CN106512083B - A kind of preparation method of medical titanium alloy - Google Patents
A kind of preparation method of medical titanium alloy Download PDFInfo
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- CN106512083B CN106512083B CN201610901549.7A CN201610901549A CN106512083B CN 106512083 B CN106512083 B CN 106512083B CN 201610901549 A CN201610901549 A CN 201610901549A CN 106512083 B CN106512083 B CN 106512083B
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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
- A61L27/14—Macromolecular materials
- A61L27/18—Macromolecular materials obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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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
- A61L27/14—Macromolecular materials
- A61L27/22—Polypeptides or derivatives thereof, e.g. degradation products
- A61L27/227—Other specific proteins or polypeptides not covered by A61L27/222, A61L27/225 or A61L27/24
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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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- 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
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
- A61L2300/406—Antibiotics
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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
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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
- A61L2300/62—Encapsulated active agents, e.g. emulsified droplets
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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
- 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
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
Abstract
The invention discloses a kind of preparation methods of medical titanium alloy, it is uniform with double emulsion methods preparation particle diameter distribution, PLGA (polylactide glycolic acid copolymer) medicine-carried nano particles of reunion lesser extent, make it have good bioactivity and anti-microbial property, it then is raw material with the titanium alloy that hydro-thermal method is handled, it is connected into APTES (3- aminopropyl triethoxysilane) figure layer with condensing reflux method, PLGA (polylactide glycolic acid copolymer) medicine-carried nano particles are promoted preferably to be connected to titanium-based surface, make it have good rush osteogenic and with certain sterilizing function, the present invention prepare resulting medical titanium alloy in the application when organism occur medical treatment infection when, the ester bond on PLGA (polylactide glycolic acid copolymer) medicine-carried nano particles surface is opened, drug can be with PLGA (polylactic acid Co-glycolic acid) degradation gradually release, inhibit the growth of bacterium, but also promote the proliferation and differentiation of osteoblast.
Description
Technical field
The present invention relates to material science and technical field of nano material, in particular to a kind of preparation side of medical titanium alloy
Method.
Background technique
Bio-medical material is for the purpose of medical treatment, for contacting with living tissue to form functional no life material
Material, including the material with biocompatibility or biological degradability, it must have good biocompatibility, good biology
Stability or controllable degradation absorbent properties, with organize the formation of the biological bioactivity being bonded, enough intensity and toughness or
With the mechanical property of Organization Matching and good processing, sterilizing and clinical manipulation performance etc..Titanium base biomaterial due to
With low modulus, good corrosion resistance and excellent describing property of biology are widely used in bone surgery.
Titanium is planted in surgical operation, and there is also some problems, such as hold in the course of surgery at postoperative a period of time implantation
Bacterium infection easily occurs.It is well known that PLGA (polylactide glycolic acid copolymer) material has unique mechanical performance, properly
Degradation rate, good biocompatibility.Recent years, PLGA (polylactide glycolic acid copolymer) material are frequently used to wrap
Wrapping up in drug discharges drug for a long time, carries out second operation after avoiding bone collection post-surgical infection.Compared to PLGA (poly- cream
Sour co-glycolic acid) film, PLGA (polylactide glycolic acid copolymer) nanoparticle can effectively wrap up medicine
Agent protects them, and increases the stability of drug.Therefore drug can gradually be released with the slow degradation of outside polymer matrix
It is put into the proliferation for inhibiting bacterium in blood.
Vancomycin is a kind of glycopeptide antibiotics, can effectively inhibit gram-positive bacteria, such as Staphylococcus aureus
Bacterium.Methicillin-resistant staphylococcus coccus can also be eradicated simultaneously.So vancomycin can be prevented effectively on metal implant
Bacterium infection.
How the characteristic of above-mentioned each substance to be combined together, it is each research people that preparation, which is more suitable for the material of medical treatment,
The problem of member's joint exploration.
Summary of the invention
To solve the above problems, the present invention provides a kind of preparation method of medical titanium alloy, to prepare both with good
Good bioactivity, and the titanium-based metal bio-medical material with antibiotic property.
The technical solution of the present invention is as follows: a kind of 1, preparation method of medical titanium alloy, it is characterised in that include the following steps:
Step 1, the preparation of particle:
1) 50-70mgPLGA (polylactide glycolic acid copolymer), 6-7mg pluronic F-68 are dissolved in 2ml dichloromethane
Alkane forms mixture, and the mixture sonic oscillation 8-12min is obtained PLGA (polylactide glycolic acid copolymer) solution；
4) 90-110mg antibiotic is completely dissolved in 0.4-0.6mL deionized water and forms antibiotic solution, it will be described anti-
Raw element solution is added in the PLGA (polylactide glycolic acid copolymer) solution, and turn upside down jog, makes PLGA (polylactic acid
Co-glycolic acid) solution sufficiently wraps up antibiotic molecule and forms colostric fluid, then the 25mg/ of 5-6mL is added into colostric fluid
Sonic oscillation 8-12min after the poly-vinyl alcohol solution of mL, the 25mg/mL polyvinyl alcohol that 34-35mL is slowly injected into after oscillation are molten
Final mixture is obtained in liquid；The final mixture 18-22h described in magnetic stirring apparatus gentle agitation again, until obtaining generating has
The reaction mixture of white powder particle；
5) reaction mixture is fitted into centrifuge tube and does centrifugal treating, isolate solid part, described solid part spends
The processing of ionized water centrifuge washing, treated, and solid part vacuum freeze drying obtains required particle；
Step 2, the preparation of amino group titanium alloy:
1) the polished titanium alloy of physics is immersed into volume ratio hydrofluoric acid (dense): nitric acid (1mol/mL): deionized water=
Chemical polishing 1-3min in the mix acid liquor of 1:4:5, then drying is washed with deionized, titanium alloy is then put into 100ml's
In reaction kettle and by the one side of physics polishing and chemical polishing upward, then in kettle the sodium hydroxide of 4mol/mL is added
Solution 50-70mL reacts 80-100min at 70-90 DEG C, cleans titanium alloy after the completion；
2) it prepares using toluene as APTES (3- aminopropyl triethoxysilane) solution of solvent, titanium alloy is soaked in institute
It states in APTES (3- aminopropyl triethoxysilane) solution, at 50-70 DEG C, is condensed back 12h, after titanium alloy takes out, then uses
Acetone impregnates titanium alloy for 24 hours, is cleaned and dried, obtains amino group titanium alloy；
Step 3, the combination of amino group titanium alloy and particle:
Amino group titanium alloy described in particle and step 2 described in step 1 is put into the deionized water of 10-30mL,
The carbodiimides of 0.2-0.8mL is added, reacts 3-5h, obtains connecing particle group titanium alloy, i.e. medical titanium alloy.
The antibiotic is one of vancomycin, Teicoplanin Targocin.
The 1 of the step 1) described in sonic oscillation frequency be 30-50Hz.
The 3 of the step 1) described in centrifugal treating be 5000r/min revolving speed be centrifuged 20-40min.
The 3 of the step 1) described in solid part deionized water centrifuge washing processing, 3 times repeatedly.
The 2 of the step 2) described in using toluene as in APTES (3- aminopropyl triethoxysilane) solution of solvent
The volume ratio of APTES (3- aminopropyl triethoxysilane) is 3%-8%.
Medical titanium made from a kind of medical titanium alloy preparation method as described in any claim in claim 1-6 is closed
Gold.
Technical effect of the invention are as follows:
The present invention provides a kind of preparation method of medical titanium alloy, not only has good bioactivity to prepare, but also tool
There is the titanium-based metal bio-medical material of antibiotic property.
In the present invention with double emulsion methods preparation particle diameter distributions uniformly, PLGA (the polylactic second of reunion lesser extent
Acid copolymer) medicine-carried nano particles, good bioactivity and anti-microbial property are made it have, is then closed with the titanium that hydro-thermal method is handled
Gold is raw material, it is connected APTES (3- aminopropyl triethoxysilane) figure layer with condensing reflux method, promotes PLGA (poly- cream
Sour co-glycolic acid) medicine-carried nano particles are preferably connected to titanium-based surface, and it makes it have and good promote osteogenic and have one
Fixed sterilizing function.
In preparation method of the present invention, synthesis carries the side of medicine PLGA (polylactide glycolic acid copolymer) nanoparticle
Method is simple and convenient, and equipment investment is few, and consumption resource is few, and enforcement difficulty is small, prepares resulting medical titanium alloy and works as life in the application
When medical treatment infection occurs for object, the ester bond on PLGA (polylactide glycolic acid copolymer) medicine-carried nano particles surface is opened, drug
It can gradually be released with the degradation of PLGA (polylactide glycolic acid copolymer), inhibit the growth of bacterium, but also promote
The proliferation and differentiation of osteoblast.
Detailed description of the invention
With reference to the accompanying drawing and embodiment the present invention is described in further detail:
Fig. 1-1 is the FE-SEM figure of alkali heat in embodiment 1.
Fig. 1-2 is the FE-SEM figure of amino in embodiment 1.
Fig. 1-3 is the FE-SEM figure that particle group is connect in embodiment 1.
Fig. 1-4 is pure titanium surface bacteria SEM figure in embodiment 1.
Fig. 1-5 is that particle group titanium alloy surface bacterium SEM figure is connect in embodiment 1.
Fig. 2 be embodiment 1 in particle different pH value different times antimicrobial efficiency.
Fig. 3-1 is that pure titanium superficial cell grows fluorogram in embodiment 1.
Fig. 3-2 is that amino group titanium alloy surface cell grows fluorogram in embodiment 1.
Fig. 3-3 is to connect particle group titanium alloy surface cell in embodiment 1 to grow fluorogram.
Specific embodiment
To be best understood from the present invention, the present invention is done further be described in detail with reference to the accompanying drawings and examples.
Pluronic F-68 of the present invention is a kind of polyoxypropylene hydrophobic by middle part (more (propylene oxides)) chain side
Face connects the nonionic formula triblock copolymer that two sections of hydrophilic polyoxyethylenes (more (ethylene oxides)) are constituted.
Embodiment 1:
(1) by 60mgPLGA (polylactide glycolic acid copolymer), 6.5mg pluronic F-68 is dissolved in 2ml methylene chloride,
40Hz sonic oscillation 10min, then 100mg antibiotic is completely dissolved in 0.5mL deionized water, antibiotic solution is added later
In PLGA (polylactide glycolic acid copolymer) solution, turn upside down jog, keeps PLGA (polylactide glycolic acid copolymer) molten
The abundant packaging medicine of liquid forms colostric fluid, then the poly-vinyl alcohol solution of the 25mg/mL of 5.5mL is added into colostric fluid, and 40Hz is super
Mixed liquor is slowly injected into the 25mg/mL poly-vinyl alcohol solution of 34.5mL after oscillation, uses magnetic stirring apparatus by sound oscillation 10min
Gentle agitation 20h, final solution lower layer obtain the powder white particles similar to salt.This solution is fitted into centrifuge tube, with
The revolving speed of 5000r/min is centrifuged 30min, is washed with deionized water, is centrifuged 3 times, collects particle, vacuum freeze drying.
(2) the polished titanium alloy of physics is put into hydrofluoric acid (dense): nitric acid (1mol/mL): deionized water=1:4:5
Mix acid liquor in chemical polishing 2min, deionized water washs drying, then this titanium alloy is put into the reaction kettle of 100ml, thrown
Upward, then the sodium hydroxide solution 60mL of configured good 4mol/mL is added in kettle in the one side of light, reacts at 80 DEG C
90min.Cleaning sample after the completion.It prepares by solvent volume of toluene than the APTES (3- aminopropyl triethoxysilane) for 5%
Titanium alloy is put into solution by solution, at 60 DEG C, is condensed back 12h, then impregnated titanium alloy for 24 hours with acetone, cleaning is dry
It is dry, it is amino group.
(3) particle and step 2 that step 1 obtains are obtained amino group titanium alloy and be put into the deionized water of 20mL, added
Enter the carbodiimides of 0.5mL, reacts 4h, obtain connecing particle group titanium alloy.
Embodiment 2:
(1) by 50mgPLGA (polylactide glycolic acid copolymer), 6mg pluronic F-68 is dissolved in 2ml methylene chloride,
30Hz sonic oscillation 8min, then 90mg antibiotic is completely dissolved in 0.4mL deionized water, antibiotic solution is added later
In PLGA (polylactide glycolic acid copolymer) solution, turn upside down jog, keeps PLGA (polylactide glycolic acid copolymer) molten
The abundant packaging medicine of liquid forms colostric fluid, then the poly-vinyl alcohol solution of the 25mg/mL of 5mL, 30Hz ultrasound is added into colostric fluid
8min is vibrated, mixed liquor is slowly injected into the 25mg/mL poly-vinyl alcohol solution of 34mL after oscillation, is softly stirred with magnetic stirring apparatus
18h is mixed, final solution lower layer obtains the powder white particles similar to salt.This solution is fitted into centrifuge tube, with 5000r/
The revolving speed of min is centrifuged 20min, is washed with deionized water, is centrifuged 3 times, collects particle, vacuum freeze drying.
(2) the polished titanium alloy of physics is put into hydrofluoric acid (dense): nitric acid (1mol/mL): deionized water=1:4:5
Mix acid liquor in chemical polishing 1min, deionized water washs drying, then this titanium alloy is put into the reaction kettle of 100ml, thrown
Upward, then the sodium hydroxide solution 50mL of configured good 4mol/mL is added in kettle in the one side of light, reacts at 70 DEG C
90min.Cleaning sample after the completion.It prepares by solvent volume of toluene than the APTES (3- aminopropyl triethoxysilane) for 3%
Titanium alloy is put into solution by solution, at 50 DEG C, is condensed back 12h, then impregnated titanium alloy for 24 hours with acetone, cleaning is dry
It is dry, it is amino group.
(3) particle and step 2 that step 1 obtains are obtained amino group titanium alloy and be put into the deionized water of 10mL, added
Enter the carbodiimides of 0.2mL, reacts 3h, obtain connecing particle group titanium alloy.
Embodiment 3:
(1) by 70mgPLGA (polylactide glycolic acid copolymer), 7mg pluronic F-68 is dissolved in 2ml methylene chloride,
50Hz sonic oscillation 12min, then 110mg antibiotic is completely dissolved in 0.6mL deionized water, antibiotic solution is added later
In PLGA (polylactide glycolic acid copolymer) solution, turn upside down jog, keeps PLGA (polylactide glycolic acid copolymer) molten
The abundant packaging medicine of liquid forms colostric fluid, then the poly-vinyl alcohol solution of the 25mg/mL of 6mL, 50Hz ultrasound is added into colostric fluid
12min is vibrated, mixed liquor is slowly injected into the 25mg/mL poly-vinyl alcohol solution of 35mL after oscillation, it is soft with magnetic stirring apparatus
22h is stirred, final solution lower layer obtains the powder white particles similar to salt.This solution is fitted into centrifuge tube, with
The revolving speed of 5000r/min is centrifuged 40min, is washed with deionized water, is centrifuged 3 times, collects particle, vacuum freeze drying.
(2) the polished titanium alloy of physics is put into hydrofluoric acid (dense): nitric acid (1mol/mL): deionized water=1:4:5
Mix acid liquor in chemical polishing 3min, deionized water washs drying, then this titanium alloy is put into the reaction kettle of 100ml, thrown
Upward, then the sodium hydroxide solution 70mL of configured good 4mol/mL is added in kettle in the one side of light, reacts at 90 DEG C
100min.Cleaning sample after the completion.It prepares by solvent volume of toluene than APTES (the 3- aminopropyl-triethoxy silicon for 8%
Alkane) solution, titanium alloy is put into solution, at 70 DEG C, is condensed back 12h, then titanium alloy is impregnated into cleaning for 24 hours with acetone
It is dry, it is amino group.
(3) particle and step 2 that step 1 obtains are obtained amino group titanium alloy and be put into the deionized water of 30mL, added
Enter the carbodiimides of 0.8mL, reacts 5h, obtain connecing particle group titanium alloy.
The preparation method exploitativeness of the present invention it can be seen from Fig. 1-1, Fig. 1-2, Fig. 1-3, Fig. 1-4, Fig. 1-5
By force, preparation efficiency is high, and effect is good.The medical titanium alloy that the present invention prepares, surface form porous nanometer structure and uniform particle
Distribution has good anti-microbial property.
PLGA (polylactide glycolic acid copolymer) medicine-carried nano particles obtained in 1 step 1 of embodiment are respectively put into
It is discharged in the phosphate buffer of different pH value (pH4.5,5.4,6.4,7.4), collects above-mentioned particle and buffered in different pH value
1,5,7,20 days release liquids are placed in liquid respectively, detect the anti-microbial property of release liquid respectively.As seen from Figure 2: different
The antibacterial effect of particle is different under pH, and the effect of the lower antibacterial of pH value is better.At low ph values, ester bond is beaten in acid situation
The drug for the more releases opened is also more, and antibacterial effect is better.
By Fig. 3-1, Fig. 3-2, Fig. 3-3 it can be seen that compared to pure titanium and amino group, the cell number on particle group surface is connect
More and cell dispersion comparison is opened bigger, illustrate that the describing property of biology for connecing particle group is good, rush osteogenic effect is more preferable,
The synergistic effect of amino and PLGA (polylactide glycolic acid copolymer) can preferably promote Oesteoblast growth.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of preparation method of medical titanium alloy, it is characterised in that include the following steps:
Step 1, the preparation of particle:
1) 50-70mgPLGA, 6-7mg pluronic F-68 are dissolved in 2mL methylene chloride and form mixture, by the mixture
Sonic oscillation 8-12min obtains PLGA solution；
2) 90-110mg antibiotic is completely dissolved in 0.4-0.6mL deionized water and forms antibiotic solution, by the antibiotic
Solution is added in the PLGA solution, and turn upside down jog, so that PLGA solution is sufficiently wrapped up antibiotic molecule and is formed colostric fluid,
Again into colostric fluid be added 5-6mL 25mg/mL poly-vinyl alcohol solution after sonic oscillation 8-12min, be slowly injected into after oscillation
Final mixture is obtained into the 25mg/mL poly-vinyl alcohol solution of 34-35mL；It is final described in magnetic stirring apparatus gentle agitation again
Mixture 18-22h, until obtaining generating the reaction mixture for having white powder particle；
3) reaction mixture is fitted into centrifuge tube and does centrifugal treating, isolate solid part, solid part deionization
The processing of water centrifuge washing, treated, and solid part vacuum freeze drying obtains required particle；
Step 2, the preparation of amino group titanium alloy:
1) the polished titanium alloy of physics is immersed into the dense hydrofluoric acid of volume ratio: 1mol/mL nitric acid: deionized water=1:4:5
Chemical polishing 1-3min in mix acid liquor, then drying is washed with deionized, then titanium alloy is put into the reaction kettle of 100mL
In and by the physics polishing and chemical polishing one side upward, then in kettle be added 4mol/mL sodium hydroxide solution
50-70mL reacts 80-100min at 70-90 DEG C, cleans titanium alloy after the completion；
2) it prepares using toluene as the APTES solution of solvent, titanium alloy is soaked in the APTES solution, at 50-70 DEG C,
Be condensed back 12h, titanium alloy take out after, then with acetone by titanium alloy impregnate for 24 hours, be cleaned and dried, obtain amino group titanium alloy；
Step 3, the combination of amino group titanium alloy and particle:
Amino group titanium alloy described in particle and step 2 described in step 1 is put into the deionized water of 10-30mL, is added
The carbodiimides of 0.2-0.8mL reacts 3-5h, obtains connecing particle group titanium alloy, i.e. medical titanium alloy.
2. a kind of preparation method of medical titanium alloy according to claim 1, it is characterised in that: the antibiotic is through the ages
One of mycin, Teicoplanin Targocin.
3. a kind of preparation method of medical titanium alloy according to claim 1, it is characterised in that: the 1 of the step 1) in
The sonic oscillation frequency is 30-50Hz.
4. a kind of preparation method of medical titanium alloy according to claim 1, it is characterised in that: the 3 of the step 1) in
The revolving speed that the centrifugal treating is 5000r/min is centrifuged 20-40min.
5. a kind of preparation method of medical titanium alloy according to claim 1, it is characterised in that: the 3 of the step 1) in
Solid part deionized water centrifuge washing processing, 3 times repeatedly.
6. a kind of preparation method of medical titanium alloy according to claim 1, it is characterised in that: the 2 of the step 2) in
Described by the volume ratio of APTES in the APTES solution of solvent of toluene is 3%-8%.
7. a kind of medical titanium alloy, it is characterised in that: the medical titanium alloy system as described in any claim in claim 1-6
Preparation Method is made.
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| CN110464873B (en) * | 2019-06-06 | 2020-05-05 | 重庆大学 | Preparation method of medical titanium implant with function of eliminating surface biological membrane |
| CN111657285B (en) * | 2020-06-19 | 2022-02-22 | 福建省宇诚环保科技有限公司 | Sterilizing and disinfecting mosquito repellent liquid and preparation method thereof |
| CN111773433B (en) * | 2020-07-21 | 2022-02-08 | 北京积水潭医院 | Preparation method of drug-loaded nano-bubble bone cement |
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