CN105688288A - Collagen based composite dental restoration membrane material and preparation method thereof - Google Patents
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Abstract
The invention discloses a collagen based composite dental restoration membrane material and a preparation method thereof. The method comprises steps as follows: type I collagen is subjected to crosslinking modification by oxidized carboxymethyl chitosan firstly, meanwhile, self-assembly of the collagen is promoted with a thermal driving method, a collagen based material is subjected to further crosslinking and pre-calcification sequentially, finally, biomimetic mineralization is performed in 1-10 times of an SBF (simulated body fluid) solution with trace PAA (polyacrylic acid) solution added, a product is subjected to freeze-drying and sterilization, and the collagen based composite dental restoration membrane material is obtained. The self-assembly of the collagen and the biomimetic mineralization are adopted, a forming process of natural teeth of a human body is simulated in the aspect of the preparation method, so that the membrane material has good biocompatibility, meanwhile, a membrane has good mechanical property and antibacterial property and an appropriate and controllable degradation rate, the raw materials are cheap and available, and the collagen based composite dental restoration membrane material can be widely applied to the field of dental restoration.
Description
Technical field
The present invention relates to collagen-based compound Oral Repair membrane material and preparation method thereof, belong to oral medical Material Field。
Background technology
Oral Repair film is by setting up one layer of biological barrier between oral soft tissue and Cranial defect, create a good Regeneration and Repair space, it can pass through optionally to stop that migration velocity cell faster enters Cranial defect district, promotes again induction oral cavity wound healing simultaneously。Obviously, good Oral Repair film should have mechanical barrier effect, vascularization, participation metabolic process and inducing action etc.。
Collagen is a kind of structural protein with biological function, accounts for the 1/3 of human body protein total amount, is the main component constituting the connective tissues such as skin, cartilage, ligament, tendon or organ。Natural type i collagen has good mechanical property and important biological property, there is biodegradable and good biocompatibility, the functions such as also very advantageous cell adhesion in tissue culture, propagation and differentiation, it has a wide range of applications value at biomedical sector。Although type i collagen has so many advantage, but it is poor to still suffer from simple collagen gel mechanical strength, has antigenicity etc., limits its application, and therefore, research worker is found various methods and improved its performance to compensate its defect。Carboxymethyl chitosan is a kind of water-solubility chitosan derivative, and having of carboxymethyl group is beneficial to later stage Ca2+The deposition of ion。Carboxymethyl chitosan also inherits the plurality of advantages such as performance such as bacteria resistance, antitumor, promotion wound healing of chitosan。Carboxymethyl chitosan after oxidation introduces aldehyde radical, can with the amino generation schiff base reaction on collagen, in-situ cross-linked, there is higher reactivity, the mechanical property of collagen-based composite film material, degradable absorbability etc. can be improved。
Self assembly is a critical nature of collagen。The basic organic frame of human body natural teeth is by NTx molecular composition, and its forming process mainly has: the synthesis of collagen stroma, extracellular assemble and biomineralization。In forming process, NTx molecule itself has first carried out a series of multilevel ordered self assembly, and its hierarchy is: the tridimensional network of tropocollagen molecule → collagen microfibrils → collagen fiber → mineralized dentin matrix。Collagen fiber provide the deposition substrate of later stage hydroxyapatite, and the non-collagen tissue at collagen fiber porose area provides the site of hydroxyapatite forming core and is arranged formation orientation, can play the effect of bridge joint hydroxyapatite and collagen。
At present, Oral Repair membrane material is mainly the simple composite of some materials。Such as, patent CN104922732A discloses a kind of oral biological film preparation method, collagen and chondroitin sulfate are configured to serosity, vacuum lyophilization is pressed into collagen composite thin film, collagen chondroitin sulfate serosity is sprayed again in two-layer collagen composite thin film, vacuum lyophilization, namely obtains collagen chondroitin sulfate compound oral biological film after high-temperature vacuum crosslinking, sterilization treatment。The preparation method that patent CN101081314B discloses the collagen/chitosan support of a kind of composite hydroxylapatite, first it be prepared for the collagen/chitosan support of crosslinking, hydroxyapatite is compound on support by the method then adopting chemical deposition, finally utilizes the method for mineralising to obtain the Composite Bone support of activity。
In said method, have the disadvantage that (1) major part collagen raw material is the hydrolyzate of tropocollagen molecule or collagen, different from the collagen fiber composition in human body natural teeth or lost collagen itself there is bioactive triple helix structure；(2) material of compound and collagen can not form mass efficient crosslinking, affect mechanical property and the degradable absorbability etc. of repair membrane material；(3) material of compound itself does not possess excellent performance, it is impossible to give repair membrane material with new more excellent performance；(4) biomimetic mineralization process is simple, does not add other elements and carries out the regulation and control of mineralising。
Summary of the invention
It is an object of the invention to provide, for oral medical Material Field, the collagen group composite material that a kind of biocompatibility is good, the forming process of human body natural teeth simulated by this membrane material in preparation method, by compound, also there is good mechanical property, bacteria resistance simultaneously and be suitable for controlled degraded and absorbed, raw material is cheap and easy to get, has a good application prospect。
It is an object of the invention to be realized by techniques below measure:
(1) preparation of oxidated carboxymethyl chitosan: join in stainless steel cauldron by the deionized water of 10 ~ 100 weight portions, then adds carboxymethyl chitosan and oxidant with the mass ratio of 1:0.1 ~ 2.5, and so as to dissolves completely。Then, lucifuge stirring reaction 10 ~ 50h at 0 ~ 20 DEG C, add the sodium chloride of 5 ~ 50 weight portions and the dehydrated alcohol of 50 ~ 1000 parts by volume, stand, by bottom liquid with the centrifugal 10 ~ 30min of 10000 ~ 15000r/min, last 3 ~ the 5d that dialyses in deionized water, namely lyophilization obtains oxidated carboxymethyl chitosan；
(2) thermal drivers NTx self assembly: NTx is dissolved in buffer so that NTx concentration is 1 ~ 5mg/ml。After the NTx solution stirred is hatched 10 ~ 24h at 37 DEG C, add oxidated carboxymethyl chitosan stirring 3 ~ 6h, then at 37 DEG C, continue hatching 10 ~ 24h, finally by standby for product lyophilization；
(3) pretreatment of collagen-based material: step (2) gained collagen-based material is immersed crosslinking 0.5 ~ 12h in cross-linking agent solution, then material is immersed at 37 DEG C the Ca (NO of 0.1 ~ 0.5mol/L3)24 ~ 24h in solution, every 12h change a Ca (NO3)2Solution, rinses with deionized water 3 times after taking-up gently；
(4) biomimetic mineralization of collagen-based material: step (3) gained collagen-based material is immersed in the SBF solution of 1 ~ 10 times at 37 DEG C, and add trace polyacrylic acid (PAA) solution, making its concentration is 20 ~ 60 μ g/ml, biomimetic mineralization 12 ~ 336h, every 12h changes the SBF solution of 1 ~ 10 times, taking-up deionized water rinses 3 times gently, freeze-dried, sterilization treatment, obtains collagen-based compound Oral Repair membrane material。
Described collagen-based compound Oral Repair membrane material and preparation method thereof, it is characterised in that described oxidant is one or both in sodium metaperiodate or sodium perchlorate。
Described collagen-based compound Oral Repair membrane material and preparation method thereof, it is characterised in that described buffer is pH value is the phosphate buffer of 7 ~ 7.5。
Described collagen-based compound Oral Repair membrane material and preparation method thereof, it is characterised in that the mass ratio of described oxidated carboxymethyl chitosan and NTx is 1 ~ 3:10。
Described collagen-based compound Oral Repair membrane material and preparation method thereof, it is characterized in that, described cross-linking agent be 1-ethyl-3-(3-DimethylAminopropyl)-carbodiimides, N-hydroxy-succinamide, genipin, procyanidin, glutaraldehyde any one or two kinds of。
Described collagen-based compound Oral Repair membrane material and preparation method thereof, it is characterised in that the mass ratio of described collagen-based material and 1 ~ 10 times of SBF solution is 1:25 ~ 300。
The collagen-based compound Oral Repair membrane material prepared by said method, its Key Performance Indicator should meet claimed below:
Outward appearance: white or slightly yellow membranoid substance, soft, without naked eyes visible foreign；
Content of beary metal :≤10 μ g/ml;
Cytotoxicity: cell-cytotoxic reaction is not more than 1 grade；
Sterility test: aseptic；
Sensitization test (STT): without tardus allergy；
Intradermoreaction is tested: constitutional stimulation index PII < 0.4。
Compared with prior art, present invention have the advantage that
(1) present invention adopts thermal drivers to promote collagen assembly, simulates the forming process of human body natural teeth, make collagen group composite material have good biocompatibility in preparation method；
(2) present invention adopts oxidated carboxymethyl chitosan to carry out composite modified to NTx, oxidated carboxymethyl chitosan produces in-situ cross-linked with NTx, significantly improving stability and the degradable absorbability of NTx, having of carboxymethyl group is beneficial to later stage Ca simultaneously2+The deposition of ion。According to Synergy, the collagen-based composite film material of the present invention also has the advantages such as bacteria resistance, non-oxidizability, promotion wound healing；
(3) present invention adopts the method that pretreatment combines with Human Physiology body fluid biomimetic mineralization, introduces and have bioactive hydroxyapatite in collagen-based material, similar to structure to the composition of human body natural teeth, is conducive to Oral Repair；
(4) present invention adds trace polyacrylic acid (PAA) solution in biomimetic mineralization process, is conducive to building in collagen-based material from nanometer to the multi-scale structure of micron, can further improve the biocompatibility of membrane material。
Detailed description of the invention
Below by enforcement, the present invention is specifically described; be necessary it is pointed out here that be; the present embodiment is served only for the present invention is further described; and it is not intended that limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of foregoing invention。
Embodiment 1
(1) preparation of oxidated carboxymethyl chitosan: join in stainless steel cauldron by the deionized water of 60 weight portions, then adds carboxymethyl chitosan and oxidant with the mass ratio of 1:1, and so as to dissolves completely。Then, lucifuge stirring reaction 48h at 20 DEG C, add the sodium chloride of 5 weight portions and the dehydrated alcohol of 600 parts by volume, stand, by bottom liquid with the centrifugal 20min of 15000r/min, finally dialyse 5d in deionized water, and namely lyophilization obtains oxidated carboxymethyl chitosan；
(2) thermal drivers NTx self assembly: NTx is dissolved in buffer so that NTx concentration is 3mg/ml。After the NTx solution stirred is hatched 20h at 37 DEG C, add oxidated carboxymethyl chitosan stirring 5h, then at 37 DEG C, continue hatching 20h, finally by standby for product lyophilization；
(3) pretreatment of collagen-based material: step (2) gained collagen-based material is immersed crosslinking 4h in 1-ethyl-3-(3-DimethylAminopropyl)-carbodiimides/N-hydroxy-succinamide solution, then material is immersed at 37 DEG C the Ca (NO of 0.2mol/L3)26h in solution, rinses with deionized water 3 times after taking-up gently；
(4) biomimetic mineralization of collagen-based material: step (3) gained collagen-based material is immersed in the SBF solution of 5 times at 37 DEG C, and add trace polyacrylic acid (PAA) solution, making its concentration is 30 μ g/ml, biomimetic mineralization 168h, every 12h changes the SBF solution of 5 times, taking-up deionized water rinses 3 times gently, freeze-dried, sterilization treatment, obtains collagen-based compound Oral Repair membrane material。
Embodiment 2
(1) preparation of oxidated carboxymethyl chitosan: join in stainless steel cauldron by the deionized water of 80 weight portions, then adds carboxymethyl chitosan and oxidant with the mass ratio of 1:0.5, and so as to dissolves completely。Then, lucifuge stirring reaction 24h at 10 DEG C, add the sodium chloride of 10 weight portions and the dehydrated alcohol of 500 parts by volume, stand, by bottom liquid with the centrifugal 20min of 10000r/min, finally dialyse 5d in deionized water, and namely lyophilization obtains oxidated carboxymethyl chitosan；
(2) thermal drivers NTx self assembly: NTx is dissolved in buffer so that NTx concentration is 5mg/ml。After the NTx solution stirred is hatched 20h at 37 DEG C, add oxidated carboxymethyl chitosan stirring 6h, then at 37 DEG C, continue hatching 20h, finally by standby for product lyophilization；
(3) pretreatment of collagen-based material: step (2) gained collagen-based material is immersed crosslinking 4h in glutaraldehyde solution, then material is immersed at 37 DEG C the Ca (NO of 0.1mol/L3)216h in solution, every 12h change a Ca (NO3)2Solution, rinses with deionized water 3 times after taking-up gently；
(4) biomimetic mineralization of collagen-based material: step (3) gained collagen-based material is immersed in the SBF solution of 1.5 times at 37 DEG C, and add trace polyacrylic acid (PAA) solution, making its concentration is 50 μ g/ml, biomimetic mineralization 240h, every 12h changes the SBF solution of 1.5 times, taking-up deionized water rinses 3 times gently, freeze-dried, sterilization treatment, obtains collagen-based compound Oral Repair membrane material。
Embodiment 3
(1) preparation of oxidated carboxymethyl chitosan: join in stainless steel cauldron by the deionized water of 50 weight portions, then adds carboxymethyl chitosan and oxidant with the mass ratio of 1:1.5, and so as to dissolves completely。Then, lucifuge stirring reaction 12h at 4 DEG C, add the sodium chloride of 15 weight portions and the dehydrated alcohol of 700 parts by volume, stand, by bottom liquid with the centrifugal 15min of 15000r/min, finally dialyse 5d in deionized water, and namely lyophilization obtains oxidated carboxymethyl chitosan；
(2) thermal drivers NTx self assembly: NTx is dissolved in buffer so that NTx concentration is 1mg/ml。After the NTx solution stirred is hatched 20h at 37 DEG C, add oxidated carboxymethyl chitosan stirring 5h, then at 37 DEG C, continue hatching 20h, finally by standby for product lyophilization；
(3) pretreatment of collagen-based material: step (2) gained collagen-based material is immersed crosslinking 6h in genipin solution, then material is immersed at 37 DEG C the Ca (NO of 0.1mol/L3)210h in solution, rinses with deionized water 3 times after taking-up gently；
(4) biomimetic mineralization of collagen-based material: step (3) gained collagen-based material is immersed in the SBF solution of 2 times at 37 DEG C, and add trace polyacrylic acid (PAA) solution, making its concentration is 40 μ g/ml, biomimetic mineralization 288h, every 12h changes the SBF solution of 2 times, taking-up deionized water rinses 3 times gently, freeze-dried, sterilization treatment, obtains collagen-based compound Oral Repair membrane material。
Claims (7)
1. collagen-based compound Oral Repair membrane material and preparation method thereof, its Key Performance Indicator is as follows:
Outward appearance: white or slightly yellow membranoid substance, soft, without naked eyes visible foreign；
Content of beary metal :≤10 μ g/ml;
Cytotoxicity: cell-cytotoxic reaction is not more than 1 grade；
Sterility test: aseptic；
Sensitization test (STT): without tardus allergy；
Intradermoreaction is tested: constitutional stimulation index PII < 0.4。
2. the collagen-based compound Oral Repair membrane material described in claim 1, it is characterised in that preparation method comprises the following steps:
(1) preparation of oxidated carboxymethyl chitosan: the deionized water of 10 ~ 100 weight portions is joined in stainless steel cauldron, then carboxymethyl chitosan and oxidant are added with the mass ratio of 1:0.1 ~ 2.5, and so as to dissolve completely, then, lucifuge stirring reaction 10 ~ 50h at 0 ~ 20 DEG C, add the sodium chloride of 5 ~ 50 weight portions and the dehydrated alcohol of 50 ~ 1000 parts by volume, stand, by bottom liquid with the centrifugal 10 ~ 30min of 10000 ~ 15000r/min, last 3 ~ the 5d that dialyses in deionized water, namely lyophilization obtains oxidated carboxymethyl chitosan；
(2) thermal drivers NTx self assembly: NTx is dissolved in buffer, making NTx concentration is 1 ~ 5mg/ml, after the NTx solution stirred is hatched 10 ~ 24h at 37 DEG C, add oxidated carboxymethyl chitosan stirring 3 ~ 6h, hatching 10 ~ 24h is continued again, finally by standby for product lyophilization at 37 DEG C；
(3) pretreatment of collagen-based material: step (2) gained collagen-based material is immersed crosslinking 0.5 ~ 12h in cross-linking agent solution, then material is immersed at 37 DEG C the Ca (NO of 0.1 ~ 0.5mol/L3)24 ~ 24h in solution, every 12h change a Ca (NO3)2Solution, rinses with deionized water 3 times after taking-up gently；
(4) biomimetic mineralization of collagen-based material: step (3) gained collagen-based material is immersed in the SBF solution of 1 ~ 10 times at 37 DEG C, and add trace polyacrylic acid (PAA) solution, making its concentration is 20 ~ 60 μ g/ml, biomimetic mineralization 12 ~ 336h, every 12h changes the SBF solution of 1 ~ 10 times, taking-up deionized water rinses 3 times gently, freeze-dried, sterilization treatment, obtains collagen-based compound Oral Repair membrane material。
3. collagen-based compound Oral Repair membrane material described in claim 2 and preparation method thereof, it is characterised in that described oxidant is one or both in sodium metaperiodate or sodium perchlorate。
4. collagen-based compound Oral Repair membrane material described in claim 2 and preparation method thereof, it is characterised in that described buffer is pH value is the phosphate buffer of 7 ~ 7.5。
5. collagen-based compound Oral Repair membrane material described in claim 2 and preparation method thereof, it is characterised in that the mass ratio of described oxidated carboxymethyl chitosan and NTx is 1 ~ 3:10。
6. collagen-based compound Oral Repair membrane material described in claim 2 and preparation method thereof, it is characterized in that, described cross-linking agent be 1-ethyl-3-(3-DimethylAminopropyl)-carbodiimides, N-hydroxy-succinamide, genipin, procyanidin, glutaraldehyde any one or two kinds of。
7. collagen-based compound Oral Repair membrane material described in claim 2 and preparation method thereof, it is characterised in that the mass ratio of described collagen-based material and 1 ~ 10 times of SBF solution is 1:25 ~ 300。
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106237386A (en) * | 2016-08-29 | 2016-12-21 | 东华大学 | A kind of natural fibroin base macropore support for bone defect healing and preparation method thereof |
| CN112206359A (en) * | 2020-08-31 | 2021-01-12 | 中国人民解放军空军军医大学 | Self-mineralized collagen membrane, preparation method and application |
| CN112267169A (en) * | 2020-10-22 | 2021-01-26 | 湖南翰坤实业有限公司 | Degradable toothbrush main material with self-cleaning function |
| CN114425103A (en) * | 2022-04-06 | 2022-05-03 | 中国科学院苏州纳米技术与纳米仿生研究所 | Bionic biogel and preparation method and application thereof |
| CN115137882A (en) * | 2022-08-03 | 2022-10-04 | 四川大学 | Method for modularly assembling collagen membrane by utilizing LB (Luria Brouss) technology |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006068972A2 (en) * | 2004-12-21 | 2006-06-29 | Ethicon, Inc. | Tissue engineering devices for the repair and regeneration of tissue |
| CN104013995A (en) * | 2014-06-26 | 2014-09-03 | 四川大学 | Oxidation chitosan graft modified porcine dermal collagen micro-nano fiber membrane and preparation method thereof |
| CN104922732A (en) * | 2014-03-19 | 2015-09-23 | 北京天新福医疗器材有限公司 | Preparation method of oral biofilm |
-
2016
- 2016-03-09 CN CN201610130834.3A patent/CN105688288B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006068972A2 (en) * | 2004-12-21 | 2006-06-29 | Ethicon, Inc. | Tissue engineering devices for the repair and regeneration of tissue |
| CN104922732A (en) * | 2014-03-19 | 2015-09-23 | 北京天新福医疗器材有限公司 | Preparation method of oral biofilm |
| CN104013995A (en) * | 2014-06-26 | 2014-09-03 | 四川大学 | Oxidation chitosan graft modified porcine dermal collagen micro-nano fiber membrane and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| XINHUA LIU等: ""Feasibility study of the natural derived chitosan dialdehyde forchemical modification of collagen"", 《INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES》 * |
| 叶勇等: ""胶原基膜材料在牙组织引导中的应用"", 《中国皮革》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106237386A (en) * | 2016-08-29 | 2016-12-21 | 东华大学 | A kind of natural fibroin base macropore support for bone defect healing and preparation method thereof |
| CN112206359A (en) * | 2020-08-31 | 2021-01-12 | 中国人民解放军空军军医大学 | Self-mineralized collagen membrane, preparation method and application |
| CN112267169A (en) * | 2020-10-22 | 2021-01-26 | 湖南翰坤实业有限公司 | Degradable toothbrush main material with self-cleaning function |
| CN114425103A (en) * | 2022-04-06 | 2022-05-03 | 中国科学院苏州纳米技术与纳米仿生研究所 | Bionic biogel and preparation method and application thereof |
| CN115137882A (en) * | 2022-08-03 | 2022-10-04 | 四川大学 | Method for modularly assembling collagen membrane by utilizing LB (Luria Brouss) technology |
| CN115137882B (en) * | 2022-08-03 | 2023-07-21 | 四川大学 | Method for modularly assembling collagen membrane by utilizing LB technology |
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