CN106885881A - A kind of experimental technique of simulating oral cavity environment is used for material and the application of the environment - Google Patents
A kind of experimental technique of simulating oral cavity environment is used for material and the application of the environment Download PDFInfo
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- CN106885881A CN106885881A CN201710101848.7A CN201710101848A CN106885881A CN 106885881 A CN106885881 A CN 106885881A CN 201710101848 A CN201710101848 A CN 201710101848A CN 106885881 A CN106885881 A CN 106885881A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses material and application that a kind of experimental technique of simulating oral cavity environment is used for the environment, experimental technique includes the treatment of configuration lactic acid solution and demineralization dentine sample；NACP resins include 100 parts of the resin containing nm amorphous calcium phosphate, 0.2 part of camphorquinone and to N, 0.8 part of N dimethylaminobenzoic acids isopentyl ester；With the effect of pH value of the PAMAM solution combination with buffer lactic acid solution, release calcium phosphorus particle and promotion demineralization dentine sample remineralization；Present invention simulation is directed to the preventing and treating that saliva amount declines patient's dental caries entirely without the extreme oral environment of saliva beneficial to carrying out；Can clinical practice the dental caries preventing and treating of patient is reduced in saliva amount, simple to operate, feasibility is high.
Description
Technical field
The present invention relates to dentistry Material Field, and in particular to a kind of experimental technique of simulating oral cavity environment is used for the ring
The material in border and application.
Background technology
Secondary caries is to cause the main reason of resin fill repairing failure, the primary dental caries of risk dental caries crowd high
Incidence with secondary caries is all far above normal population；Saliva is promoting demineralization tooth hard tissue remineralization, is suppressing dental caries progress
During play vital effect；Saliva, can because having powerful buffer capacity rich in compositions such as bicarbonates
Penetrate into bacterial biof iotalm, neutralize the acid product of cariogenic bacteria, raise the pH value of local microenvironment；Also, in saliva rich in calcium,
Phosphonium ion, it is possible to decrease the solubility of the main component-hydroxyapatite of dental hard tissue, promotes its remineralization；However, about 30%
Population all can with the symptom of dry, reason include the Excess free enthalpy of alcohol, the taking of some drugses, it is malnutritive, some
Systemic disease, salivary gland function obstacle etc.；Because of the reduction of salivary secretion total amount, salivary flow may be down to normal level
15%-33%, it is meant that biomembrane center bacterial acid product, offer calcium, the saliva amount of phosphorus particle can be provided and be greatly reduced；Saliva
Liquid measure is reduced and takes place mostly in the elderly, and research shows, the incidence of American's cementum caries increases and raises with the age；Wherein,
Cementum caries incidence is only 7% in young man；And the incidence of disease may be up to 56% in being more than the elderly of 75 years old；In addition, because of incidence
Tumour and receive radiotherapy patient can occur saliva amount drastically reduction, cause the generation of rampant caries；At present, for saliva
The patient for reducing is measured, effective preventing decayed tooth method is clinically there is no, the disease by mitigating dry using some Saliva Substitutes is only capable of
Shape, but it is very little for the protective effect of tooth；Therefore, finding can protect material and the side of such crowd dental hard tissue
Method has high clinical meaning；There is presently no very effective experimental technique and material.
The content of the invention
The experimental technique that saliva amount drastically reduces patient's oral environment is simulated the invention provides a kind of, and for the oral cavity
The material of environment and application.
The technical solution adopted by the present invention is：A kind of experimental technique of simulating oral cavity environment, comprises the following steps：
（1）Configuration lactic acid solution
The NaCl solution of 133mmol/L is added in the lactic acid solution of 50mmol/L, until the pH value of lactic acid solution is 4；
（2）By demineralization dentine sample in step（1）Processed in the solution for obtaining
By demineralization dentine sample step（1）In the solution that obtains immersion treatment is carried out under the conditions of 37 DEG C, it is often small by 24
When change a solution, continue 21 days.
A kind of material in simulating oral cavity environment, its component is as follows by weight percentage：Phosphoric acid containing nm amorphous
100 parts of the resin of calcium abbreviation NACP, 0.2 part of camphorquinone and p- N, 0.8 part of N- dimethylaminobenzoic acids isopentyl ester, nothing containing nanometer
Its component of the resin of amorphous calcium phosphate is as follows by weight percentage：Nm amorphous calcium phosphate 40%, barium Boroalumino silicate glasses
20% and EBPM40%, wherein EBPM are that ethoxylated bisphenol A dimethylacrylates and pyromellitic acid anhydride glyceride press quality
Than being 1:1 mixture for constituting；Barium Boroalumino silicate glasses through 4% 3-（Methacryloxypropyl）Propyl trimethoxy silicane and
2% n-propylamine silanization gained.
The application of a kind of material for simulating oral cavity environment, with end group for the polyamidoamine dendroid of amino is polymerized
Thing solution is used in combination；Application method be by polyamide that the end group that demineralization dentine sample concentration is 1mg/mL is amino-
After amine type dendrimer solution immersion treatment 1h, the resin after solidification is placed in the contact of demineralization dentine sample surface.
Further, in the environment buffer lactic acid solution pH value.
Further, calcium, phosphorus particle are discharged in the environment.
Further, demineralization dentine sample remineralization is promoted in the environment.
Further, the recovery of demineralization dentine sample hardness is promoted in the environment.
The beneficial effects of the invention are as follows：
（1）Invention emulates pure acid, not calcic phosphorus particle the extreme oral environment entirely without saliva, be conducive to carrying out pin
Decline the preventing and treating of patient's dental caries to saliva amount；
（2）The invention discloses a kind of material for improving simulating oral cavity environment, can clinical practice in saliva amount reduce patient
Dental caries preventing and treating；
（3）The invention provides a kind of application process containing NACP resin materials, can be with solution in buffered analog oral environment
PH, discharges calcium phosphorus particle, promotes demineralization dentine remineralization；
（4）The method of the invention is simple to operate, feasibility is high.
Brief description of the drawings
Fig. 1 be in the embodiment of the present invention 1 four treatment groups after simulating oral cavity environment changes the liquid time in difference after 15 minutes
The pH value of solution.
Fig. 2 be in the embodiment of the present invention 1 four treatment groups after simulating oral cavity environment changes the liquid time in difference after 60 minutes
The pH value of solution.
Fig. 3 be the embodiment of the present invention 1 in four treatment groups it is molten after 3 hours after simulating oral cavity environment changes the liquid time in difference
The pH value of liquid.
Fig. 4 be in the embodiment of the present invention 1 four treatment groups after simulating oral cavity environment changes the liquid time in difference after 24 hours
The pH value of solution.
Fig. 5 be the embodiment of the present invention 2 in four treatment groups in simulating oral cavity environment the calcium in the solution that different time is measured
The concentration of ion.
Fig. 6 be the embodiment of the present invention 2 in four treatment groups in simulating oral cavity environment the phosphorus in the solution that different time is measured
The concentration of ion.
Fig. 7 be the embodiment of the present invention 3 in four treatment groups simulating oral cavity environment process 21 days after it is small perpendicular to dentine
Observe the scanning electron microscope (SEM) photograph of dentine sample in pipe direction.
Fig. 8 be the embodiment of the present invention 3 in four treatment groups simulating oral cavity environment process 21 days after it is small parallel to dentine
Observe the scanning electron microscope (SEM) photograph of dentine sample in pipe direction.
Fig. 9 is four treatment groups dentine sample table after simulating oral cavity environment is processed 21 days in embodiment 3 in the present invention
The calcium atom percentage that face is measured by EDS.
Figure 10 is four treatment groups dentine sample table after simulating oral cavity environment is processed 21 days in embodiment 3 in the present invention
The phosphorus atoms percentage that face is measured by EDS.
Figure 11 is for four treatment groups process 7,14 and 21 days backteeth sheets in simulating oral cavity environment in embodiment 4 in the present invention
Matter firmness change and normal dentine, phosphoric acid acid etching backteeth eigen hardness figure.
Specific embodiment
The present invention will be further described with specific embodiment below in conjunction with the accompanying drawings.
Carry out in simulating oral cavity environment in following embodiments, the experimental technique of simulating oral cavity environment includes following step
Suddenly：
（1）Configuration lactic acid solution
The NaCl solution of 133mmol/L is added in the lactic acid solution of 50mmol/L, until the pH value of lactic acid solution is 4；This
Solution is simulation entirely without saliva, in acid extreme oral environment；
（2）By demineralization dentine sample in step（1）Processed in the solution for obtaining
Demineralization dentine sample is placed in the conical flask that a volume is 1.5ml, 1ml steps are used（1）In the solution that obtains 37
Immersion treatment is carried out under the conditions of DEG C, often a solution was changed by 24 hours, continues 21 days；Added using water-bath in this experimental procedure
Thermal environment ensures to be constantly in 37 DEG C of conditions；By demineralization dentine sample by above-mentioned treatment, you can to simulate tooth in pure acid
The extreme oral environment without saliva without calcium phosphorus particle of property.
A kind of material in simulating oral cavity environment, the referred to as resin containing NACP, its component are as follows by weight percentage：
100 parts of resin containing nm amorphous calcium phosphate, 0.2 part and p- N of camphorquinone, 0.8 part of N- dimethylaminobenzoic acids isopentyl ester,
Its component of resin containing nm amorphous calcium phosphate is as follows by weight percentage：Nm amorphous calcium phosphate 40%, barium boron manosil AS
Salt glass 20% and EBPM40%, wherein EBPM are ethoxylated bisphenol A dimethylacrylates and pyromellitic acid anhydride glyceride
In mass ratio it is 1:1 mixture for constituting；Wherein the median grain diameter of barium Boroalumino silicate glasses is 1.4 μm, is barium boron manosil AS
Salt glass through 4% 3-（Methacryloxypropyl）Propyl trimethoxy silicane and 2% n-propylamine silanization gained, purchased from Deng Shibai
Global group；Camphorquinone and p- N, N- dimethylaminobenzoic acid isopentyl ester are used as the light-initiated of the resin containing cyclopentadiene resin
Agent.
The application of a kind of material for simulating oral cavity environment, with end group for the polyamidoamine dendroid of amino is polymerized
Thing solution is used in combination；Application method be by polyamide that the end group that demineralization dentine sample concentration is 1mg/mL is amino-
After amine type dendrimer solution immersion treatment 1h, the resin after solidification is placed in the contact of demineralization dentine sample surface；End
Base uses third generation end group to be polymerized for the polyamidoamine dendroid of amino for the polyamide-amine type branch-shape polymer of amino
50mgPAMAM powder is dissolved in 50ml distilled water thing, abbreviation PAMAM the PAMAM solution for obtaining 1mg/mL under normal temperature, normal pressure；
Third generation end group for amino polyamide-amine type branch-shape polymer be with ethylenediamine for starting core, repeatedly with acrylic acid first
Ester by amidation process with ethylenediamine by being prepared from after Michael addition reactions again；It is new purchased from Weihai Chen Yuan chemical industry
Materials Co., Ltd；The particle of nm amorphous calcium phosphate used is obtained by spray drying process；Specific method is as follows：Carbonic acid
Calcium and Dicalcium Phosphate are dissolved in acetum respectively, obtain the final concentration of 8mmol/L of calcium ion, phosphorus particle final concentration of
The solution of 5.333mmol/L, water and acid are evaporated during the spray solution is entered into a heater, and electrostatic precipitator is collected dried
Particle, the NACP mean particle sizes obtained by the method are 116nm.
The specific preparation method of demineralization dentine sample is as follows in example below：
（1）Outpatient Service Stomatology collects in vitro healthy third molar, with 0.005% thymol solution disinfection 4h, with distillation water logging
Bubble, in 4 DEG C of preservations；
（2）With diamond blade in enamelo-cemental junction top about 4mm at perpendicular to the direction of long axis of tooth cut 4 × 4 × 1mm tooth
Essential sample；
（3）Dentine sample simulates dentine demineralization with 37% phosphoric acid solution immersion treatment 15s；
（4）The ultrasonically treated 10min of dentine sample distilled water of demineralization uses PBS to remove surface bacterial plaque（phosphate-
Buffered saline, pH=7.4）Solution soaks, in 4 DEG C of preservations.
The dentine sample after demineralization is divided into four groups in following examples, every group of six samples, the every group of specific side for the treatment of
Method is as follows：
（1）Control group：Each demineralization dentine sample is dried up after being processed with 100 μ L distilled water immersions；
（2）PAMAM groups：Each demineralization dentine sample uses distilled water flushing with 100 μ LPAMAM solution immersion treatment 1h；
（3）NACP groups：The NACP trees of 2 × 2 × 12mm after 3 pieces of photocurings are placed in the contact of each demineralization dentine sample surface
Fat bar；
（4）PAMAM+NACP groups：With after 100 μ LPAMAM solution immersion treatments 1h, surface contacts each demineralization dentine sample
Place the NACP resin streaks of 2 × 2 × 12mm after 3 pieces of photocurings.
Embodiment 1
Tested using above-mentioned simulating oral cavity environment, 15min after changing liquid respectively at the 1st, 3,5,7,10,14 and 21 days,
60min, 3h and the four groups of pH of lactic acid solution of measurement in 24 hours；Test result is as Figure 1-4；Breast in PAMAM groups and control group
The pH value substantially constant of acid solution is in 4；The pH value of NACP groups and PAMAM+NACP groups is essentially identical.
The lactic acid solution of NACP groups and PAMAM+NACP groups rose to 6.0 at the 1st day during 15min；NACP groups and PAMAM+
The lactic acid solution of NACP groups rose to 6.5 at the 1st day during 60min；The lactic acid solution of NACP groups and PAMAM+NACP groups at the 1st day,
6.9 are risen to during 3h；Solution ph measured by first day to the 21st day is declined slightly；NACP groups and PAMAM+NACP groups are
21 days, pH value rose to 5.5 during 15min；6.5 are risen to during 3h；Illustrate the buffered acid solutions that the resin containing NACP can be stronger
PH value, improves the environment of dentine remineralization.
Embodiment 2
Tested using above-mentioned simulating oral cavity environment, respectively at using Spectrophotometric Determination after the 1st, 3,5,7,10,14 and 21 days
Measure calcium, phosphate ion concentration in four groups of lactic acid solutions；1ml solution is taken during measurement every time to measure；Measurement result such as Fig. 5 and Fig. 6
It is shown；Calcium phosphorus particle concentration all substantially constants are in 0 in PAMAM groups and control group solution；Calcium in NACP groups and PAMAM+NACP groups,
Phosphate ion concentration is basically identical.
It the 1st day is 37mmol/L that calcium ion concentration is in NACP groups and PAMAM+NACP group solution, is within the 21st day 6mmol/
L, phosphate ion concentration the 1st day is 15mmol/L, is within the 21st day 3mmol/L；Illustrate that the resin containing NACP can be in pure acidity, without calcium
Calcium, phosphonium ion necessary to the essential remineralization of pressure are discharged in the solution of phosphorus particle.
Embodiment 3
Tested using above-mentioned simulating oral cavity environment, after testing 21 days, each sample diamond blade is cut to two halves, half
For detecting cross section（Perpendicular to dentinal tubule direction）, second half is used to detect vertical section（Parallel to dentinal tubule
Direction）；Every part of sample is soaked in the PBS solution containing 1% glutaraldehyde and preserves 4h in 4 DEG C, is then dehydrated with graded ethanol, 100%
Hmds rinse after metal spraying；Scanning electron microscopic observation sample is used, while detecting chemical element group with energy dispersive spectrometry
Point；Its ESEM testing result is as shown in Figure 7 and Figure 8；Chemical element component result is as shown in Figure 9 and Figure 10；A figures in Fig. 7
Represent scanning electron microscope (SEM) photograph of the control group perpendicular to dentinal tubule direction；Figure C is its partial enlarged drawing；B figures are represented in Fig. 7
Perpendicular to the scanning electron microscope (SEM) photograph in dentinal tubule direction, figure D is its partial enlarged drawing to PAMAM groups；E figures represent NACP groups in Fig. 7
Perpendicular to the scanning electron microscope (SEM) photograph in dentinal tubule direction, figure G is its partial enlarged drawing；F figures represent that PAMAM+NACP groups are hung down in Fig. 7
Directly in the scanning electron microscope (SEM) photograph in dentinal tubule direction, figure H is its partial enlarged drawing；I figures represent control group parallel to tooth sheet in Fig. 8
The scanning electron microscope (SEM) photograph in matter tubule direction；Figure K is its partial enlarged drawing；J figures represent PAMAM groups parallel to dentinal tubule in Fig. 8
The scanning electron microscope (SEM) photograph in direction；Figure L is its partial enlarged drawing；M figures represent ANCP groups sweeping parallel to dentinal tubule direction in Fig. 8
Retouch electron microscope；Figure O is its partial enlarged drawing；I figures represent scanning of the PAMAM+NACP groups parallel to dentinal tubule direction in Fig. 8
Electron microscope；Figure P is its partial enlarged drawing；Open tubules in the sample of PAMAM groups and control group as shown in Figure 7 and Figure 8,
Without mineral precipitation, visible exposed dentin collagen fiber under high power lens；In NACP group samples, it is seen that a small amount of mineral deposition is in tooth
In tubules；In PAMAM+NACP groups, a large amount of needle-like mineral depositions in dentinal tubule, close dentinal tubule, away from
The depth that 30 μm of surface still can observe the generation of remineralization.
Control group and PAMAM group EDS figures have no calcium P elements peak；NACP groups EDS schemes visible calcium P elements peak；PAMAM+
NACP groups EDS schemes visible strong calcium P elements peak；Dentin surface's calcium atom percentage is as shown in figure 9, dentin surface's phosphorus
Atom percentage is as shown in Figure 10；Illustrate that PAMAM solution can be in saliva of the present invention amount drastically with the combination of NACP resins
Reduce preferable promotion demineralization dentine remineralization in patient's oral environment.
Embodiment 4
Tested using above-mentioned simulating oral cavity environment, four groups of hardness of dentine sample, dimension were measured respectively at the 7th, 14,21 days
Family name's diamond probe stops 10s to measure hardness with being supported on sample for 20g, each sample measurement 6 times；Also measure simultaneously strong
Health dentine sample, the hardness of the dentine sample after phosphoric acid acid etching demineralization as control, as a result as shown in figure 11；Normal tooth sheet
The hardness of matter is 0.57GPa, and the dentine hardness after phosphoric acid acid etching demineralization is 0.32GPa；The dentine of PAMAM groups and control group
Hardness near 0.2GPa at the 7th day；Near 0.1GPa at the 21st day；PAMAM+NACP group dentine hardness liter at the 7th day
To 0.43GPa, near 0.49GPa at the 14th day rises to 0.53GPa at the 21st day；Without statistics between normal dentine hardness
Learn difference；Illustrate that PAMAM solution can promote demineralization tooth sheet with the combination of NACP resins in the extreme oral environment of present invention simulation
The recovery of matter hardness.
The embodiment of the present invention test result indicate that, simulation saliva amount drastically reduces the dentine ore deposit again of patient's oral environment
Change experimental technique, can extreme oral environment of the preferable simulation entirely without saliva in vitro；And PAMAM solution and NACP resins
Combination can in this extreme environment, discharge calcium phosphorus particle, promote demineralization dentine remineralization；To be directed to saliva amount from now on drastically
The investigation of materials for reducing the preventing and treating of patient's dental caries provides new model and thinking.
Claims (7)
1. a kind of experimental technique of simulating oral cavity environment, it is characterised in that comprise the following steps：
(1) lactic acid solution is configured
The NaCl solution of 133mmol/L is added in the lactic acid solution of 50mmol/L, until the pH value of lactic acid solution is 4；
(2) demineralization dentine sample is processed in the solution that step (1) is obtained
Demineralization dentine sample is carried out into immersion treatment with the solution obtained in step (1) under the conditions of 37 DEG C, it is often small by 24
When change a solution, continue 21 days.
2. a kind of material in simulating oral cavity environment described in claim 1, it is characterised in that its component is by weight percentage
It is as follows：100 parts of resin containing nm amorphous calcium phosphate, 0.2 part of camphorquinone and p- N, N- dimethylaminobenzoic acid isopentyl ester
0.8 part, its component of the resin containing nm amorphous calcium phosphate is as follows by weight percentage：Nm amorphous calcium phosphate 40%, barium
Boroalumino silicate glasses 20% and EBPM40%, wherein EBPM are ethoxylated bisphenol A dimethylacrylates and Pyromellitic Acid
Dianhydride glyceride is 1 in mass ratio:1 mixture for constituting；Barium Boroalumino silicate glasses through 4% 3- (methacryloxypropyl) third
Base trimethoxy silane and 2% n-propylamine silanization gained.
3. a kind of application of the material for being used for simulating oral cavity environment as claimed in claim 3, it is characterised in that：It is amino with end group
Polyamide-amine type branch-shape polymer solution be used in combination；It by demineralization dentine sample concentration is 1mg/ that application method is
After the end group of mL is for the polyamide-amine type branch-shape polymer solution immersion treatment 1h of amino, in demineralization dentine sample surface
The resin after solidification is placed in contact.
4. application according to claim 3, it is characterised in that：The pH value of buffer lactic acid solution in the environment.
5. application according to claim 3, it is characterised in that：Calcium, phosphorus particle are discharged in the environment.
6. application according to claim 3, it is characterised in that：Promote demineralization dentine sample ore deposit again in the environment
Change.
7. application according to claim 3, it is characterised in that：Promote demineralization dentine sample hardness in the environment
Recover.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109298146A (en) * | 2018-09-11 | 2019-02-01 | 郑州大学第附属医院 | Imitate the experimental provision of oral environment and the research method of dental enamel Demineralization |
| CN112999094A (en) * | 2021-03-01 | 2021-06-22 | 广西医科大学附属口腔医院 | Nano complex for inducing bionic internal mineralization of collagen fibers and preparation method thereof |
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| US6001897A (en) * | 1997-01-13 | 1999-12-14 | American Dental Association Health Foundation | Polymerizable conditioners for adhesive bonding to dentin and enamel |
| CN101102741A (en) * | 2004-11-16 | 2008-01-09 | 3M创新有限公司 | Dental compositions with calcium phosphorus releasing glass |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109298146A (en) * | 2018-09-11 | 2019-02-01 | 郑州大学第附属医院 | Imitate the experimental provision of oral environment and the research method of dental enamel Demineralization |
| CN109298146B (en) * | 2018-09-11 | 2021-09-28 | 郑州大学第一附属医院 | Experimental device for simulating oral tooth enamel demineralization and research method for tooth enamel demineralization |
| CN112999094A (en) * | 2021-03-01 | 2021-06-22 | 广西医科大学附属口腔医院 | Nano complex for inducing bionic internal mineralization of collagen fibers and preparation method thereof |
| CN112999094B (en) * | 2021-03-01 | 2022-06-17 | 广西医科大学附属口腔医院 | Nano complex for inducing bionic internal mineralization of collagen fibers and preparation method thereof |
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Application publication date: 20170623 |