CN100448424C - Nano zinc oxide clove oil root canal filling material and its preparing method - Google Patents
Nano zinc oxide clove oil root canal filling material and its preparing method Download PDFInfo
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- CN100448424C CN100448424C CNB2006100896325A CN200610089632A CN100448424C CN 100448424 C CN100448424 C CN 100448424C CN B2006100896325 A CNB2006100896325 A CN B2006100896325A CN 200610089632 A CN200610089632 A CN 200610089632A CN 100448424 C CN100448424 C CN 100448424C
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Abstract
The present invention relates to oral root canal treating material, and is especially a kind of root canal filling material of nanometer zinc oxide and clove oil and its preparation process. The root canal filling material consists of powder in 60-75 wt% and clove oil in 25-40 wt%, and the powder consists of inorganic nanometer ZnO of 10-280 nm size 46-90 wt%, inorganic nanometer ZrO2 of 10- 600 nm size 5-40 wt%, inorganic nanometer hydro xyapatite of 80-100 nm size not more than 10 wt%, inorganic nanometer silver carrying antibiotic powder of 90-150 nm size not more than 10 wt%, thymol 2-10 wt%, anaerobe resisting medicine not more than 10 wt%, antibiotic not more than 25 wt%, and steroid glucocorticoid <1 wt%. Compared with available technology, the present invention has the advantages of high X-ray resistance, high flowability, high biocompatibility, low dissolubility and low cost.
Description
Technical field
The invention belongs to material for endodontic treatment field, medical oral cavity, particularly a kind of nano zinc oxide clove oil root canal filling material and preparation method thereof.
Background technology
The bar passage is all arranged in the root of the tooth of our every tooth, have dental nerve, blood vessel etc. to pass through therebetween, be referred to as the root pipe.Root canal is exactly the operation of carrying out in this passage, generally include root canal preparation, root canal disinfection and root pipe and fill three steps: at first thoroughly remove clean with apparatus the dental nerve of inflammation, necrosis and a large amount of antibacterial and corrupt substances, put canal filling material behind the poison, the root pipe is by close packing, and playing protects from infection spreads.The method plays as far as possible to preserve to be suffered from tooth and avoids pulling out, and subdue focal infection, rebuild effects such as suffering from tooth health, be to treat not recoverability pulpitis, the effective ways of pulp necrosis and various periapical periodontitiss at present.
Therefore, selected root canal filling material will have lasting disinfective action, can promote the healing of sharp all pathological changes, and the filler of zone of preference sterilization composition seems particularly important.For canal filling material, require its tangible analyte that do not have in addition, solubility is not more than 3% of mass fraction; When method was according to the rules tested, the diameter of each dish was 20-33mm; The thick dish of 2mm is not less than the thick aluminium sheet of 3mm to the attenuation of X ray.
The root canal filling material of present domestic use is that common zinc oxide, iodoform and medicine and simple mediation of Oleum Caryophylli are made basically, external product cortisomol root canal filling material is external at present a kind of root canal filling material of popularizing, mainly contain prednisolone acetate, paraformaldehyde, zinc oxide, lead oxide and excipient, compare with domestic oxide powder and zinc eugenol paste commonly used, increased prednisolone acetate and excipient composition.With external product cortisomol root canal filling material as experimental group, domestic root canal filling material is organized in contrast, there are some researches show: (" clinical and experimental medicine " magazine in March, 2004,3 the 1st phases of volume, the 19-20 page or leaf, author: Chang Shimin, Han Peiyan, Xing Rudong) experimental group treatment back 31.4% is suffered from tooth and pain do not occurred, and accumulative total 80.0% is suffered from pain relieving fully in the tooth 2 days; Accumulative total 97.1% is suffered from pain relieving fully in the tooth 4 days, and 12.5% suffers from tooth and pain do not occur after the treatment of control group, and accumulative total 42.5% is suffered from pain relieving fully in the tooth 2 days, and accumulative total 80.0% is suffered from pain relieving fully in the tooth 4 days.
Though and the external more domestic ZOE paste of import root canal filling material effect is better, mostly costs an arm and a leg.In addition, main sterilization component is the sterilization antibacterials in the existing root canal filling material, and all there is certain side effect in these medicines to human body.
Summary of the invention
The object of the present invention is to provide a kind of have penetrating property of the resistance of X ray preferably, flowability, biocompatibility, dissolubility is low, antimicrobial efficiency is high, cheap nano zinc oxide clove oil root canal filling material and preparation method.
According to above-mentioned purpose, technical scheme of the present invention is: mainly be that nano inorganic material is applied in this novel root canal filling material, substitute existing ingredient, improving its therapeutic efficiency, and reduce cost with nano inorganic material, specific as follows:
The chemical composition of this filler is that powder accounts for 60%～75%, and Oleum Caryophylli accounts for 25%～40%;
Wherein: the chemical composition of powder (weight %) is: inorganic constituents nano-ZnO 46%～90%, particle diameter are 10～280nm; Inorganic constituents nanometer ZrO
25%～40%, its particle diameter is 10～600nm; Inorganic constituents nanometer hydroxyapatite≤10%, particle diameter are 80～100nm; Its particle diameter is 90～150nm; Inorganic constituents nano silver-supported antibacterial powder≤10%, its particle diameter are 90～150nm; Thymol 2%～10%, anti-anaerobic agent≤10%, antibiotic≤25%, steroid glucocorticoid＜1%.
The nano-ZnO granule that is adopted is that the bar-shaped or flower shapes of sphere, ellipse, bar-shaped needle-like, four angular pin shapes, four jiaos are one or more.
Inorganic constituents nanometer ZrO
2For through Y
2O
3Stable cubic phase ZrO
2
The inorganic constituents nano-hydroapatite particles be shaped as needle-like, long telomere directly is 1～20nm, short telomere directly is 1～5nm.
The main component of inorganic constituents nano silver-supported antibacterial powder is that nanometer hydroxyapatite carries nano titanium oxide silver.
Anti-anaerobic agent is any in metronidazole, tinidazole and the ornidazole.
Antibiotic is any in erythromycin series, Tetracyclines and the cephalosporins medicine.
The steroid glucocorticoid is any in dexamethasone, prednisolone, prednisolone acetate, hydrocortisone and the cortisone acetate.
The method for preparing above-mentioned nano zinc oxide clove oil root canal filling material comprises following concrete steps:
At first above-mentioned powder is constituted by proportioning and adopt double spiral agitator with its mix homogeneously, wherein double spiral agitator mixing rotating speed is 10～180 rev/mins, and incorporation time is 5～60min; And then powder and Oleum Caryophylli concocted in 1: 1～3: 1 ratios, the temperature that is in harmonious proportion is 23 ℃ ± 1 ℃, relative humidity is 45%～55% during mediation.
According to above-mentioned purpose and technical scheme, the foundation of chemical composition of the present invention is:
Nano-ZnO granule of the present invention is sphere, ellipse, bar-shaped needle-like, four angular pin shapes, four jiaos of bar-shaped or flower shapes, and its particle diameter is 10～280nm.Nano zine oxide is because particle diameter is little, and surface atom quantity substantially exceeds traditional particle, and surface atom has very high energy owing to lacking contiguous coordination atom, so can strengthen the affinity of zinc oxide, improves antimicrobial efficiency.Nano zine oxide utilizes the active oxygen species of its generation to cause microbial damage or zinc ion stripping and the intravital albumen of microorganism or nucleic acid functional group to react and realizes antibiotic.There are some researches show that in 5 minutes, nano zine oxide is 98.86% to the sterilizing rate of golden yellow staphylococcus, escherichia coli are 99.93%, apparently higher than common zinc oxide.
Nanometer ZrO of the present invention
2For through Y
2O
3Stable cubic phase ZrO
2, its particle diameter is 10～600nm.Usually being applied in resistance in traditional root canal filling material, to penetrate material be barium sulfate.The nano zircite particle size is small, is stable oxide very, has acidproof, alkaline-resisting, corrosion-resistant, resistance and high temperature resistance property, is a kind of new material that is applied to oral environment.The present invention with nano zircite as an alternative the resistance of barium sulfate penetrate material, with the situation of barium sulfate same amount under, can reach effect above the resistance X ray of barium sulfate, improved the biocompatibility of material largely.
Nano-hydroapatite particles of the present invention is a needle-like, and its particle diameter is 80～100nm.Hydroxyapatite has excellent biological compatibility, and the physiology substrate that is fit to new bone apposition can be provided, and induces inostosis, stimulates the surrounding bone tissue regeneration, and the cementum deposition, and the sealing apical foramen of tooth quickens the diseased region healing, and root fills and can not be organized absorption.Nanometer hydroxyapatite is the hydroxyapatite of nanorize, compares with conventional hydroxyapatite, and nanometer hydroxyapatite toughness and physical and mechanical property all strengthen greatly, and biocompatibility and biological activity are good than the former.And nanometer hydroxyapatite (HA) all has inhibitory action to the growth and breeding of Streptococcus mutans, Streptococcus sanguis, actinomyces viscosus, and Streptococcus sobrinus, porphyromonas gingivalis are had the growth of promotion effect; Yttrium/HA the nano microcrystalline that contains yttrium 1mol% and 5mol% all has inhibitory action to Streptococcus mutans, Streptococcus sobrinus, Streptococcus sanguis, actinomyces viscosus, and to porphyromonas gingivalis unrestraint effect.
Its main component of nano silver-supported antibacterial powder of the present invention is that nanometer hydroxyapatite carries nano titanium oxide silver, and its particle diameter is 90～150nm.Visible light and the ultraviolet light that this antibacterial had both had nano titanium oxide itself sterilizes down, antiviral, bacterium for degrading, organic effect, and having is not again having the nanometer hydroxyapatite under the light source to carry potent antibiotic, the kill virus effect of nano titanium oxide silver.This nano antibacterial agent main component is a nano titanium oxide nanometer silver chelating body, has that antibacterial ability is strong, scope is wide, the time long grain is thin evenly, heat resisting temperature is high, will never change colour, use easily, slow characteristics such as execute.Effect significantly strengthens than antibiotics to gram-bacteria owing to novel inorganic composition nano silver-supported antibacterial powder, and has good biocompatibility, can play the effect that substitutes antibiotic medicine in novel root canal filling material.
The antibiotic that the present invention is used for the root canal filling material treatment mainly contains erythromycin series, Tetracyclines and cephalosporins medicine, and they mainly play certain inhibitory action to gram-bacteria, but anaphylaxis is the topmost side effect of this class medicine.
The anti-anaerobic agent that the present invention is used for root canal filling material is mainly metronidazole, tinidazole and ornidazole.Because of metronidazole has certain toxicity and potential carcinogenecity, tinidazole becomes the antianaerobic-microbacterial drug commonly used that substitutes metronidazole, but also there is rare toxic and side effects in tinidazole.The pretty clear effect that waits the people to study ornidazole treatment oral anaerobe infection disease of fourth, its total effective rate is 83.3%, tinidazole only is 73.3%.Though still there is certain side reaction, its effect significantly strengthens.
Root-canal filling of the present invention comprises dexamethasone, prednisolone, prednisolone acetate, hydrocortisone and cortisone acetate with the steroid glucocorticoid of introducing in the powder.In root canal, glucocorticoids is for infecting and non-infectious inflammation person has powerful antiinflammatory action, can alleviate the oozing out of periapical tissue, edema, leukocyte infiltration in early days and engulf reaction in inflammation, thereby alleviate swelling and pain symptom.It is little to add the glucocorticoids consumption in filler, local valid density height, the side effect of avoiding whole body to bring with hormone medicine.
The filler that the present invention compared with prior art prepares has penetrating property of the resistance of X ray preferably, flowability, biocompatibility, dissolubility is low, antimicrobial efficiency is high, cheap advantage.Above-mentioned advantage is specific as follows:
1, in 5 minutes, nano zine oxide is 98.86% to the sterilizing rate of golden yellow staphylococcus, and escherichia coli are 99.93%, apparently higher than common zinc oxide.
2, the present invention with nano zircite as an alternative the resistance of barium sulfate penetrate material, with the situation of barium sulfate same amount under, can reach effect above the resistance X ray of barium sulfate, improved the biocompatibility of material largely.The thick dish of the 2mm that is made by the root canal filling material that adds nano zircite is better than the thick aluminum plate of 6mm to the attenuation of X ray;
3, effect significantly strengthens than antibiotics to gram-bacteria owing to inorganic constituents nano silver-supported antibacterial powder, and has good biocompatibility, can play the effect that substitutes antibiotic medicine in novel root canal filling material.
4, the present invention's antibiotic of being used for root canal filling material treatment mainly contains erythromycin series, Tetracyclines and cephalosporins medicine, and they mainly play certain inhibitory action to gram-bacteria, but anaphylaxis is the topmost side effect of this class medicine.
5, the effect of ornidazole treatment oral anaerobe infection disease, its total effective rate is 83.3%, tinidazole only is 73.3%.Though still there is certain side reaction, its effect significantly strengthens.
6, adding glucocorticoids consumption is little in filler, local valid density height, the side effect of avoiding whole body to bring with hormone medicine.
The specific embodiment
When the present invention adopted double spiral agitator to mix by the raw mix that proportioning constitutes, its rotating speed was 30 rev/mins, the about 20min of incorporation time.The root canal filling material that the present invention relates to is to be 23 ℃ ± 1 ℃ in temperature, and relative humidity is 45%～55%, and powder and Oleum Caryophylli are made in ratio blending in 1: 1～3: 1.
Embodiment 1:
Zinc oxide and barium sulfate are evenly made powder according to certain mixed, itself and the Oleum Caryophylli ratio with 2: 1 is in harmonious proportion, it is as shown in table 1 below to record its flow diameter data.
The flowability of root tube material behind the table 1 adding barium sulfate
| Sequence number | Zinc oxide/g | Barium sulfate/g | Zinc oxide barium sulfate mass ratio | Flow diameter/mm |
| 1 | 0.2045 | 0 | —— | 36.2 |
| 2 | 0.1996 | 0.046 | 4∶1 | 30.9 |
| 3 | 0.2165 | 0.0728 | 3∶1 | 28.5 |
| 4 | 0.2087 | 0.1035 | 2∶1 | 25.6 |
| 5 | 0 | 0.2130 | —— | 23.5 |
Zinc oxide and nano zircite are evenly made powder according to certain mixed, itself and the Oleum Caryophylli ratio with 2: 1 is in harmonious proportion, it is as shown in table 2 below to record its flow diameter data.
The flowability of root tube material behind the table 2 adding nano zircite
| Sequence number | Zinc oxide/g | Zirconium oxide/g | Zinc oxide zirconium oxide mass ratio | Flow diameter/mm |
| 1 | 0.2045 | 0 | —— | 36.2 |
| 2 | 0.1987 | 0.0386 | 5∶1 | 31.5 |
| 3 | 0.2015 | 0.0633 | 3∶1 | 30 |
| 4 | 0.2077 | 0.1064 | 2∶1 | 28.5 |
| 5 | 0 | 0.2010 | —— | 22 |
Mobile obvious the good of barium sulfate that add of root canal filling material that adds nano zircite, respectively No. 3 two groups of materials in last table 1 and the table 2 are done the X ray resistance and penetrate test, the result shows: the thick dish of the 2mm that is made by the root canal filling material that adds nano zircite is better than the thick aluminium sheet of 6mm to the attenuation of X ray; And the thick dish of the 2mm that the root canal filling material that adds barium sulfate is made is better than the thick aluminium sheet of 2mm to the attenuation of X ray.
Embodiment 2:
With weight ratio is 51% zinc oxide, 25% barium sulfate, and 5% thymol, 18.75% coral second erythromycin and 0.25% steroid glucocorticoid stir and make its mix homogeneously.
The powder that prepared and Oleum Caryophylli transferred with 2.5: 1 ratio mix, prepared root canal filling material dissolubility is low, its mobile general, penetrating property of X ray resistance a little less than.
Embodiment 3:
With weight ratio is 50% nano zine oxide, 23% nano zircite, and the thymol of nanometer hydroxyapatite 5%, 4%, 17.75% coral second erythromycin and 0.25% steroid glucocorticoid stir and make its mix homogeneously.
The powder and the Oleum Caryophylli that are prepared are mixed with 2.5: 1 ratio accent, and prepared root canal filling material dissolubility is low, and has good flowability, penetrating property of X ray resistance.
Embodiment 4:
With weight ratio is 46% nano zine oxide, 20% nano zircite, and the thymol of nanometer hydroxyapatite 4%, 4%, 8% tinidazole, 17.75% erythromycin and 0.25% steroid glucocorticoid stir and make its mix homogeneously.
The powder and the Oleum Caryophylli that are prepared are mixed with 2.5: 1 ratio accent, and prepared root canal filling material dissolubility is low, and has good flowability, penetrating property of X ray resistance.
Embodiment 5:
The nano silver-supported antibacterial powder is to gram-bacteria staphylococcus aureus and escherichia coli, as shown in table 3, and the bacteriostasis rate more than the effect 2min is all greater than 93%.
Table 3 nano silver-supported antibacterial powder is to staphylococcus aureus and colibacillary bacteriostasis rate
| Action time (min) | 2 | 5 | 10 | 20 |
| To staphylococcus aureus bacteriostasis rate (%) | 93.67 | 94.64 | 95.35 | 96.29 |
| To escherichia coli bacteriostasis rate (%) | 93.01 | 94.35 | 95.45 | 96.82 |
Embodiment 6:
With weight ratio is 55% nano zine oxide, 28% nano zircite, and the thymol of nano silver-supported antibacterial powder 5%, 4%, 7.75% tinidazole, 0.25% steroid glucocorticoid stir and make its mix homogeneously.
The powder and the Oleum Caryophylli that are prepared are mixed with 2.5: 1 ratio accent, and prepared root canal filling material dissolubility is low, and has good flowability, penetrating property of X ray resistance.Replace the antibiotics medicine with the nano silver-supported antibacterial powder, its anti-gram-bacteria effect significantly strengthens, and has improved the biocompatibility of root canal filling material.
Claims (9)
1, a kind of nano zinc oxide clove oil root canal filling material, it is characterized in that the chemical composition of this filler is: powder accounts for 60%～75%, and Oleum Caryophylli accounts for 25%～40%;
Wherein: the chemical composition weight % of powder is: inorganic constituents nano-ZnO 46%～90%, particle diameter are 10～380nm; Inorganic constituents nanometer ZrO
25%～40%, its particle diameter is 10～600nm; Inorganic constituents nanometer hydroxyapatite≤10%, particle diameter are 80～100nm; Inorganic constituents nano silver-supported antibacterial powder≤10%, its particle diameter are 90～150nm; Thymol 2%～10%, anti-anaerobic agent≤10%, antibiotic≤25%, steroid glucocorticoid＜1%.
2, nano zinc oxide clove oil root canal filling material according to claim 1 is characterized in that the nano-ZnO granule that adopted is more than one of sphere, ellipse, bar-shaped needle-like, four angular pin shapes, four jiaos of bar-shaped or colored shapes.
3, nano zinc oxide clove oil root canal filling material according to claim 1 is characterized in that inorganic constituents nanometer ZrO
2For through Y
2O
3Stable cubic phase ZrO
2
4, nano zinc oxide clove oil root canal filling material according to claim 1 is characterized in that the needle-like that is shaped as of inorganic constituents nano-hydroapatite particles, and long telomere directly is 1～20nm, and short telomere directly is 1～5nm.
5, nano zinc oxide clove oil root canal filling material according to claim 1, the main component that it is characterized in that inorganic constituents nano silver-supported antibacterial powder are that nanometer hydroxyapatite carries nano titanium oxide and nanometer silver chelating body.
6, nano zinc oxide clove oil root canal filling material according to claim 1 is characterized in that anti-anaerobic agent is any in metronidazole, tinidazole and the ornidazole.
7, nano zinc oxide clove oil root canal filling material according to claim 1 is characterized in that antibiotic is any in erythromycin series, Tetracyclines and the cephalosporins medicine.
8, nano zinc oxide clove oil root canal filling material according to claim 1 is characterized in that the steroid glucocorticoid is any in dexamethasone, prednisolone, prednisolone acetate, hydrocortisone and the cortisone acetate.
9, the preparation method of nano zinc oxide clove oil root canal filling material according to claim 1 is characterized in that this method comprises following concrete steps:
At first above-mentioned powder is constituted by proportioning, adopt double spiral agitator with its mix homogeneously, wherein double spiral agitator mixing rotating speed is 10～180 rev/mins, and incorporation time is 5～60min; And then powder and Oleum Caryophylli concocted in 1.5: 1～3: 1 ratios, the temperature that is in harmonious proportion is 23 ℃ ± 1 ℃, relative humidity is 45%～55% during mediation.
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| CN103690376B (en) * | 2013-12-31 | 2015-09-23 | 徐崇明 | Dental pulp root canal filling paste |
| CN105055176B (en) * | 2015-08-11 | 2018-08-21 | 何祥一 | A kind of tea polyphenols root canal sealant with good physical and bacteriostasis property |
| CN106747402A (en) * | 2016-12-23 | 2017-05-31 | 江南大学 | A kind of preparation method of novel antibacterial bioceramic porous material |
| CN107854322A (en) * | 2017-10-24 | 2018-03-30 | 武汉大学 | A kind of preparation method of nano calcium hydroxide for root canal filling material |
| CN115137653A (en) * | 2018-03-30 | 2022-10-04 | 徐崇明 | Filling paste for dental pulp conservation treatment and preparation method thereof |
| CN114191314A (en) * | 2021-12-01 | 2022-03-18 | 张占山 | Mineral filling material and preparation method and application thereof |
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