CN106822996A - The method that implant surface builds BMP/PLA controlled-release coatings - Google Patents
The method that implant surface builds BMP/PLA controlled-release coatings Download PDFInfo
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- CN106822996A CN106822996A CN201611209510.5A CN201611209510A CN106822996A CN 106822996 A CN106822996 A CN 106822996A CN 201611209510 A CN201611209510 A CN 201611209510A CN 106822996 A CN106822996 A CN 106822996A
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/28—Materials for coating prostheses
- A61L27/34—Macromolecular materials
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- A—HUMAN NECESSITIES
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/06—Titanium or titanium alloys
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/54—Biologically active materials, e.g. therapeutic substances
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/26—Acidic compositions for etching refractory metals
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
- A61L2300/252—Polypeptides, proteins, e.g. glycoproteins, lipoproteins, cytokines
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/412—Tissue-regenerating or healing or proliferative agents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/60—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special physical form
- A61L2300/602—Type of release, e.g. controlled, sustained, slow
- A61L2300/604—Biodegradation
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/18—Modification of implant surfaces in order to improve biocompatibility, cell growth, fixation of biomolecules, e.g. plasma treatment
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61L2420/00—Materials or methods for coatings medical devices
- A61L2420/02—Methods for coating medical devices
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2420/00—Materials or methods for coatings medical devices
- A61L2420/06—Coatings containing a mixture of two or more compounds
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- A—HUMAN NECESSITIES
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- A61L2420/00—Materials or methods for coatings medical devices
- A61L2420/08—Coatings comprising two or more layers
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/12—Materials or treatment for tissue regeneration for dental implants or prostheses
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Abstract
The invention discloses a kind of method that implant surface builds BMP/PLA controlled-release coatings.75 μm of TiO of the cleaned implant surface that will polish2Surface acid etching processing is carried out after particle sandblasting in etching agent, then coats PLA and BMP 2 successively after alkali heat-treatment.The method of the present invention effectively increases the roughness of implant surface and surface can, the activity on reinforcing material surface, increased the load capacity and PLA of bmp protein and the bond strength of implant surface, simultaneously using the support performance of PLA, build BMP/PLA coatings, the slow release of BMP 2 is adjusted by PLA auto-degradations, promotes the process of bone healing of planting body and bone tissue.
Description
Technical field
The invention belongs to bio-medical implant field, and in particular to a kind of implant surface builds BMP/PLA sustained releases and applies
The method of layer.
Background technology
Titanium has the advantages that good biocompatibility, mechanical property and machining potentiality, currently as tooth kind
Plant material material is in department of stomatology extensive use.However, titanium has biologically inert in itself, after being implanted body, trigger healing time long, raw
Thing activity is low, induction Bone Defect Repari ability the problems such as.In order to improve its bioactivity, at present mostly using plasma spraying, from
The microphysics pattern and chemical composition of the technological transformation implant surfaces such as sub- sputtering, electrophoresis, microwave sintering, being formed has preferably
The rough porous surface of biocompatibility, and the bond strength of plantation physical culture bone tissue is improve, but such planting body and bone group
It is still physical combination between knitting, but without osteoinductive energy, the biocompatibility with surrounding tissue is low, clinically tooth-planting
The cycle for the treatment of is considerably long, and the life to patient brings inconvenience.In recent years, in the microphysics shape of transformation implant surface
On the basis of looks, its surface prepare or coating bioactive molecule coating or film, reach promote Gegenbaur's cell propagation and
Break up to promote the formation of new bone, shorten treatment cycle.
Bone morphogenetic protein (BMP) is efficient bone-inducing factor, can be filled by inducing undifferentiated in Bone Defect Repari early stage
Cell plastid and marrow stromal cell is irreversible is divided into cartilage cell and Gegenbaur's cell and induces new bone formation.At present, BMP is made
It is short in physiological conditions for the research that bioactive molecule introduces implant surface is a lot, but because the amount of BMP absorption is very limited
Degraded is fast released or absorbed in time, therefore cannot be in the local effect for playing and persistently irritating with induced osteogenesis, it is biological
Activity is difficult to be not fully exerted.
The content of the invention
In view of above-mentioned problems of the prior art, it is an object of the invention to provide one kind there is BMP-2 to be sustained work(
The preparation method of the composite coating of energy.
Technical scheme is as follows:
A kind of method that implant surface builds BMP/PLA controlled-release coatings, comprises the following steps:
(1) titanium metal implants surface is polished step by step with 200,300,600 and 2000 mesh sand paper, is cleaned, in 60 DEG C of bakings
It is dry;
(2) with 75 μm of TiO2Particle, blasting treatment is carried out by nozzle to implant surface;
(3) planting body after blasting treatment is placed in mixing etching agent of the hydrofluoric acid with hydrochloric acid composition carries out surface etch
Treatment, takes out planting body and is cleaned by ultrasonic, natural drying at room temperature;
(4) surface etching treatment, dried planting body will be carried out and will be placed in 60 DEG C, 5mol/L NaOH solutions incubation 24-
48h, after water ultrasonic cleaning, drying, 1-2h is processed at 600 DEG C;
(5) planting body after high-temperature process is sterilized 24-48h under ultraviolet light;
(6) PLA is dissolved in CH3Cl3, add distilled water to be made emulsion, the kind that step (5) middle-ultraviolet lamp is disinfected
Implant, aseptically immerses in PLA emulsion, is placed in ventilation evaporation water and solvent, repeats aforesaid operations for several times,
Obtain PLA coating planting body;
(7) in PLA coating planting body immersion 1-3mg/mL BMP-2 solution, 24-48h is placed at 4 DEG C, vacuum is cold
It is lyophilized dry.
Further, in above-mentioned technical proposal of the invention, in step (2), described blasting treatment condition is:Pressure
Contracting air pressure is 0.3-0.4MPa, and nozzle is 5-10cm with a distance from implant surface, and injecting time is 2-10s.
Further, in above-mentioned technical proposal of the invention, in step (3), described mixing etching agent is 47%
HF and 38% HCl with volume ratio 1:The mixed liquor of 1 mixing.
Further, in above-mentioned technical proposal of the invention, in step (3), described surface etching treatment temperature
It it is 60 DEG C, the etching processing time is 10-20min.
Further, in above-mentioned technical proposal of the invention, in step (7), BMP-2 solution one was changed every 12 hours
It is secondary.
Further, in above-mentioned technical proposal of the invention, the preparation process of the BMP-2 solution is:BMP-2 is molten
Solution is in the PBS that pH value is 7.0 or is dissolved in SBF solution.
PLA (polylacticacid, PLA) is a kind of important polyester biodegradable high molecular polymer, its master
Chain contains the unstable chemical bond for being easily hydrolyzed or digesting, and so as to hydrolyze de- ester in vivo, lactic acid monomer is generated, in body
Pyruvic acid is generated in the presence of interior lactic dehydrogenase, tricarboxylic acid cycle is participated in as energetic supersession material, end-product is Н2О and
СО2, transpulmonary, kidney, skin excretion.PLA has good mechanical performance and a biocompatibility, its three-dimensional porous structure and
Biodegradable becomes the important slow release stent material of the growth factors such as BMP
The present invention is combined and uses kinds of surface treatment technology, and the surface of metal titanium to planting body is surface-treated, effectively
The roughness and surface energy, the activity on reinforcing material surface of implant surface are improve, the load capacity of bmp protein is increased and is gathered
Lactic acid, while using the support performance of PLA, building BMP-2/PLA coatings, is dropped to the bond strength on surface by PLA itself
The slow release of solution regulation BMP-2, promotes the process of bone healing of planting body and bone tissue.BMP-2/PLA coating surfaces are not
Disconnected to update, histocyte adhesion growth promotes the integration of planting body and bone tissue, shortens treatment cycle.
Specific embodiment
Following non-limiting examples can make one of ordinary skill in the art be more fully understood the present invention, but not with
Any mode limits the present invention.In following embodiments, unless otherwise specified, the experimental technique for being used is conventional method, institute
Chemically company can be bought with reagent etc..
Embodiment 1
A kind of method that implant surface builds BMP/PLA controlled-release coatings, comprises the following steps:
(1) titanium metal implants surface is polished step by step with 200,300,600 and 2000 mesh sand paper, is cleaned, in 60 DEG C of bakings
It is dry;
(2) with 75 μm of TiO2Particle, blasting treatment, described blasting treatment condition are carried out to implant surface by nozzle
For:Compressed air pressure is 0.3-0.4MPa, and nozzle is 5cm with a distance from implant surface, and injecting time is 5s;
(3) planting body after blasting treatment is placed in mixing etching agent of the hydrofluoric acid with hydrochloric acid composition carries out surface etch
Treatment, etching processing temperature is 60 DEG C, and the etching processing time is 10min, takes out planting body and is cleaned by ultrasonic, natural drying at room temperature;
(4) surface etching treatment, dried planting body will be carried out and will be placed in 60 DEG C, 5mol/L NaOH solutions incubation 24h,
After being cleaned by ultrasonic with water, 1h is processed at 600 DEG C after drying;
(5) planting body after high-temperature process is sterilized 24h under ultraviolet light;
(6) PLA is dissolved in CH3Cl3, add distilled water to be made emulsion, the kind that step (5) middle-ultraviolet lamp is disinfected
Implant, aseptically immerses in PLA emulsion, is placed in ventilation evaporation water and solvent, repeats aforesaid operations for several times,
Obtain PLA coating planting body;
(7) in PLA coating planting body immersion 1mg/mL BMP-2 solution, 24h is placed at 4 DEG C, vacuum refrigeration is done
It is dry, changed BMP-2 solution once every 12 hours;
Wherein, in step (3), described mixing etching agent is 47% HF and 38% HCl is with volume ratio 1:1 mixing
Mixed liquor;BMP-2 is dissolved in step (7) in the SBP solution that pH value is 7.0, obtains BMP-2 solution.
The thickness of composite coating is 10.8 μm, disengages the amount of BMP-2 in vitro with ELISA method detection composite coating, determines knot
Fruit display, after coating soaks 4 weeks in PBS solution, has discharged the 75% of gross weight.
Embodiment 2
A kind of method that implant surface builds BMP/PLA controlled-release coatings, comprises the following steps:
(1) titanium metal implants surface is polished step by step with 200,300,600 and 2000 mesh sand paper, is cleaned, in 60 DEG C of bakings
It is dry;
(2) with 75 μm of TiO2Particle, blasting treatment, described blasting treatment condition are carried out to implant surface by nozzle
For:Compressed air pressure is 0.3-0.4MPa, and nozzle is 10cm with a distance from implant surface, and injecting time is 10s;
(3) planting body after sandblasting is placed in mixing etching agent of the hydrofluoric acid with hydrochloric acid composition is carried out at surface etch
Reason, etching processing temperature is 60 DEG C, and the etching processing time is 20min, takes out planting body and is cleaned by ultrasonic, natural drying at room temperature;
(4) surface etching treatment, dried planting body will be carried out and will be placed in 60 DEG C, 5mol/L NaOH solutions incubation 48h,
After being cleaned by ultrasonic with water, 1h is processed at 600 DEG C after drying;
(5) planting body after high-temperature process is sterilized 48h under ultraviolet light;
(6) PLA is dissolved in CH3Cl3, add distilled water to be made emulsion, the kind that step (5) middle-ultraviolet lamp is disinfected
Implant, aseptically immerses in PLA emulsion, is placed in ventilation evaporation water and solvent, repeats aforesaid operations for several times,
Obtain PLA coating planting body;
(7) in PLA coating planting body immersion 3mg/mL BMP-2 solution, 48h is placed at 4 DEG C, vacuum refrigeration is done
It is dry, changed BMP-2 solution once every 12 hours;
Wherein, in step (3), described mixing etching agent is 47% HF and 38% HCl is with volume ratio 1:1 mixing
Mixed liquor;BMP-2 is dissolved in step (7) in the PBS that pH value is 7.0.
The thickness of composite coating is 12.1 μm, disengages the amount of BMP-2 in vitro with ELISA method detection composite coating, determines knot
Fruit display, after coating soaks 4 weeks in PBS solution, has discharged the 80% of gross weight.
Claims (6)
1. a kind of method that implant surface builds BMP/PLA controlled-release coatings, comprises the following steps:
(1) titanium metal implants surface is polished step by step with 200,300,600 and 2000 mesh sand paper, is cleaned, in 60 DEG C of drying;
(2) with 75 μm of TiO2Particle, blasting treatment is carried out by nozzle to implant surface;
(3) the good planting body of blasting treatment is placed in mixing etching agent of the hydrofluoric acid with hydrochloric acid composition is carried out at surface etch
Reason, takes out planting body and is cleaned by ultrasonic, natural drying at room temperature;
(4) dried planting body is placed in 60 DEG C, 5mol/L NaOH solutions incubation 24-48h, after being cleaned by ultrasonic with water, is dried
1-2h is processed at 600 DEG C afterwards;
(5) planting body after high-temperature process is sterilized 24-48h under ultraviolet light;
(6) PLA is dissolved in CH3Cl3, add distilled water to be made emulsion, the plantation that step (5) middle-ultraviolet lamp is disinfected
Body, aseptically immerses in PLA emulsion, is placed in ventilation evaporation water and solvent, repeats aforesaid operations for several times, obtains
PLA coating planting body;
(7) in PLA coating planting body immersion 1-3mg/mL BMP-2 solution, 24-48h is placed at 4 DEG C, vacuum refrigeration is done
It is dry.
2. method according to claim 1, it is characterised in that in step (2), described blasting treatment condition is:Pressure
Contracting air pressure is 0.3-0.4MPa, and nozzle is 5-10cm with a distance from implant surface, and injecting time is 2-10s.
3. method according to claim 1, it is characterised in that in step (3), described mixing etching agent is 47%
Hydrofluoric acid and 38% hydrochloric acid are with volume ratio 1:The mixed liquor of 1 mixing.
4. method according to claim 1, it is characterised in that in step (3), described surface etching treatment temperature is
60 DEG C, the etching processing time is 10-20min.
5. method according to claim 1, it is characterised in that in step (7), BMP-2 solution one was changed every 12 hours
It is secondary.
6. method according to claim 1, it is characterised in that the preparation process of the BMP-2 solution is:BMP-2 is molten
Solution is in the PBS that pH value is 7.0 or is dissolved in SBF solution.
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KR20140124550A (en) * | 2013-04-17 | 2014-10-27 | 한국기계연구원 | Method for manufacturing coating layer for surface treatment of implant, coating layer for surface treatment of implant manufactured thereby, and implant including the same |
CN104451685A (en) * | 2014-12-30 | 2015-03-25 | 哈尔滨工业大学 | Preparation method for forming second-level porous active surface structure on titanium material surface through mixed alkali |
CN105537589A (en) * | 2016-01-28 | 2016-05-04 | 佛山市安齿生物科技有限公司 | Surface treatment method for SLM molded titanium implant |
KR20160056345A (en) * | 2014-11-10 | 2016-05-20 | 주식회사 레모넥스 | Implant containing nanocarrier for implanting into a living body and the method for preparing thereof |
CN105662621A (en) * | 2016-02-23 | 2016-06-15 | 浙江工业大学 | Porous dental implant capable of carrying drug sustained release system and manufacturing method thereof |
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2016
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CN201119919Y (en) * | 2007-11-12 | 2008-09-24 | 耿建平 | Dental implant with bone induction liveness coating |
CN101234201A (en) * | 2008-01-24 | 2008-08-06 | 上海交通大学 | High molecule impregnation implantation sustained-release drug delivering system and preparation thereof |
KR20140124550A (en) * | 2013-04-17 | 2014-10-27 | 한국기계연구원 | Method for manufacturing coating layer for surface treatment of implant, coating layer for surface treatment of implant manufactured thereby, and implant including the same |
KR20160056345A (en) * | 2014-11-10 | 2016-05-20 | 주식회사 레모넥스 | Implant containing nanocarrier for implanting into a living body and the method for preparing thereof |
CN104451685A (en) * | 2014-12-30 | 2015-03-25 | 哈尔滨工业大学 | Preparation method for forming second-level porous active surface structure on titanium material surface through mixed alkali |
CN105537589A (en) * | 2016-01-28 | 2016-05-04 | 佛山市安齿生物科技有限公司 | Surface treatment method for SLM molded titanium implant |
CN105662621A (en) * | 2016-02-23 | 2016-06-15 | 浙江工业大学 | Porous dental implant capable of carrying drug sustained release system and manufacturing method thereof |
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