CN104826159A - Medical titanium metal implant material and preparation method thereof - Google Patents
Medical titanium metal implant material and preparation method thereof Download PDFInfo
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- CN104826159A CN104826159A CN201510200604.5A CN201510200604A CN104826159A CN 104826159 A CN104826159 A CN 104826159A CN 201510200604 A CN201510200604 A CN 201510200604A CN 104826159 A CN104826159 A CN 104826159A
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- titanium metal
- implant material
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Abstract
The invention provides a medical titanium metal implant material and a preparation method thereof. The medical titanium metal implant material includes a titanium metal, titania nanotubes grown on the titanium metal surface in a matrix arrangement, a biodegradable superpolymer coating the end face of a titania nanotube layer in the matrix arrangement and sealing the titania nanotubes, and an anti-inflammatory antibacterial drug loaded in the titania nanotubes. The medical titanium metal implant material has the characteristics of being high in drug loading capacity and capable of making drug properties of the drug slowly released.
Description
Technical field
The invention belongs to medicine and medical instruments field, relate to a kind of medical titanium metal implant material and preparation method thereof.
Background technology
Due to the quickening of population in the world aging, cause osteoporosis, the case of fracture increases; In addition natural disaster, traffic accident, industrial injury etc. are traumatogenic increases, and makes the demand of medical embedded material growing.In the U.S., have more than 600,000 routine joints and Orthopeadic Surgery implant surgery every year; In Europe, have every year more than 400,000 routine mankind sclerous tissues surgical implantation.The whole world has about 2,000,000 cover spinal column implant systems to be used, and with annual 14% speed increment; China artificial joint replaces annual rate of growth up to 30%, the residual patient of existing 7,750,000 limb and annual newly-increased 3,000,000 bone injury patients.As can be seen here, medical embedded material is had great potentialities, and also needs increasing researcher badly and puts in the research of biomaterial.
Bio-medical titanium metal material is due to its good mechanical property, workability, be widely used in hard tissue substituting material and the vascular graftses such as cardiac valve, intravascular stent such as artificial bone, joint, tooth implant with near elastic modelling quantity, corrosion resistance and the good biocompatibility of people's bone photo.But titanium and titanium alloys itself exists the shortcoming of biologically inert, can not reach synostosis after implant into body with surrounding tissue, just simple machinery is sealed, is easily wrapped up by fibrous tissue and isolates with host tissue, if things go on like this can cause thrombosis and cause graft failure.In addition, in clinical operation, bacteriological infection is a very common large problem, and comprehensively sterilization and sterile working still keep away the generation of unavoidable postoperative infection.Main solution route is injection of antibiotics clinically, but injection of antibiotic has specificity, needs long term injections and can produce drug resistance strain.Medicine carrying type implant material, at implant surfaces fixed point release medicine, not only can avoid some unnecessary side effect, and can control drug level.
The surface topology of implant material and chemical composition at the absorption of Function protein matter, cell adhesion, move, sprawl, breed and play vital effect in the biological behaviour such as differentiation.Along with the fast development of micro-/ nano technology, be widely studied by regulating and controlling related biological behavior in implant material surface construction micro/nano structure.Meanwhile, from bionics angle, build micro-/ nano composite construction in biomedical material surface and can reach the mechanical sealed object with osseous tissue.
Large quantity research shows, the titania nanotube of appropriate size can promote osteoblastic function, and proposed first as a kind of brand-new drug delivery platform for medical implant at titania nanotube in 2007, titania nanotube can load any medicine, and can reach by the length of titania nanotube, diameter and pipe thickness the release controlling medicine.
At present, TiO
2the preparation method of nanotube mainly comprises following three kinds: i.e. template, hydro-thermal method and electrochemistry anodic oxidation.Due to low cost and the characteristic such as preparation method is simple, hydrothermal synthesis method and anodizing have the probability be widely used.Anodic oxidation is the method that the orderly Nano tube array of titanium dioxide of preparation is the most frequently used at present.Anodizing due to its preparation method simple, controlled and advantages such as high-sequential, have obvious advantage when preparing titania nanotube.From 1999, Zwilling etc. reported and in metal titanium sheet, obtain nanoporous oxide structure by anodizing.Calendar year 2001, Gong etc. reach the Nano tube array of titanium dioxide of 0.5 micron and high-sequential in hydrofluoric acid aqueous solution Anodic Oxidation legal system for length first.
PLGA (PLGA) is a kind of good biocompatibility, biodegradable and nontoxic high polymer.There is good degradation property, its degradation rate can be controlled accurately by the character of group contained by the ratio of change molecular weight, lactic acid (LA) and hydroxyacetic acid (GA) and the end of the chain and quantity.It has been widely used in bio-medical material aspect, as trachea is changed, and ligament reconstructive, surgical dressing, dental prosthetic, and tissue engineering bracket.Can support and promote Bone Defect Repari and bone remoulding as the material applied in organizational project, be therefore a kind of application implant material more widely.
The present invention is directed to the bone renovating material of titania nanotube as medicine carrying type of the deficiency of titania nanotube sustained drug release effect and the coating of invention degradable high polymer.Titania nanotube and degradable high polymer all have good biocompatibility, can not produce in vivo and repel and other specific reactions.Using titania nanotube as pharmaceutical carrier, high drug loading can be realized.Adopt degradable high polymer as outer field encapsulating material, the controllable release of medicine can be realized.Therefore the bone renovating material of this kind of medicine carrying type had both achieved high drug loading, achieved again the property of medicine slow releasing of medicine, and can support and promote Bone Defect Repari and bone remoulding.
Summary of the invention
The object of this invention is to provide that a kind of drug loading is high, the medical titanium metal implant material of the property of medicine slow releasing that can make medicine and preparation method thereof.
In order to achieve the above object, on the one hand, the invention provides a kind of medical titanium metal implant material, it comprises titanium, be grown on the titania nanotube of the arrangement in matrix of surface of metal titanium, also comprise the titania nanotube end face and the degradable high polymer of sealing titania nanotube that are coated on the arrangement in matrix and the drug for diminishing inflammation and antibiosis be loaded in titania nanotube.
Second aspect, the invention provides a kind of preparation method of medical titanium metal implant material, comprises the steps:
A. with titanium for anode, with containing F
-solution be electrolyte, voltage be 20-40V, temperature reacts 1-8h under being 30-60 DEG C of condition, cleaning, dry, obtains the titanium of the titania nanotube that superficial growth has matrix to arrange;
B. drug for diminishing inflammation and antibiosis is loaded in the titania nanotube obtained to steps A;
C. to the titania nanotube end face coating degradable high polymer solution of matrix arrangement, after drying, target product is obtained.
The invention has the beneficial effects as follows:
(1) the medical titanium metal implant material prepared by, the degradable high polymer coating on surface has good biologic activity, is conducive to the osteoblastic adhesion of implant into body, moves, sprawls, breeds and the biological behaviour such as differentiation;
(2) TiO is utilized
2the specific surface area that nanotube is large, load drug for diminishing inflammation and antibiosis, along with the degraded of polymer coating, drug release out, shows good antibacterial ability;
(3) utilize degradable high polymer as medicament slow release layer, by controlling the thickness of medicament slow release layer, regulate and control drug release rate, drug release natural law is 40 days.
Accompanying drawing explanation
Fig. 1 is the structural representation of medical titanium metal implant material of the present invention;
Fig. 2 is the scanning electron microscope spectrogram of the titania nanotube layer end face of the matrix arrangement that embodiment one obtains;
Fig. 3 is the surface topography scanning electron microscope spectrogram after sample that embodiment one obtains applies one deck PLGA;
Fig. 4 is the longitudinal section scanning electron microscope spectrogram after sample that embodiment one obtains applies one deck PLGA;
Fig. 5 is drug release situation collection of illustrative plates in vitro after the different number of plies PLGA of the medical titanium metal implant coated materials that obtains of embodiment one.
Detailed description of the invention
As shown in Figure 1, one aspect of the present invention provides a kind of medical titanium metal implant material 100, it comprises titanium 1, be grown on the titania nanotube 2 of the arrangement in matrix on titanium 1 surface, also comprise titania nanotube 2 end face and the degradable high polymer 3 of sealing titania nanotube 2 that are coated on the arrangement in matrix and the drug for diminishing inflammation and antibiosis 4 be loaded in titania nanotube.
Preferably, described titanium 1 comprises pure titanium metal, Ti-6Al-4V alloy, Ti-6Al-7Nb alloy, Ti-5Al-2.5Sn alloy, Ti-5Al-2.5Fe alloy and Nitinol.Described titanium 1 can be that lamellar, tubulose or strip etc. can imagine the shape obtained.
Preferably, described degradable high polymer 3 is one or more the mixture in llowing group of materials: Acetic acid, hydroxy-, bimol. cyclic ester/lactide copolymer, polyglycolic acid, polylactic acid, polycaprolactone and chitosan.Preferred further, described degradable high polymer 3 coating layer thickness is 0.75-10 micron.
Preferably, described drug for diminishing inflammation and antibiosis 4 is one or more mixture of following material: ibuprofen, ceftazidime, ciprofloxacin, gentamycin sulfate, Furbenicillin, cefradine and cefmetazole.
Second aspect present invention provides a kind of preparation method of medical titanium metal implant material 100, comprises the steps:
A. with titanium 1 for anode, with containing the solution of F-for electrolyte, voltage be 20-40V, temperature reacts 1-8h under being 30-60 DEG C of condition, cleaning, dry, obtains the titanium 1 of the titania nanotube 2 that superficial growth has matrix to arrange;
B. drug for diminishing inflammation and antibiosis 4 is loaded in the titania nanotube 2 obtained to steps A;
C. to titania nanotube 2 end face coating degradable high polymer 3 solution of matrix arrangement, after drying, target product is obtained.
Described degradable high polymer 3 is one or more the mixture in llowing group of materials: Acetic acid, hydroxy-, bimol. cyclic ester/lactide copolymer, polyglycolic acid, polylactic acid, polycaprolactone and chitosan.Preferably, described degradable high polymer 3 solution quality volume ratio is 1-5%, and described degradable high polymer 3 solution applies several times, and each coated weight is 0.02-0.05mL.
Preferably, in described steps A, electrolyte is 0.1-0.4wt%NH
4f, 1-5vol%H
2the ethylene glycol of O or glycerin solution.
Alternatively optimal way, in described steps A, electrolyte is 0.25vt%-1vt%HF aqueous solution or is 0.05-0.2mol/L F
-with 0.5-0.2mol/L SO4
2-aqueous solution.
Preferably, the process of loading drug for diminishing inflammation and antibiosis 4 in described step B comprises, and it is in drug for diminishing inflammation and antibiosis 4 solution of 50-200mg/ml that the titanium 1 of the titania nanotube 2 that superficial growth steps A obtained has matrix to arrange immerses concentration, dry.Described drying can adopt heat drying, also can adopt the mode of static volatilization.
Alternatively optimal way, the process of loading drug for diminishing inflammation and antibiosis 4 in described step B comprises, and the mode of drug for diminishing inflammation and antibiosis 4 with vacuum infiltration is loaded in titania nanotube.
Preferably, described degradable high polymer 3 solution can select following solvent: chloroform, dichloromethane, ethyl acetate, Isosorbide-5-Nitrae-dioxane, dilute hydrochloric acid and spirit of vinegar.Preferably, described steps A also comprises, and carries out polishing, etching pretreatment to titanium 1 surface.Concrete, described polishing step comprises: by titanium 1 polishing grinding, and be placed in acetone ultrasonic cleaning and be about 30min, ultrasonic cleaning is about 20min in deionized water subsequently, for subsequent use.Concrete, described etching processing etching liquid is by 10%HF, 40%HNO
3and 50%H
2o mixes.Further, polished titanium 1 is encapsulated process, surrounding is wound around copper wire, the approved sample product back side is coated with epoxide-resin glue, outside not exposed to copper wire, only expose question response surface, use the electric conductivity of sample after circuit tester test package again, after determining conduction, be placed in etching liquid, the processing time is 1-10s.
Below in conjunction with specific embodiment, set forth the present invention further.
For a better understanding of the present invention, below in conjunction with drawings and Examples the present invention done and describe in detail further.
Embodiment 1
Step one,
Sample pretreatment, by pure titanium metal sheet polishing grinding, be placed in acetone ultrasonic cleaning and be about 30min, ultrasonic cleaning is about 20min in deionized water subsequently, for subsequent use.
Step 2,
The configuration of etching liquid, etching liquid is respectively 10%HF by volume ratio, 40%HNO
3and 50%H
2o mixes.For subsequent use.
Step 3,
The configuration of electrolyte in anodic oxidation reactions process, it consists of 0.3wt%NH
4f, 3vol%H
2the ethylene glycol solution of O, for subsequent use.
Step 4,
Configuration degradable high polymer solution, in present case, degradable high polymer used is PLGA and PLGA, and solvent for use is chloroform, and weight by volume concentration is 1%, for subsequent use.
Step 5,
Sample encapsulating process, is wound around copper wire in sample surrounding, is coated with the approved sample product back side with epoxide-resin glue, outside not exposed to copper wire, only exposes question response surface.Use circuit tester test package sample electric conductivity again, conduction can carry out following step.
Step 6,
Sample etching processing, step 4 has been encapsulated the pure titanium metal sheet handled well and be placed in the etching liquid of step 2 configuration, the processing time is 5s.
Step 7,
Sample after above-mentioned process is anode, and graphite is as negative electrode, and be put in the plastic cup of the electrolyte that step 3 configuration is housed, pure titanium metal sheet is placed in below liquid level of electrolyte, described beaker is placed in water-bath magnetic stirring apparatus, constantly stirs.Voltage is 30V, and reaction 1h, temperature is 60 DEG C.
Step 8,
Taken out by sample, use ethanol, deionized water ultrasonic cleaning sample 5min respectively, drying can obtain the pure titanium metal sheet of the titania nanotube 2 that superficial growth has matrix to arrange.To the titania nanotube 2 end face shooting scanning electron microscope spectrogram that described matrix is arranged, as shown in Figure 2.
Step 9,
Sample load drug for diminishing inflammation and antibiosis 4, the sample of the titania nanotube 2 having matrix to arrange superficial growth is immersed in drug for diminishing inflammation and antibiosis 4 solution, and present case drug for diminishing inflammation and antibiosis 4 used solution is the alcoholic solution of the ibuprofen of 100mg/ml, leaves standstill 3 days.
Step 10,
Use spin coating method, the PLGA that the sample surfaces coating step four after step 9 process configures, coating layer thickness is respectively 1, and 3,5,8,10 layers, drying, as shown in Figure 3, longitudinal section pattern as shown in Figure 4 for the surface topography of coating one deck PLGA.
The slow release situation of drugs in vitro, test condition and testing procedure as follows:
1. will be coated with 0 respectively, 1,3,5,8, the medical titanium metal implant material sample of the PLGA of 10 layers is immersed in 100ml PBS buffer solution respectively, preserves at 37 DEG C of temperature.
2., at front 6h, take out 5ml PBS buffer solution every 1h, in afterwards 40 days, take out 5ml PBS buffer solution every day.It is to be measured that each time point takes out PBS solution, separately adds the fresh PBS solution of 5ml.
3. measure drug in solution ultraviolet absorptivity to be measured with ultra-violet and visible spectrophotometer.According to the ultraviolet standard curve of medicine, calculate the concentration of medicine.Last is transverse axis with soak time, and liquid drug concentration to be measured draws the drug release patterns shown in Fig. 5 for the longitudinal axis.
As shown in Figure 5, after applying 10 layers of medicament controlled-release coating, the release time of medicine is 40 days.
Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Claims (10)
1. a medical titanium metal implant material, it comprises titanium, be grown on the titania nanotube of the arrangement in matrix of surface of metal titanium, it is characterized in that: also comprise the titania nanotube end face and the degradable high polymer of sealing titania nanotube that are coated on the arrangement in matrix and the drug for diminishing inflammation and antibiosis be loaded in titania nanotube.
2. medical titanium metal implant material as claimed in claim 1, is characterized in that: described titanium comprises pure titanium metal, Ti-6Al-4V alloy, Ti-6Al-7Nb alloy, Ti-5Al-2.5Sn alloy, Ti-5Al-2.5Fe alloy and Nitinol.
3. medical titanium metal implant material as claimed in claim 1, is characterized in that: described degradable high polymer is one or more the mixture in llowing group of materials: Acetic acid, hydroxy-, bimol. cyclic ester/lactide copolymer, polyglycolic acid, polylactic acid, polycaprolactone and chitosan.
4. medical titanium metal implant material as claimed in claim 1, is characterized in that: described drug for diminishing inflammation and antibiosis is one or more mixture of following material: ibuprofen, ceftazidime, ciprofloxacin, gentamycin sulfate, Furbenicillin, cefradine and cefmetazole.
5. a preparation method for medical titanium metal implant material, comprises the steps:
A. with titanium for anode, with containing F
-solution be electrolyte, voltage be 20-40V, temperature reacts 1-8h under being 30-60 DEG C of condition, cleaning, dry, obtains the titanium of the titania nanotube that superficial growth has matrix to arrange;
B. drug for diminishing inflammation and antibiosis is loaded in the titania nanotube obtained to steps A;
C. to the titania nanotube end face rotary coating degradable high polymer solution of matrix arrangement, after drying, target product is obtained.
6. the preparation method of medical titanium metal implant material as claimed in claim 5, is characterized in that: in described steps A, electrolyte is 0.1-0.4wt%NH
4f, 1-5vol%H
2the ethylene glycol of O or glycerin solution.
7. the preparation method of medical titanium metal implant material as claimed in claim 5, is characterized in that: in described steps A, electrolyte is 0.25vt%-1vt%HF aqueous solution or is 0.05-2mol/L F
-with 0.5-2mol/L SO4
2-aqueous solution.
8. the preparation method of medical titanium metal implant material as claimed in claim 5, it is characterized in that: the process of loading drug for diminishing inflammation and antibiosis in described step B comprises, it is in the drug for diminishing inflammation and antibiosis solution of 50-200mg/mL that the titanium of the titania nanotube that superficial growth steps A obtained has matrix to arrange immerses concentration, dry.
9. the preparation method of medical titanium metal implant material as claimed in claim 5, is characterized in that: the process of loading drug for diminishing inflammation and antibiosis in described step B comprises, the mode of drug for diminishing inflammation and antibiosis vacuum infiltration is loaded in titania nanotube.
10. the preparation method of medical titanium metal implant material as claimed in claim 5, is characterized in that: described steps A also comprises, and carries out polishing, etching pretreatment to surface of metal titanium.
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| CN105251054A (en) * | 2015-11-17 | 2016-01-20 | 广西中医药大学 | Method for preparing titanium dioxide nanotubes with antibacterial and anticancer functions through ruthenium complex |
| CN105288723A (en) * | 2015-11-17 | 2016-02-03 | 广西中医药大学 | Method for treating titanium dioxide nano-tubes by using iridium coordination compound |
| CN105288727A (en) * | 2015-11-17 | 2016-02-03 | 广西中医药大学 | Method for preparing antibacterial and anti-cancer titanium dioxide nano-tubes by using rhodium coordination compound |
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| CN105288724A (en) * | 2015-11-20 | 2016-02-03 | 广西中医药大学 | Method for treatment of titanium dioxide nanotubes with curcumin derivative |
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| CN105396174A (en) * | 2015-11-20 | 2016-03-16 | 广西中医药大学 | Method for preparing titanium dioxide nanotube with antibacterial and anti-cancer properties |
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| CN109692695A (en) * | 2018-12-27 | 2019-04-30 | 东北大学 | A kind of near infrared light response type nano composite titania material and preparation method thereof |
| CN109692695B (en) * | 2018-12-27 | 2022-02-01 | 东北大学 | Near-infrared light response type nano titanium dioxide composite material and preparation method thereof |
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| CN112336918A (en) * | 2020-10-27 | 2021-02-09 | 北京大学口腔医学院 | Preparation method of implant material |
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