solution for being 0.8 mol/L with magnesium chloride compound concentration；
Step 2 adjusts above-mentioned magnesium salt solution pH value to 10 with sodium hydroxide, continues under normal pressure and 60 DEG C of stirring conditions
It is stirred to react 5h, Tween 80 is added during the reaction, the additional amount of Tween 80 is 1 wt% of magnesium salts；
Step 3 is cooled to room temperature after reaction, is then separated by solid-liquid separation gained suspension, solid is washed,
It is drying to obtain Magnesium Hydroxide Nano-particles.Gained nano-sized magnesium hydroxide is needle-shaped (Fig. 3) in the length of 300 nm.
Two) preparation of antibiotic property tooth root canal filling material
9.2 g of calcium hydroxide, 0.5 g of magnesium chloride, 0.3 g of dimethicone, 3 g of nano-sized magnesium hydroxide are weighed respectively.With
Nano-sized magnesium hydroxide is made stable suspension and (stirring such as can be used or ultrasonic method will by 0.2% polyvinyl alcohol water solution
Nano-sized magnesium hydroxide is dispersed in the aqueous solution of 0.2% polyvinyl alcohol and obtains).Then according to 1 mg:0.2 ml of solid-to-liquid ratio,
Calcium hydroxide, magnesium chloride, dimethicone are added in the suspension of nano-sized magnesium hydroxide and reconciled uniformly, antibiotic property tooth is obtained
Root canal filling material.
Antibacterial experiment
Using suspension antisepsis test the present invention in nano-sized magnesium hydroxide to Escherichia coli (E coli), golden yellow grape
The anti-of coccus (SAU) kills effect.
The physiological saline suspension for preparing the acicular nanometer magnesium hydroxide of 0.8 mg/mL long, 300 nm or so, after sealing
0.103 MPa, 20 min of high pressure steam sterilization under the conditions of 121 DEG C, it is spare.
Microbionation will be tested on plating medium, take single bacterium colony switching in nutrient broth after 37 DEG C of 24 h of culture
In, 20 h are cultivated at 37 DEG C.Bacterium solution concentration dilution will be tested to 10 using gradient dilution method-5.1mL 10 is taken respectively-5Reality
Test bacterium solution (Escherichia coli be it is simultaneous need anaerobic gram-negative bacteria to represent, staphylococcus aureus to be simultaneous needs anaerobic gram-positive
Bacterium represents) it is added dropwise in the normal saline solution containing nano-sized magnesium hydroxide, it is placed on magnetic stirring apparatus and forms it into suspension
(while using normal saline solution without nano-sized magnesium hydroxide as the blank control group of antibacterial experiment).1mL sample is extracted respectively
Product drop is pushed away on sterilized plate count agar plate with spreading rod even, then plate is put into 37 DEG C of biochemical cultivation cases and is inverted
Cultivate 24 h.Sterilizing rate is calculated using the method for plate culture count.
Hemolytic test
According to the 4th part of 16886.4-2003. BiologicalEvaluationofMedicalDevice of GB/T: interacting and test with blood
The regulation and haemolysis of selection, which are judged, to be required, and carries out hemolytic test to antibiotic property tooth root canal filling material of the invention.Wherein, part
Step is listed below:
Red blood cell is made into 5% cell suspension with physiological saline, it is spare.Several test tubes are taken to be separately added into 2.5ml's 5%
2.5ml sterile distilled water is added in positive control test tube, 2.5ml physiological saline is added in negative control test tube for red cell suspension,
The leaching liquor that the antibacterial tooth root canal filling material of 2.5ml is added in experimental group test tube (prepares and can be found in GB/T 16886.4-
2003).All examination liquid in pipe are taken out after being incubated 1 hour in 37 DEG C, centrifugation moves to supernatant in cuvette, using purple
Outside-visible spectrophotometer measures absorbance (OD) value at 545nm wavelength, and calculates hemolysis rate.Every group of operation repetitive 3
Pipe.The calculation formula of hemolysis rate Z are as follows:
Z(%) = (Dt- Dnc)/(Dpc- Dnc) × 100%. (formula 1)
In equation 1, DtFor sample absorbance value, DncFor the absorbance value of negative control group, DpcFor positive controls
Absorbance value.Judgment criteria: when hemolysis rate < 5%, it can determine whether that the material does not have haemocylolysis.
Cytotoxicity test:
The leaching liquor of antibiotic property tooth root canal filling material is prepared using 10% calf serum and cell culture medium, specifically: claim
Antibiotic property tooth root canal filling material l g is taken, the DMEM culture medium l0 ml of the calf serum containing l0% is added after high pressure sterilization.Oscillation
In 5% CO after mixing2It is placed 3 days for 37 DEG C in cell incubator, then obtains supernatant through 3 000 r/min centrifugal treatings,
It is tested using after filter filtration sterilization for subsequent cell MTT.
The l cell L929 for taking growth stable adds small containing l0% after 0.25% trypsin digestion, 3 min
The DMEM culture medium of cow's serum terminates digestion, so that attached cell is fallen off with sterilizing pasteur pipet piping and druming, with blood cell counting plate into
Row cell count is made into 10 with DMEM culture medium as needed4/ ml cell suspension inoculation is set in 96 well culture plates, every 100 μ l of hole
In 37 DEG C, 5%CO224 h are cultivated in incubator.The original fluid in hole and non-attached cell are discarded after cell is adherent.Experiment
The 100 μ l of leaching liquor of antibiotic property tooth root canal filling material is added in group, and the DMEM culture of the calf serum containing l0% is added in blank control group
The 100 μ l of the culture medium of DMEM containing serum for containing 5% dimethyl sulfoxide (DMSO) is added in 100 μ l of base, positive controls.Every group sets 6 again
Continue to cultivate in hole.L, 3,5,7 day after dosing respectively inhale and abandon original fluid, replace fresh medium, last simultaneously every
MTT(5 mg/L is added in hole) 20 μ l, continue after cultivating 4 h, 150 μ l of DMSO, micro oscillation 10 is added in reject extraction raffinate, every hole
Min, the absorbance value (OD) when surveying wavelength on enzyme linked immunological instrument and being 570 nm, records result.Do 3 Duplicate Samples (p<
0.05).
Nano-sized magnesium hydroxide is through XRD test analysis and relevant calculation and TEM electron diffraction analysis and grain morphology size
(see Fig. 1 to Fig. 3): the nano-sized magnesium hydroxide of the present embodiment is in needle-shaped, the nano-sized magnesium hydroxide of long 300 nm or so known to test
Sterilizing rate after contacting with Escherichia coli, staphylococcus aureus 7 hours reaches 100%(and sees Fig. 6 to Fig. 7).
Using the hemolysis and cell of antibiotic property tooth root canal filling material made from above-mentioned experimental method detection embodiment 1
Toxicity, as a result are as follows: without hemolytic, cytotoxicity is 0 grade, has good cell compatibility.
Embodiment 2
A kind of antibiotic property tooth root canal filling material, preparation step are as follows:
One) preparation of nano-sized magnesium hydroxide
Step 1, the magnesium salt solution for being 0. 01 mol/L with magnesium acetate compound concentration；
Step 2 adjusts above-mentioned magnesium salt solution pH value to 13 with sodium hydroxide, continues under normal pressure and 80 DEG C of stirring conditions
It is stirred to react 7h, polyethylene glycol is added during the reaction, the additional amount of polyethylene glycol is 8 wt% of magnesium salts；
Step 3 is cooled to room temperature after reaction, is then separated by solid-liquid separation, and solid is washed, is drying to obtain nanometer
Magnesium hydrate powder.
Two) preparation of antibiotic property tooth root canal filling material
8.8 g of calcium hydroxide, 0.6 g of magnesium chloride, 0.6 g of dimethicone, 1 g of nano-sized magnesium hydroxide are weighed respectively.With
Stable suspension is made in nano-sized magnesium hydroxide by 0.1% Aqueous Solutions of Polyethylene Glycol.Then according to 1 mg:0.5 of solid-to-liquid ratio
Calcium hydroxide, magnesium chloride, dimethicone are added in the suspension of nano-sized magnesium hydroxide and reconcile uniformly, obtain antibacterial by ml
Property tooth root canal filling material.
Nano-sized magnesium hydroxide is through XRD test analysis and relevant calculation and TEM electron diffraction analysis and grain morphology size
Known to test: the nano magnesia of the present embodiment is corynebacterium, and major diameter is 100 nm, and minor axis is that 10 nm(are shown in Fig. 4).Nanometer hydrogen
Sterilizing rate after magnesia contacts 7 hours with Escherichia coli, staphylococcus aureus reaches 100%.
Using the hemolysis and cell of antibiotic property tooth root canal filling material made from above-mentioned experimental method detection embodiment 2
Toxicity, as a result are as follows: without hemolytic, cytotoxicity is 0 grade, has good cell compatibility.
Embodiment 3
A kind of antibiotic property tooth root canal filling material, preparation step are as follows:
One) preparation of nano-sized magnesium hydroxide
Step 1, the magnesium salt solution for being 0.6 mol/L with magnesium nitrate compound concentration；
Step 2 adjusts above-mentioned magnesium salt solution pH value to 12 with potassium hydroxide, continues under normal pressure and 50 DEG C of stirring conditions
6 h are stirred to react, Sodium Polyacrylate is added during the reaction, the additional amount of Sodium Polyacrylate is 7 wt% of magnesium salts；
Step 3 is cooled to room temperature after reaction, is then separated by solid-liquid separation suspension, and solid is washed, dry
Up to Magnesium Hydroxide Nano-particles.
Two) preparation of antibiotic property tooth root canal filling material
9 g of calcium hydroxide, 0.5 g of magnesium chloride, 0.5 g of dimethicone, 2 g of nano-sized magnesium hydroxide are weighed respectively.With dense
For the ethyl alcohol of 2% polyvinylpyrrolidone stable hang is made with water (volume ratio 3:1) mixed solution in nano-sized magnesium hydroxide by degree
Supernatant liquid.Then according to 1 mg:0.6 ml of solid-to-liquid ratio, calcium hydroxide, magnesium chloride, dimethicone are added to a nanometer hydroxide
It is reconciled uniformly in the suspension of magnesium, obtains antibiotic property tooth root canal filling material.
Nano-sized magnesium hydroxide is through XRD test analysis and relevant calculation and TEM electron diffraction analysis and grain morphology size
Known to test: the nano-sized magnesium hydroxide of the present embodiment is that long 80 nm are needle-shaped.Nano-sized magnesium hydroxide and Escherichia coli, golden yellow Portugal
Sterilizing rate after grape coccus contacts 7 hours reaches 100%.
Using the hemolysis and cell of antibiotic property tooth root canal filling material made from above-mentioned experimental method detection embodiment 3
Toxicity, as a result are as follows: without hemolytic, cytotoxicity is 0 grade, has good cell compatibility.
Embodiment 4
A kind of antibiotic property tooth root canal filling material, preparation step are as follows:
One) nano-sized magnesium hydroxide is purchased from Beijing Deco Dao Jin Science and Technology Ltd..
Two) preparation of antibiotic property tooth root canal filling material
9 g of calcium hydroxide, calcium chloride 0.4g, 0.6 g of glycerol, 1.5 g of nano-sized magnesium hydroxide are weighed respectively.It is with concentration
Stable suspension is made in nano-sized magnesium hydroxide by the Sodium Polyacrylate of 0.7 % and the aqueous solution of calgon (weight ratio 1:1)
Liquid.Then according to 1 mg:0.4 ml of solid-to-liquid ratio, calcium hydroxide, calcium chloride, glycerol are added to the suspension of nano-sized magnesium hydroxide
It is reconciled uniformly in liquid, obtains antibiotic property tooth root canal filling material.
Nano-sized magnesium hydroxide is through XRD test analysis and relevant calculation and TEM electron diffraction analysis and grain morphology size
Known to test: the nano magnesia of the present embodiment is hexagonal flake, a length of 20 nm or so.Nano-sized magnesium hydroxide and Escherichia coli,
Sterilizing rate after staphylococcus aureus contacts 7 hours reaches 100%.
Using the hemolysis and cell of antibiotic property tooth root canal filling material made from above-mentioned experimental method detection embodiment 4
Toxicity, as a result are as follows: without 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, preparation step are as follows:
One) preparation of nano-sized magnesium hydroxide
Step 1, the magnesium salt solution for being 1.5 mol/L with magnesium sulfate compound concentration；
Step 2 adjusts above-mentioned magnesium salt solution pH value to 11 with potassium hydroxide under normal pressure and 70 DEG C of stirring conditions, after
It is continuous to be stirred to react 6h, Tween 80 is added during the reaction, the additional amount of Tween 80 is 2 wt% of magnesium salts；
Step 3 is cooled to room temperature after reaction, is then separated by solid-liquid separation suspension, and solid is washed, dry
Up to Magnesium Hydroxide Nano-particles.
Two) preparation of antibiotic property tooth root canal filling material
9 g of calcium hydroxide, 0.5 g of calcium chloride, 0.5 g of glycerol, 2.5 g of nano-sized magnesium hydroxide are weighed respectively.It is with concentration
Stable suspension is made in nano-sized magnesium hydroxide by 1.5% polyacrylic acid aqueous solution.Then according to 1 mg:1 ml of solid-to-liquid ratio,
Calcium hydroxide, calcium chloride, glycerol are added in the suspension of nano-sized magnesium hydroxide and reconciled uniformly, antibiotic property canalis radicis dentis is obtained and fills
Filling chock material.
Nano-sized magnesium hydroxide is through XRD test analysis and relevant calculation and TEM electron diffraction analysis and grain morphology size
Known to test: 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
Sterilizing rate after contacting with Escherichia coli, staphylococcus aureus 7 hours reaches 100%.
Using the hemolysis and cell of antibiotic property tooth root canal filling material made from above-mentioned experimental method detection embodiment 5
Toxicity, as a result are as follows: without 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, preparation step are as follows:
One) preparation of nano-sized magnesium hydroxide
Step 1, the magnesium salt solution for being 0.05 mol/L with magnesium acetate compound concentration；
Step 2 adjusts above-mentioned magnesium salt solution pH value to 11 with potassium hydroxide, continues under normal pressure and 70 DEG C of stirring conditions
It is stirred to react 6h, polyethylene glycol is added during the reaction, the additional amount of polyethylene glycol is 6 wt% of magnesium salts；
Step 3 is cooled to room temperature after reaction, is then separated by solid-liquid separation suspension, and solid is washed, dry
Up to Magnesium Hydroxide Nano-particles.
Two) preparation of antibiotic property tooth root canal filling material
9 g of calcium hydroxide, 0.5 g of magnesium chloride, 0.5 g of dimethicone, 3 g of nano-sized magnesium hydroxide are weighed respectively.With dense
Stable suspension is made in nano-sized magnesium hydroxide by the sodium carboxymethyl cellulose solution of degree 1%.Then according to 1 mg of solid-to-liquid ratio:
Calcium hydroxide, magnesium chloride, dimethicone are added in the suspension of nano-sized magnesium hydroxide and reconcile uniformly, obtain by 0.3 ml
Antibiotic property tooth root canal filling material.
Nano-sized magnesium hydroxide is through XRD test analysis and relevant calculation and TEM electron diffraction analysis and grain morphology size
Known to test: the nano-sized magnesium hydroxide of the present embodiment is hexagonal flake, long 80 nm or so (see figure 5).Nano-sized magnesium hydroxide and big
Enterobacteria, the sterilizing rate after staphylococcus aureus contact 7 hours reach 100%.
Using the hemolysis and cell of antibiotic property tooth root canal filling material made from above-mentioned experimental method detection embodiment 6
Toxicity, as a result are as follows: without 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, preparation step are as follows:
One) preparation of nano-sized magnesium hydroxide
Step 1, the magnesium salt solution for being 0.6 mol/L with magnesium chloride compound concentration；
Step 2 adjusts above-mentioned magnesium salt solution pH value to 12 with potassium hydroxide, continues under normal pressure and 70 DEG C of stirring conditions
It is stirred to react 6h, Sodium Polyacrylate is added during the reaction, the additional amount of Sodium Polyacrylate is 5 wt% of magnesium salts；
Step 3 is cooled to room temperature after reaction, is then separated by solid-liquid separation suspension, and solid is washed, dry
Up to Magnesium Hydroxide Nano-particles.
Two) preparation of antibiotic property tooth root canal filling material
9 g of calcium hydroxide, 0.5 g of magnesium chloride, 0.5 g of glycerol, 1 g of nano-sized magnesium hydroxide are weighed respectively.It is with concentration
Stable suspension is made in nano-sized magnesium hydroxide by 0.5% calgon and the aqueous solution of polyethylene glycol (weight ratio 2:1).
Then according to 1 mg:0.5 ml of solid-to-liquid ratio, calcium hydroxide, magnesium chloride, glycerol are added in the suspension of nano-sized magnesium hydroxide
It reconciles uniformly, obtains antibiotic property tooth root canal filling material.
Nano-sized magnesium hydroxide is through XRD test analysis and relevant calculation and TEM electron diffraction analysis and grain morphology size
Known to test: 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
Sterilizing rate after contacting with Escherichia coli, staphylococcus aureus 7 hours reaches 100%.
Using the hemolysis and cell of antibiotic property tooth root canal filling material made from above-mentioned experimental method detection embodiment 7
Toxicity, as a result are as follows: without 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, preparation step are as follows:
One) preparation of nano-sized magnesium hydroxide
Step 1, the magnesium salt solution for being 0.2 mol/L with magnesium sulfate compound concentration；
Step 2 adjusts above-mentioned magnesium salt solution pH value to 13 with sodium hydroxide under normal pressure and 70 DEG C of stirring conditions, after
It is continuous to be stirred to react 6h, Tween 80 is added during the reaction, the additional amount of Tween 80 is 1 wt% of magnesium salts；
Step 3 is cooled to room temperature after reaction, is then separated by solid-liquid separation suspension, and solid is washed, dry
Up to Magnesium Hydroxide Nano-particles.
Two) preparation of antibiotic property tooth root canal filling material
9 g of calcium hydroxide, 0.5 g of magnesium chloride, 0.5 g of dimethicone, 3 g of nano-sized magnesium hydroxide are weighed respectively.Use matter
Stable suspension is made in nano-sized magnesium hydroxide by lauryl sodium sulfate (SDS) aqueous solution of amount concentration 0.5%.Then according to
1 mg:0.3 ml of solid-to-liquid ratio, calcium hydroxide, magnesium chloride, dimethicone are added in the suspension of nano-sized magnesium hydroxide and are adjusted
With it is uniform, obtain antibiotic property tooth root canal filling material.
Nano-sized magnesium hydroxide is through XRD test analysis and relevant calculation and TEM electron diffraction analysis and grain morphology size
Known to test: the nano-sized magnesium hydroxide of the present embodiment is needle-shaped to be about 80 nm or so.Nano-sized magnesium hydroxide and Escherichia coli, gold
Sterilizing rate after staphylococcus aureus contacts 7 hours reaches 100%.
Using the hemolysis and cell of antibiotic property tooth root canal filling material made from above-mentioned experimental method detection embodiment 8
Toxicity, as a result are as follows: without 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, preparation step are as follows:
One) preparation of nano-sized magnesium hydroxide
Step 1, the magnesium salt solution for being 0. 6 mol/L with magnesium chloride compound concentration；
Step 2 adjusts above-mentioned magnesium salt solution pH value to 10 with potassium hydroxide, continues under normal pressure and 80 DEG C of stirring conditions
7 h are stirred to react, polyethylene glycol is added during the reaction, the additional amount of polyethylene glycol is 8 wt% of magnesium salts；
Step 3 is cooled to room temperature after reaction, is then separated by solid-liquid separation suspension, and solid is washed, dry
Up to Magnesium Hydroxide Nano-particles.
Two) preparation of antibiotic property tooth root canal filling material
9 g of calcium hydroxide, calcium chloride 0.6 g, dimethicone 0.4g, 1.5 g of nano-sized magnesium hydroxide are weighed respectively.With
The mixed solution of the ethyl alcohol and water (volume ratio 1:2) of the polyethylene glycol of 1.5 % and polyacrylic acid (weight ratio 1:4) is by nanometer hydrogen-oxygen
Change magnesium and stable suspension is made.Then according to 1 mg:0.5 ml of solid-to-liquid ratio, by calcium hydroxide, calcium chloride, dimethicone
It is added in the suspension of nano-sized magnesium hydroxide and reconciles uniformly, obtain antibiotic property tooth root canal filling material.
Nano-sized magnesium hydroxide is through XRD test analysis and relevant calculation and TEM electron diffraction analysis and grain morphology size
Known to test: the nano magnesia of the present embodiment is hexagonal flake, is about 100 nm.Nano-sized magnesium hydroxide and Escherichia coli, gold
Sterilizing rate after staphylococcus aureus contacts 7 hours reaches 100%.
Using the hemolysis and cell of antibiotic property tooth root canal filling material made from above-mentioned experimental method detection embodiment 9
Toxicity, as a result are as follows: without hemolytic, cytotoxicity is 0 grade, has good cell compatibility.
Claims (3)
1. a kind of antibiotic property tooth root canal filling material, including solid-liquid dispersing system and solid phase components, which is characterized in that solid-liquid dispersing
The weight ratio of nano-sized magnesium hydroxide and solid phase components in system is 0.1-0.3:1；
The solid-liquid dispersing system, which refers to, is dispersed in suspension obtained in dispersant solution for nano-sized magnesium hydroxide；Institute
State the miscible solutions of aqueous solution or water and ethyl alcohol that dispersant solution is dispersant weight concentration 0.1wt% -3wt%；Described point
The weight concentration of powder refers to percentage of the dispersant weight relative to the sum of magnesium hydroxide weight and liquid phase weight；The dispersion
Agent is polyvinyl alcohol, polyethylene glycol, polyacrylic acid, Sodium Polyacrylate, sodium carboxymethylcellulose, polyvinylpyrrolidone, 12
The mixture of one or more of sodium alkyl sulfate and calgon.
2. antibiotic property tooth root canal filling material according to claim 1, which is characterized in that the solid phase components include hydrogen-oxygen
Change calcium, calcium chloride or magnesium chloride and dimethicone or glycerol；Wherein, each raw material weight percentage of the solid phase components
Are as follows: calcium chloride or magnesium chloride 3% -6%, dimethicone or glycerol 3% -6%, surplus are calcium hydroxide.
3. the preparation method of antibiotic property tooth root canal filling material described in claim 1, which is characterized in that by solid phase components and solid-liquid
Dispersion reconciles uniformly in the ratio of 1 mg:0.2-1.0ml to obtain the final product.
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