CN105055176B - A kind of tea polyphenols root canal sealant with good physical and bacteriostasis property - Google Patents
A kind of tea polyphenols root canal sealant with good physical and bacteriostasis property Download PDFInfo
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- CN105055176B CN105055176B CN201510489626.8A CN201510489626A CN105055176B CN 105055176 B CN105055176 B CN 105055176B CN 201510489626 A CN201510489626 A CN 201510489626A CN 105055176 B CN105055176 B CN 105055176B
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- root canal
- tea polyphenols
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Abstract
The invention discloses tea polyphenols root canal sealants, belong to oral cavity material technical field.The tea polyphenols root canal sealant of the present invention is that tea polyphenols are added in zinc oxide clove oil sealer, the effect of making tea polyphenols, zinc oxide and caryophyllus oil, generates collaboration, clearly enhance its bacteriostasis property, the toxicity for effectively reducing zinc oxide clove oil simultaneously is a kind of with good physical and bacteriostasis property tea polyphenols root canal sealant.Bacteriostatic experiment shows that tea polyphenols root canal sealant prepared by the present invention has good inhibiting effect to indicator bacteria；Physical Experiment shows that the physical property of tea polyphenols root canal sealant meets the performance standard of sealer；Clinical test shows that tea polyphenols root canal sealant can effectively reduce the incidence of the acute diseases such as pain after root canal, while can improve the long-term success rate of root canal.Therefore, it is expected to apply to clinic as a kind of novel root canal sealing material.
Description
Technical field
The invention belongs to oral cavity material technical fields, are related to a kind of root canal sealant, more particularly to a kind of with good object
Reason and bacteriostasis property tea polyphenols root canal sealant.
Background technology
Root canal is dental pulp and the most effective therapy of periapical disease, and the success rate of root canal at present is 53%-
95%, how to continue the success rate of raising root canal is still the research hotspot of domestic and foreign scholars.Root canal fail the reason of be
It is various, such as misoperation etc. in the complexity of root canal system, therapeutic process, research shows that it is main the reason is that microorganism because
The bacterium of element, obstinate not easy-clear results in the failure of root canal.The main reason for root canal fails is microbiological factor,
Inhibit the growth of Candida albicans and enterococcus faecalis significant for the mortality for reducing root canal.Although root canal sealing
Added with antibiotic has preferable fungistatic effect in agent, but the abuse of antibiotic causes many bio-safeties such as bacterial resistance in recent years
Problem, so it is critically important to find a kind of good natural drug of bacteriostasis property as the additive of root canal sealant.
Zinc oxide clove oil root canal sealant is a kind of root canal sealant with bacteriostasis property, but its clinical and
Certain cytotoxicity is shown in vitro study（Its toxicity is mainly derived from the caryophyllus oil released after its solidification
Phenol）, therefore bring limitation to its clinical application.
Tea polyphenols (Tea Polyphenols, TP) are the general names of Polyphenols chemical substance in tealeaves, are to have guarantor in tealeaves
One of main ingredient of health-care function has the effects that remove halitosis, promotes canker sore healing, anti-oral cavity radiation injury, simultaneously
Tea polyphenols can inhibit the growth of oral cavity various pathogens.Some researches show that tea polyphenols for Candida albicans, the excrement in root pipe
The formation of the biomembranes such as enterococcus has inhibiting effect.But tea polyphenols are added in root canal sealant, it develops a kind of novel
There is not been reported for tea polyphenols root canal sealant.
Invention content
The object of the present invention is to provide a kind of preparation sides with good physical and bacteriostasis property tea polyphenols root canal sealant
Method.
One, the preparation of tea polyphenols root canal sealant
The present invention tea polyphenols root canal sealant, be in zinc oxide clove oil sealer be added tea polyphenols be uniformly mixed and
.Wherein the mass percent of tea polyphenols and zinc oxide is 0.25-1%, 99.75-99%；Tea polyphenols is dense in tea polyphenols sealer
Degree is 2.5-10g/L.
Two, the performance test of tea polyphenols root canal sealant
1. the measurement of bacteriostasis property
Using agar diffusion method, indicator bacteria be Candida albicans ( Canidia albicans, C.albicans)ATCC
10231, enterococcus faecalis (Enterococcus faecalis, E.faecalis) ATCC 29212, staphylococcus aureus
(Staphylococcus aureus, S.aureus) ATCC 25923, Escherichia coli (Escherichia coli, E.coli) 25922 reference cultures (offer of oral microorganism key lab of State Nationalities Affairs Commission of Northwest University for nationalities) of ATCC.
10 μ L of bacterium solution are mixed into when 100mLBHI medium sterilizations postcooling is to 45 DEG C（CFU 1x106/ml）, pour into be solidified in culture dish
It is uniformly punched with card punch afterwards.According to the tea polyphenols root pipe that different quality containing is added in the hole laid successively clockwise
Sealer, until it is concordant with media surface, negative control is done with zinc oxide root canal sealant；Tablet is placed in 37 DEG C of incubator trainings
It supports for 24 hours.Antibacterial circle diameter is measured according to crossing method electronic ruler.
The bacteriostasis of different quality containing root canal sealant is as shown in Figure 1, wherein Blank is negative control group（Oxidation
Zinc caryophyllus oil root canal sealant）；A, the mass fraction that B, C, D respectively represent tea polyphenols is 0.25%, 0.5%, 1% and 2%.Statistical
Each group sealer inhibition zone size and group difference are as shown in Figure 2 after analysis（* it indicatesp<0.05）.Antibacterial circle diameter：Blank<A<B
<C<D；WhereinC.albicansWithE.faecalis Blank and A andS.aureus Blank and A, the A nothing compared between B groups
Significant difference (P>0.05), compare significant difference (P two-by-two between other groups<0.05).
Above-mentioned bacteriostatic experiment is the results show that 0.25% tea polyphenols sealer inhibits the energy of Candida albicans and enterococcus faecalis
Power and control group are without significant difference, when mass fraction increases to 0.5%（5 g/L）When just significant difference, show tea polyphenols
Bacteriostasis is proportionate with concentration；1%, 1.5% tea polyphenols sealer is very strong to the inhibiting effect of staphylococcus aureus,
With blank group, 0.25%, 0.5% there were significant differences；In addition, 0.25% sealer shows stronger inhibition to Escherichia coli
Effect.Therefore, the tea polyphenols root canal sealant that prepared by the present invention has good inhibiting effect, and 0.5%, 1% to indicator bacteria
Sealer with 1.5% is substantially better than blank group and 0.25% to the inhibiting effect of indicator bacteria.
2. the measurement of mobility
Using ISO 6878:2001 method, conveying 0.05mL (± 0.005mL) sealer are placed in glass core,
The weight block of second piece of glass plate and 100g (± 2g) is pressed in above after 180s (± 5s).Removed after 10min weight block and
Measure pressed sealer test piece diameter.Each sealer test piece measures 3 times, is accurate to 0.001mm.
Each group sealer mobility size and group difference are as shown in figure 3, mobility size：Blank>A>B>C>D；
Blank and A, A there was no significant difference compared between B groups (P>0.05), compare significant difference (P between other groups two-by-two<
0.05)。
Clinically root-canal filling requires sealer to be easily accessible tiny irregular collateral vessel, realizes fully strict fill
It fills out, therefore sealer should have good mobility.This result of study show, be added tea polyphenols rear enclosed agent mobility with
The increase of tea polyphenols mass fraction and reduce, this may be because the presence of tea polyphenols increases the viscosity of material, identical
Load under the less sealer containing tea polyphenols be easy to form the plane being relatively large in diameter, have better mobility, can prevent micro-
Biology and metabolite enter root pipe, prevent the subinfection again of bacterium from leading to the failure of root canal.
3. the measurement of film thickness
Using ISO 6878:2001 method measures the thickness for two glass plates being in contact.Conveying 0.05mL (±
0.005mL) sealer places it in the center of a glass sheets, and second piece of glass plate is put then at center.Since reconciliation
With loading system to the vertical load for applying 150N at the top of glass plate when 180s (± l0s), it is ensured that sealer is completely filled with two
Between glass plate.Thickness of two glass plates together with closing agent film is measured after l0min, is measured 3 times respectively, is taken its average value conduct
Glass plate and the overall thickness for closing agent film are obtained by calculating the difference of the sheet thickness with sealer and without sealer
Go out film thickness.Each sealer test piece measures 3 times, is accurate to l μm.
Each group sealer film thickness size and group difference are as shown in figure 4, film thickness size：Blank<A<B<C<D；
Compare significant difference (P between all groups two-by-two<0.05).
It is an important channel for improving successful rate of root canal therapy to reduce Micro blazed-grating in root canal, and sealer is thin
Film thickness, which crosses conference, makes the gap between gutta-percha and root canal wall increase, and reduces the caking property of root canal sealant, increases Micro blazed-grating
Chance.This result of study shows that sealer film thickness is thickened with the increase of tea polyphenols mass fraction, may be with tea polyphenols
A kind of compounding substances are related, and ingredient is not of uniform size, and particle spacing increases after being mixed with zinc oxide, and film thickness accordingly increases.
According to ISO 6878:2001 standard, film thickness should be not more than 50 μm.The experimental results showed that the film of tea polyphenols sealer is thick
Degree meets national sector standard.
4. the measurement of shrinkage
Using ISO 6878:2001 method, the 2g materials that reconcile are slightly super to be filled in mold, after fixed 5min, is put into opposite
Humidity is 95%-100%, and temperature is in the environment of 37 DEG C (± 1 DEG C).Mold is taken out after 1 day, examination is polished on the damp sand paper of P600
Sample both ends.Its height is measured after removal mold, is accurate to l0 μm.It is stored in 30d in the distilled water of 37 DEG C (± 1 DEG C) afterwards,
Specimen height is measured again, is accurate to 10 μm.The percentage for calculating the variation and former height of specimen height, completes 3 above-mentioned surveys
Amount, shrinkage of the average value as material.
Each group sealer shrinkage size and group difference are as shown in figure 5, shrinkage size：Blank<A<B<C<D；
Blank there was no significant difference compared between A groups (P>0.05), compare significant difference (P between other groups two-by-two<0.05).
The shrinkage of sealer is excessive to will also result in Micro blazed-grating, increases the chance that root pipe infects again.The display of this result of study,
The shrinkage of sealer increases with the mass fraction of tea polyphenols and is increased, and 2% tea polyphenols sealer contraction is the most apparent,
Reason is that the active force between zinc oxide and tea polyphenols particle be not as strong as zinc oxide itself, causes after material solidification in deionization
It is slightly dissolved in water, generates contraction.According to ISO 6878:2001 standard blocking agent shrinkage should be not more than 1.0%.
5. deliquescent measurement
According to the method for M.G.Gandolfi etc. to ISO 6876:2001 method is improved.By material filling in mould
It in tool, is put into climatic chamber after fixed, waits for that sample is taken out in solidification completely for it, measures its mass M 1, is accurate to 0.001g.Afterwards
Sample is placed in deionized water, in the environment of 37 DEG C (± 1 DEG C), is taken out after impregnating 1 day, 7 days and 14 days respectively, after dry
Weigh M2, completes 3 above-mentioned measurements, average value is as final M1 and M2.The dissolving of sealer is calculated using formula
Degree, formula are as follows：Solubility=(M1-M2)/M1 × 100%.
Each group sealer dissolubility size and group difference are as shown in fig. 6, dissolubility size：Blank<A<B<C<D；First
It：Blank is with A, B with C, B with D, C there was no significant difference compared between D groups (P>0.05), the 7th day：A and B, A and C, B and C
Compared to there was no significant difference (P between group>0.05), fortnight：A is the same as C, B there was no significant difference compared between C groups (P>0.05),
Compare significant difference (P between remaining group two-by-two<0.05).
The dissolving of root canal sealant can be such that the closed performance of material reduces, and lead to the generation of Micro blazed-grating, while chemical substance
Release periapical tissue can be stimulated to lead to the failure of root canal, therefore the dissolubility of sealer is also to influence root canal
One key factor.This research experiment the results show that sealer dissolubility with tea polyphenols mass fraction and number of days increase
And increase, it is satisfied by ISO 6876:2001 standard, ensure the close contact of root canal filling material and root canal wall dentine it is seamless go out
It is existing, to reduce the generation of Micro blazed-grating, root canal sealant is made to have comparatively ideal sealing ability.
Three, toxicity test
Using mtt assay, when L-929 cells reach the logarithmic growth end of term, and cell tends to fusion, collagenase digesting dispersion,
It is made into 5 × 104The cell suspension of a/ml takes 96 porocyte culture plates, 100 μ l cell suspensions is added per hole, in containing 5%CO2, it is wet
It is cultivated under the conditions of 37 DEG C of degree and waits for that cell is adherent for 24 hours, discard the original fluid in hole, the DMEM cultures of 100 μ l are separately added into per hole
Base（Negative control group）And the material leaching liquor of tetra- groups of A, B, C, D, continue culture for 24 hours with taken out after 48h.It is added per hole
The MTT50 μ l of 5mg/ml continue after cultivating 4h, are cleaned 2 times with PBS, discard liquid in hole and terminate reaction.150 μ l are added per hole
Dimethyl sulfoxide (DMSO)（DMSO）, 10min is gently shaken at 37 DEG C, surveys its OD value, enzyme-linked instrument wavelength is 490nm.Pattern detection OD
Value takes mean value.Cell opposite proliferation rate is calculated using formula（RGR）, formula is as follows：RGR=ODExperimental group/ODControl group×100%.Tool
Body standard is as shown in Table 1.
Cytotoxicity series corresponding to each group sealer RGR sizes is as shown in table 2, and cytotoxicity size is：Blank>A
>B>C>D>Neg.。
Each group sealer RGR sizes and group difference are as shown in fig. 7, RGR sizes：Blank<A<B<C<D< Neg.；24h：
B there was no significant difference compared between C groups (P>0.05), 48h：B there was no significant difference compared between C groups (P>0.05), remaining group
Between compare significant difference (P two-by-two<0.05).
Zinc oxide clove oil root canal sealant shows certain cytotoxicity in clinical and in vitro study, poison
Property be mainly derived from the Eugenol that is released after its solidification.Extract of the tea polyphenols as tealeaves is a kind of crude drug
Object has no toxic side effect, and has very strong anti inflammatory detoxication effect, and tea polyphenols are added into zinc oxide clove oil sealer,
Effectively reduce the toxicity of zinc oxide clove oil sealer.
Four, clinical test
206 of the patient 206 of selection dental pulp disease or periapical disease suffer from tooth, wherein man 109, female 97, the age 18 ~
63 years old, be permanent teeth.Inclusion criteria is：Patient body health, unsystematic disease；Movable degree≤1 °；X-ray film shows that root pipe is logical
Freely, no calcification；Tip of a root development is completed, tip of a root rarefaction diameter≤1cm.It is respectively A groups that tooth, which will all be suffered from, to be randomly divided into 4 groups（Tea
Polyphenol mass fraction is 0.25%）52 wherein labial teeths 25, backteeth 27, B groups（Tea polyphenols mass fraction is 0.5%）51 its
Middle labial teeth 26, backteeth 25, C groups（Tea polyphenols mass fraction is 1%）52 wherein labial teeths 26, backteeth 26, Blank groups
（ZOE pastes）51, wherein labial teeth 25, backteeth 26.It is all to suffer from tooth further consultation after tight root canal 1 week, according to trouble
Tooth pain condition is divided into 4 grades, respectively reactionless：Any pain；Slightly：Mild pain, occlusion is uncomfortable, can voluntarily alleviate；In
Degree：Spontaneous pain influences to be engaged, and oral anti-inflammatory drug can be alleviated；Severe：Spontaneous pain, apical area swelling, oral anti-inflammatory drug
In vain.The results are shown in Table 3 for it.Curative effect of root canal therapy is divided into successfully and is failed by further consultation again after all patients 1 year, standard
For：Success：No conscious sympton, without pain, no sinus is kowtowed, x-ray shows that primitive root point rarefaction disappears or reduces；Failure：There is subjective symptoms,
Pain is kowtowed, sinus occurs or former sinus is not closed, x-ray shows that primitive root point rarefaction is unchanged or expands, and suffers from tooth and treats or pull out again
It removes.Its result is as shown in Table 4.
Above-mentioned clinical test shows that tea polyphenols root canal sealant can effectively reduce the acute diseases such as pain after root canal
Incidence, while the long-term success rate of root canal can be improved.
In conclusion tea polyphenols are added in zinc oxide clove oil sealer in the present invention, make tea polyphenols, zinc oxide and cloves
Effect of oil generates collaboration, hence it is evident that enhances its bacteriostasis property, while effectively reducing the toxicity of zinc oxide clove oil, is a kind of
With good physical and bacteriostasis property tea polyphenols root canal sealant, there is stronger inhibition for enterococcus faecalis and Candida albicans
Effect, while there is the physical property for meeting national standard, it is expected to apply to clinic as a kind of novel root canal sealing material.
Description of the drawings（* p is indicated<0.05）
Fig. 1 is the bacteriostasis of different quality containing root canal sealant；
Fig. 2 is that the biocidal property of different quality containing root canal sealant compares；
Fig. 3 is that the mobility of different quality containing root canal sealant compares；
Fig. 4 is that the film thickness of different quality containing root canal sealant compares；
Fig. 5 is that the shrinkage of different quality containing root canal sealant compares；
Fig. 6 is the dissolubility of different quality containing root canal sealant（1d、7d、14d）Compare；
Fig. 7 is different quality containing root canal sealant cytotoxicity（24h、48h）Compare.
Specific implementation mode
The preparation of tea polyphenols root canal sealant of the present invention and performance are described further below by specific embodiment.
The tea polyphenols 1% of mass fraction, zinc oxide 99% are mixed and made into pulvis, then are mixed with caryophyllus oil by embodiment 1
It is even, tea polyphenols sealer, wherein a concentration of 10 g/L of tea polyphenols is made.Its property indices is shown in Fig. 1-7.
The tea polyphenols 0.5% of mass fraction, zinc oxide 99.5% are mixed and made into pulvis, then are mixed with caryophyllus oil by embodiment 2
Uniformly, tea polyphenols sealer, wherein a concentration of 5 g/L of tea polyphenols is made.Its property indices is shown in Fig. 1-7.
The tea polyphenols 0.25% of mass fraction, zinc oxide 99.75% are mixed and made into pulvis by embodiment 3, then mixed with caryophyllus oil
It closes uniformly, tea polyphenols sealer, wherein a concentration of 2.5 g/L of tea polyphenols is made.Its property indices is shown in Fig. 1-7.
Tea polyphenols purity 98% in above-described embodiment and experiment, by Shanghai, she blocks biological Co., Ltd and provides.
Claims (2)
1. a kind of tea polyphenols root canal sealant with good physical and bacteriostasis property is added in zinc oxide clove oil sealer
Enter tea polyphenols to be uniformly mixed and obtain；The mass percent of the tea polyphenols and zinc oxide is 0.5-1%, 99.5-99%.
2. the tea polyphenols root canal sealant with good physical and bacteriostasis property as described in claim 1, it is characterised in that：Tea is more
A concentration of 2.5-10g/L of tea polyphenols in phenol block agent.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1899240A (en) * | 2006-07-07 | 2007-01-24 | 安泰科技股份有限公司 | Nano zinc oxide clove oil root canal filling material and its preparing method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5865207A (en) * | 1981-10-13 | 1983-04-18 | Sunstar Inc | Cement for teeth root canal filling |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1899240A (en) * | 2006-07-07 | 2007-01-24 | 安泰科技股份有限公司 | Nano zinc oxide clove oil root canal filling material and its preparing method |
Non-Patent Citations (3)
| Title |
|---|
| Comparative Toxicity of Eugenol and Its Quinone Methide Metabolite in Cultured Liver Cells Using Kinetic Fluorescence Bioassays;David C.Thompson et al;《toxicology and applied pharmacology》;19981231(第149期);第55-63页 * |
| 根管充填材料加入茶多酚抑制白色念珠菌生物膜的生成;许颖等;《中国组织工程研究》;20130521;第17卷(第21期);第3983-3990页 * |
| 绿茶多酚对甲醛致内皮细胞株（HUVEC-12）损伤的影响及其机制;邹云飞;《中国优秀博硕士学位论文全文数据库（硕士） 医药卫生科技辑》;20061115(第11期);第23-26页 * |
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