CN101732761A - Joint prosthesis by using titanium oxide nanotubes to load bone morphogenetic protein - Google Patents
Joint prosthesis by using titanium oxide nanotubes to load bone morphogenetic protein Download PDFInfo
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Abstract
The invention relates to a joint prosthesis by using titanium oxide nanotubes to load bone morphogenetic proteins and a preparation method thereof. The surface of a metallic matrix of the joint prosthesis is provided with a tubular titanium oxide nanotube array layer which is irradiated by ultraviolet rays; and the bone morphogenetic proteins (BMP) are loaded in the tubular titanium oxide nanotube array layer further. The preparation method for the joint prosthesis by using the titanium oxide nanotubes to load the bone morphogenetic proteins comprises the following steps: processing the joint prosthesis by adopting pure titanium or a titanium alloy; then obtaining the tubular titanium oxide nanotube array layer on the surface of the pure titanium or the titanium alloy joint prosthesis through a two-step anodic oxidation technique, and irradiating the titanium oxide nanotube array layer by the ultraviolet rays; and finally, loading the bone morphogenetic proteins in the titanium oxide nanotube array layer which is irradiated by the ultraviolet rays through a centrifugal loading technique.
Description
Technical field
The present invention relates to a kind of artificial joint with titanium oxide nanotubes to load bone morphogenetic protein, particularly relate to a kind of surface and have, belong to the artificial joint material technical field through artificial joint of the titania nanotube load bone morphogenetic proteins (BMP) of irradiation under ultraviolet ray and preparation method thereof.
Background technology
The whole world is annual to have the 1500000 joints lose function patients that cause because of degenerated and inflammatory arthritis need carry out artificial joint replacement approximately.Wherein metal material is used the earliest as the manufacture of intraocular joint, and the application at present clinical is also still extensive.As time goes on show with clinical research that the artificial joint ubiquity artificial joint of metal material situation such as become flexible, sink or fracture causes bone resorption, is one of major complications that influences prosthetic replacement's late result.
Bone morphogenetic protein (bone morphogenetic protein, BMP) be the multi-functional somatomedin of a class, can induce bone and cartilage to form in vivo, and express during, repair of cartilage early stage in limbs growth, endochondral ossification, fracture, the fetal development and the Regeneration and Repair of skeleton played an important role.The bone morphogenetic protein immunogenicity is low, does not generally cause to have only slight zest by immunological rejection, and this provides a good prospect for the articular cartilage reparation.But the BMP diffusivity is strong, and the independent implantation of BMP is organized liquid very soon and rinses out and be organized the enzyme degraded, is difficult to keep concentration and can not play one's part to the full around target cell.With carrier with the BMP slow release in the target location, be a convenience and effective route of administration.Ideal BMP carrier material should have following characteristics: (1) can carry BMP and keep its activity; (2) have the good biofacies same sex, can keep the porosity of release, be beneficial to osteoblast and creep; (3) no cytotoxicity, non-immunogenicity has biodegradability, and is compound easy with BMP; (4) carrier material is easy to obtain, sterilizes and lays in.
Pure titanium and alloy thereof have the oxide layer titanium that outstanding biocompatibility is mainly given the credit to surface attachment, and the major advantage of surface oxide layer is: (1) titanium dioxide has lower intrinsic toxicity; (2) dissolubility of titanium dioxide in water is very low; (3) reactivity with biomolecule is very low, near chemical inertness.
Titanium dioxide has excellent biological compatibility, and the titanium dioxide surface with nanostructured can promote osteoblastic adhesion, growth and propagation.Under irradiation under ultraviolet ray, the nano titanium oxide surface produces many active oh groups, helps improving hydrophilic, and then improves cell compatibility.So, cause the present invention.
Summary of the invention
The objective of the invention is to propose a kind of method for preparing with the artificial joint of titanium oxide nanotubes to load bone morphogenetic protein, construct nano tubular structure by two step anodizings at metal base surface, under irradiation under ultraviolet ray, improve the hydrophilic and the cell compatibility of nano tubular structure, pass through the centrifugal load technology at last at nanotube layer internal burden bone morphogenetic protein.Titania nanotube load bone morphogenetic proteins layer and the substrate combinating strength prepared are good, and preparation technology is simple, and is workable.
The present invention is realized by the following technical programs:
At this artificial joint material metal base surface the titanium dioxide nanotube array layer with tubular structure of one deck through irradiation under ultraviolet ray arranged, further load has bone morphogenetic protein (BMP) in its layer.
The step of concrete preparation is as follows:
1) at first select for use pure titanium or titanium alloy to process artificial joint;
2) artificial joint surface preparation: behind the surface grinding, use acetone, deionized water and dehydrated alcohol supersound washing 10-120 minute successively, use HF and HNO subsequently
3And mixed solution (volume ratio is 1: 4: 5) the chemical polishing 20-120 second of water, behind the deionized water cleaning down, dry up stand-by again;
3) two step anodic oxidations prepare titania nanotube: with the artificial joint of surface preparation as anode, graphite or platinum are negative electrode, in moisture organic electrolyte solution, carry out the anodic oxidation first time, concrete anodic oxidation parameter is: voltage is 20-240V, time is 12-200 hour, the two poles of the earth distance is 3-10cm, and temperature remains room temperature.After the anodic oxidation for the first time, take out, in percent by volume is in the hydrochloric acid solution of 5-30vol% ultrasonic cleaning 0.5-3 hour, after taking-up dries up, artificial joint is carried out the anodic oxidation second time again under aforementioned anodic oxidation first time parameter condition, take out then, with dehydrated alcohol ultrasonic cleaning 10-30 minute, after being to soak 0.5-3 hour in the hydrochloric acid solution of 5-30vol%, percent by volume takes out again, with dehydrated alcohol and deionized water alternately clean 6-10 all over after, at 60-100 ℃ of following drying sample, obtain titanium dioxide nanotube array layer again on the artificial joint surface;
4) artificial joint of above-mentioned surface coverage titanium dioxide nanotube array layer is used irradiation under ultraviolet ray in deionized water or in atmosphere, improve hydrophilic and cell compatibility.The uviol lamp that uses is high voltage mercury lamp, and irradiation time is no less than 10 hours;
5) the titanium dioxide nanotube array layer internal burden bone morphogenetic protein that adopts the centrifugal load technology crossing at last through irradiation under ultraviolet ray, there is artificial joint to place the centrifuge container bottom surface coverage through the titanium dioxide nanotube array layer of irradiation under ultraviolet ray, pour the mixed solution that bone morphogenetic protein and phosphate buffered saline(PBS) are formed again into, liquid level flooded artificial joint to half of centrifuge container or 2/3rds height, and bone morphogenetic protein concentration is 0.1-50mgL
-1, centrifugal under the room temperature (1500-80000Rpm) soaked 0.5-10 hour.Take out, get final product bioactive artificial joint of the present invention.
It is solvent that moisture organic electrolyte solution of the present invention adopts ethylene glycol, and other effective ingredient is: water 0-10vol% (percent by volume), phosphoric acid 2-10vol% (percent by volume), ammonium fluoride 0.1-0.9wt% (mass percent).
The titania nanotube rule oriented of the inventive method preparation is arranged, and titania nanotube is producing perpendicular to the matrix direction, and caliber reaches 50-800nm, and pipe range is 1-150 μ m, and specific surface area is big.
The artificial joint with titanium oxide nanotubes to load bone morphogenetic protein of the present invention's preparation has the following advantages and beneficial effect:
1. Nano tube array of titanium dioxide is shone with ultraviolet light, will produce many active oh groups, help improving hydrophilic, and then improve cell compatibility on its surface.
2. compare with common titanium dioxide layer, Nano tube array of titanium dioxide is orienting stephanoporate, and specific surface area is higher, helps the load of bone morphogenetic protein and to the controlled release of bone morphogenetic protein.
3. the titanium dioxide nanotube array layer of anodic oxidation formation is that matrix is generated in-situ, and is fine with the adhesion of matrix.Bone morphogenetic protein has good induced osteogenesis effect, can form firm physiology with osseous tissue in the short time and combine.Therefore, be expected to increase artificial joint stability.
Description of drawings
Fig. 1 is the concrete preparation process figure of the present invention.
Fig. 2 is scanning electron microscope (SEM) photo of the titanium dioxide nanotube array layer form of the artificial articular surface of the present invention with tubular structure.
The specific embodiment
Embodiment 1
(1) at first select for use titanium alloy to process artificial joint;
(2) artificial joint surface preparation: behind the surface grinding, use acetone, deionized water and dehydrated alcohol supersound washing 10-30 minute successively, use HF and HNO subsequently
3And mixed solution (volume ratio is 1: 4: 5) the chemical polishing 20-40 second of water, behind the deionized water cleaning down, hair dryer dries up stand-by again;
(3) prepare moisture organic electrolyte solution: employing ethylene glycol is solvent, and other effective ingredient is: water 2vol% (percent by volume), phosphatase 24 vol% (percent by volume), ammonium fluoride 0.3wt% (mass percent);
(4) two step anodic oxidations prepare titania nanotube: with the artificial joint of surface preparation as anode, graphite or platinized platinum are negative electrode, in moisture organic electrolyte solution, carry out the anodic oxidation first time, concrete anodic oxidation parameter is: voltage is 60V, anodizing time is 18 hours, the two poles of the earth distance is 3-10cm, and temperature remains room temperature.After the anodic oxidation for the first time, take out, in percent by volume is in the hydrochloric acid solution of 10vol% ultrasonic cleaning 0.5-3 hour, after taking-up dries up, artificial joint is carried out the anodic oxidation second time again under aforementioned anodic oxidation first time parameter condition, take out then, with dehydrated alcohol ultrasonic cleaning 10-30 minute, after being to soak 0.5-3 hour in the hydrochloric acid solution of 10vol%, percent by volume takes out again, with dehydrated alcohol and deionized water alternately clean 6-10 all over after, at 60-100 ℃ of following drying sample, obtain titanium dioxide nanotube array layer again on the artificial joint surface;
(5) artificial joint of above-mentioned surface coverage titanium dioxide nanotube array layer is used irradiation under ultraviolet ray in deionized water or in atmosphere, improve hydrophilic and cell compatibility.The uviol lamp that uses is high voltage mercury lamp, shines 15 hours;
(6) the titanium dioxide nanotube array layer internal burden bone morphogenetic protein that adopts the centrifugal load technology crossing at last through irradiation under ultraviolet ray, there is artificial joint to place the centrifuge container bottom surface coverage through the titanium dioxide nanotube array layer of irradiation under ultraviolet ray, pour the mixed solution of the phosphate buffered saline(PBS) composition of bone morphogenetic protein and 0.1mol/L again into, liquid level flooded artificial joint to half of centrifuge container or 2/3rds height, and bone morphogenetic protein concentration is 0.1-50mgL
-1, centrifugal under the room temperature (5000Rpm) soaked 0.5-10 hour, took out, get final product the artificial joint of the present invention.
Embodiment 2
(1) at first select for use titanium alloy to process artificial joint;
(2) artificial joint surface preparation: behind the surface grinding, use acetone, deionized water and dehydrated alcohol supersound washing 30-60 minute successively, use HF and HNO subsequently
3And mixed solution (volume ratio is 1: 4: 5) the chemical polishing 40-60 second of water, behind the deionized water cleaning down, hair dryer dries up stand-by again;
(3) prepare moisture organic electrolyte solution: employing ethylene glycol is solvent, and other effective ingredient is: water 2vol% (percent by volume), phosphatase 24 vol% (percent by volume), ammonium fluoride 0.5wt% (mass percent);
(4) two step anodic oxidations prepare titania nanotube: with the artificial joint of surface preparation as anode, graphite or platinized platinum are negative electrode, in moisture organic electrolyte solution, carry out the anodic oxidation first time, concrete anodic oxidation parameter is: voltage is 80V, time is 18 hours, the two poles of the earth distance is 3-10cm, and temperature remains room temperature.After the anodic oxidation for the first time, take out, in percent by volume is in the hydrochloric acid solution of 10vol% ultrasonic cleaning 0.5-3 hour, after taking-up dries up, artificial joint is carried out the anodic oxidation second time again under aforementioned anodic oxidation first time parameter condition, take out then, with dehydrated alcohol ultrasonic cleaning 10-30 minute, after being to soak 0.5-3 hour in the hydrochloric acid solution of 10vol%, percent by volume takes out again, with dehydrated alcohol and deionized water alternately clean 6-10 all over after, at 60-100 ℃ of following drying sample, obtain titanium dioxide nanotube array layer on the artificial joint surface again, its SEM photo is seen Fig. 2;
(5) artificial joint of above-mentioned surface coverage titanium dioxide nanotube array layer is used irradiation under ultraviolet ray in deionized water or in atmosphere, improve hydrophilic and cell compatibility.The uviol lamp that uses is high voltage mercury lamp, shines 30 hours;
(6) the titanium dioxide nanotube array layer internal burden bone morphogenetic protein that adopts the centrifugal load technology crossing at last through irradiation under ultraviolet ray, there is artificial joint to place the centrifuge container bottom surface coverage through the titanium dioxide nanotube array layer of irradiation under ultraviolet ray, pour the mixed solution of the phosphate buffered saline(PBS) composition of bone morphogenetic protein and 0.1mol/L again into, liquid level flooded artificial joint to half of centrifuge container or 2/3rds height, and bone morphogenetic protein concentration is 0.1-50mgL
-1, centrifugal under the room temperature (2000Rpm) soaked 0.5-10 hour, took out, get final product the artificial joint of the present invention.
Embodiment 3
(1) at first select for use pure titanium to process artificial joint;
(2) artificial joint surface preparation: behind the surface grinding, use acetone, deionized water and dehydrated alcohol supersound washing 60-90 minute successively, use HF and HNO subsequently
3And mixed solution (volume ratio is 1: 4: 5) the chemical polishing 60-80 second of water, behind the deionized water cleaning down, hair dryer dries up stand-by again;
(3) prepare moisture organic electrolyte solution: employing ethylene glycol is solvent, and other effective ingredient is: water 4vol% (percent by volume), phosphoric acid 6vol% (percent by volume), ammonium fluoride 0.5wt% (mass percent);
(4) two step anodic oxidations prepare titania nanotube: with the artificial joint of surface preparation as anode, graphite or platinized platinum are negative electrode, in moisture organic electrolyte solution, carry out the anodic oxidation first time, concrete anodic oxidation parameter is: voltage is 40V, time is 24 hours, the two poles of the earth distance is 3-10cm, and temperature remains room temperature.After the anodic oxidation for the first time, take out, in percent by volume is in the hydrochloric acid solution of 20vol% ultrasonic cleaning 0.5-3 hour, after taking-up dries up, artificial joint is carried out the anodic oxidation second time again under aforementioned anodic oxidation first time parameter condition, take out then, with dehydrated alcohol ultrasonic cleaning 10-30 minute, after being to soak 0.5-3 hour in the hydrochloric acid solution of 20vol%, percent by volume takes out again, with dehydrated alcohol and deionized water alternately clean 6-10 all over after, at 60-100 ℃ of following drying sample, obtain titanium dioxide nanotube array layer again on the artificial joint surface;
(5) artificial joint of above-mentioned surface coverage titanium dioxide nanotube array layer is used irradiation under ultraviolet ray in deionized water or in atmosphere, improve hydrophilic and cell compatibility.The uviol lamp that uses is high voltage mercury lamp, and irradiation time is no less than 10 hours;
(6) the titanium dioxide nanotube array layer internal burden bone morphogenetic protein that adopts the centrifugal load technology crossing at last through irradiation under ultraviolet ray, there is artificial joint to place the centrifuge container bottom surface coverage through the titanium dioxide nanotube array layer of irradiation under ultraviolet ray, pour the mixed solution of the phosphate buffered saline(PBS) composition of bone morphogenetic protein and 0.1mol/L again into, liquid level flooded artificial joint to half of centrifuge container or 2/3rds height, and bone morphogenetic protein concentration is 0.1-50mgL
-1, centrifugal under the room temperature (10000Rpm) soaked 0.5-10 hour, took out, get final product the artificial joint of the present invention.
Embodiment 4
(1) at first select for use titanium alloy to process artificial joint;
(2) artificial joint surface preparation: behind the surface grinding, use acetone, deionized water and dehydrated alcohol supersound washing 90-120 minute successively, use HF and HNO subsequently
3And mixed solution (volume ratio is 1: 4: 5) the chemical polishing 80-120 second of water, behind the deionized water cleaning down, hair dryer dries up stand-by again;
(3) prepare moisture organic electrolyte solution: employing ethylene glycol is solvent, and other effective ingredient is: water 2vol% (percent by volume), phosphoric acid 5vol% (percent by volume), ammonium fluoride 0.5wt% (mass percent);
(4) two step anodic oxidations prepare titania nanotube: with the artificial joint of surface preparation as anode, graphite or platinized platinum are negative electrode, in moisture organic electrolyte solution, carry out the anodic oxidation first time, concrete anodic oxidation parameter is: voltage is 80V, time is 12 hours, the two poles of the earth distance is 3-10cm, and temperature remains room temperature.After the anodic oxidation for the first time, take out, in percent by volume is in the hydrochloric acid solution of 20vol% ultrasonic cleaning 0.5-3 hour, after taking-up dries up, artificial joint is carried out the anodic oxidation second time again under aforementioned anodic oxidation first time parameter condition, take out then, with dehydrated alcohol ultrasonic cleaning 10-30 minute, after being to soak 0.5-3 hour in the hydrochloric acid solution of 20vol%, percent by volume takes out again, with dehydrated alcohol and deionized water alternately clean 6-10 all over after, at 60-100 ℃ of following drying sample, obtain titanium dioxide nanotube array layer again on the artificial joint surface;
(5) artificial joint of above-mentioned surface coverage titanium dioxide nanotube array layer is used irradiation under ultraviolet ray in deionized water or in atmosphere, improve hydrophilic and cell compatibility.The uviol lamp that uses is high voltage mercury lamp, and irradiation time is no less than 10 hours;
(6) the titanium dioxide nanotube array layer internal burden bone morphogenetic protein that adopts the centrifugal load technology crossing at last through irradiation under ultraviolet ray, there is artificial joint to place the centrifuge container bottom surface coverage through the titanium dioxide nanotube array layer of irradiation under ultraviolet ray, pour the mixed solution of the phosphate buffered saline(PBS) composition of bone morphogenetic protein and 0.1mol/L again into, liquid level flooded artificial joint to half of centrifuge container or 2/3rds height, and bone morphogenetic protein concentration is 0.1-50mgL
-1, centrifugal under the room temperature (1500-80000Rpm) soaked 0.5-10 hour, took out, get final product the artificial joint of the present invention.
Claims (2)
1. artificial joint with titanium oxide nanotubes to load bone morphogenetic protein, it is characterized in that: described artificial joint with titanium oxide nanotubes to load bone morphogenetic protein is selected pure titanium or titanium alloy processing for use, adopt two step anodizing technologies to obtain to have the titanium dioxide nanotube array layer of tubular structure then at pure titanium or titanium alloy artificial joint surface, again titanium dioxide nanotube array layer is carried out irradiation under ultraviolet ray, adopt the centrifugal load technology at the titanium dioxide nanotube array layer internal burden bone morphogenetic protein through irradiation under ultraviolet ray at last, the preparation method of being addressed with the artificial joint of titanium oxide nanotubes to load bone morphogenetic protein is carried out as follows:
1) at first select for use pure titanium or titanium alloy to process artificial joint;
2) artificial joint surface preparation: behind the surface grinding, use acetone, deionized water and dehydrated alcohol supersound washing 10-120 minute successively, use HF and HNO subsequently
3And mixed solution (volume ratio is 1: 4: 5) the chemical polishing 20-120 second of water, behind the deionized water cleaning down, dry up stand-by again;
3) two step anodic oxidations prepare titania nanotube: with the artificial joint of surface preparation as anode, graphite or platinum are negative electrode, in moisture organic electrolyte solution, carry out the anodic oxidation first time, concrete anodic oxidation parameter is: voltage 20-240V, response time 12-200 hour, the two poles of the earth are apart from 3-10cm, and temperature remains room temperature.After the anodic oxidation for the first time, take out, in percent by volume is in the hydrochloric acid solution of 5-30vol% ultrasonic cleaning 0.5-3 hour, after taking-up dries up, artificial joint is carried out the anodic oxidation second time again under aforementioned anodic oxidation first time parameter condition, take out then, with dehydrated alcohol ultrasonic cleaning 10-30 minute, after being to soak 0.5-3 hour in the hydrochloric acid solution of 5-30vol%, percent by volume takes out again, with dehydrated alcohol and deionized water alternately clean 6-10 all over after, at 60-100 ℃ of following drying sample, obtain titanium dioxide nanotube array layer again on the artificial joint surface;
4) artificial joint of above-mentioned surface coverage titanium dioxide nanotube array layer is used irradiation under ultraviolet ray in deionized water or in atmosphere, improve hydrophilic and cell compatibility.The uviol lamp that uses is high voltage mercury lamp, and irradiation time is no less than 10 hours;
5) the titanium dioxide nanotube array layer internal burden bone morphogenetic protein that adopts the centrifugal load technology crossing at last through irradiation under ultraviolet ray, there is artificial joint to place the centrifuge container bottom surface coverage through the titanium dioxide nanotube array layer of irradiation under ultraviolet ray, pour the mixed solution that bone morphogenetic protein and phosphate buffered saline(PBS) are formed again into, liquid level flooded artificial joint to half of centrifuge container or 2/3rds height, and bone morphogenetic protein concentration is 0.1-50mgL
-1, centrifugal under the room temperature (1500-80000Rpm) soaked 0.5-10 hour, took out, get final product bioactive artificial joint of the present invention.
2. the preparation method of using the artificial joint of titanium oxide nanotubes to load bone morphogenetic protein as claimed in claim 1, it is characterized in that it is solvent that moisture organic electrolyte solution adopts ethylene glycol, other effective ingredient is: water 0-10vol% (percent by volume), phosphoric acid 2-10vol% (percent by volume), ammonium fluoride 0.1-0.9wt% (mass percent).
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| CN103046102A (en) * | 2013-01-29 | 2013-04-17 | 哈尔滨工业大学 | Method for preparing macroscopical porous micro-arc oxidation coating based on two-step process |
| CN105903074A (en) * | 2014-09-17 | 2016-08-31 | 上海施必康医疗器械有限公司 | Preparation method for active drug sustained-release coating on surface of craniomaxillofacial repairing titanium mesh |
| CN106110391A (en) * | 2016-08-29 | 2016-11-16 | 福建医科大学附属口腔医院 | A kind of have skeletonization and antibacterial nano drug-carrying device and preparation method thereof concurrently |
| WO2018160480A1 (en) * | 2017-03-02 | 2018-09-07 | Titanium Fusion Technologies, Llc | Composite joint arthroplasty systems and methods |
| US11406502B2 (en) | 2017-03-02 | 2022-08-09 | Optimotion Implants LLC | Orthopedic implants and methods |
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| CN105903074B (en) * | 2014-09-17 | 2018-09-14 | 上海施必康医疗器械有限公司 | Repair the preparation method of titanium net surface active drugs controlled-release coating in cranium jaw face |
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| WO2018160480A1 (en) * | 2017-03-02 | 2018-09-07 | Titanium Fusion Technologies, Llc | Composite joint arthroplasty systems and methods |
| US10456143B2 (en) | 2017-03-02 | 2019-10-29 | Titanium Fusion Technologies, Llc | Composite joint arthroplasty systems and methods |
| US11406502B2 (en) | 2017-03-02 | 2022-08-09 | Optimotion Implants LLC | Orthopedic implants and methods |
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