CN107313092B - A method of on medical metal surface, preparation has Electro-stimulate response composite microcapsule - Google Patents
A method of on medical metal surface, preparation has Electro-stimulate response composite microcapsule Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/02—Electrolytic coating other than with metals with organic materials
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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
- A61L27/28—Materials for coating prostheses
- A61L27/34—Macromolecular materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- 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
- 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
- A61L27/56—Porous materials, e.g. foams or sponges
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Abstract
本发明公开了一种在医用金属表面制备具有电刺激响应复合微囊的方法，本发明属于生物材料技术领域。本发明将多巴胺单体、导电高分子单体和带负电的药物配成的电解液接入三电极电化学系统中，以具有微球模板阵列的医用金属材料为工作电极，在医用金属表面沉积得到多巴胺、导电高分子和药物复合包裹的微球模板，最后将所述微球全部溶解后制得表面复合微囊包被的医用金属材料。本发明实现医用金属材料表面改性，在其表面制备一层功能性导电复合微囊，所述复合微囊不仅能通过电信号控制药物释放并且通过电信号可直接调控干细胞分化；将药物刺激与物理刺激相互协同，既减小了对药物的依赖及其副作用，也提高了医用金属的骨诱导能力。
The invention discloses a method for preparing composite microcapsules with electrical stimulation response on the surface of medical metal, and belongs to the technical field of biomaterials. In the present invention, the electrolyte solution prepared by dopamine monomer, conductive polymer monomer and negatively charged drug is connected to the three-electrode electrochemical system, and the medical metal material with the microsphere template array is used as the working electrode, and deposited on the surface of the medical metal A microsphere template compound-wrapped by dopamine, conductive macromolecule and medicine is obtained, and finally the microspheres are all dissolved to prepare a surface composite microcapsule-coated medical metal material. The invention realizes the surface modification of medical metal materials, and prepares a layer of functional conductive composite microcapsules on the surface. The composite microcapsules can not only control drug release through electrical signals but also directly regulate stem cell differentiation through electrical signals; The physical stimuli cooperate with each other, which not only reduces the dependence on drugs and their side effects, but also improves the osteoinductive ability of medical metals.
Description
Technical field
The invention belongs to technical field of biological materials, more particularly to a kind of preparation on medical metal surface, and there is electro photoluminescence to ring
The method for answering composite microcapsule.
Background technique
The bone defect as caused by many reasons is clinically very common, and the Bone Defect Repari of large area and weight bearing Bone Defect Repari
It is the problem of clinical treatment often faces.Medical metal material is main weight bearing bone renovating material, it is a kind of as biology
The metal or alloy of material, medical metal material are a kind of bio-inert materials, mechanical strength and fatigue resistance with higher
Can, there is good biomechanical property and relevant physical property, however the bioactivity of medical metal material is its use
In a performance indicator to be improved.
The mankind have entered the epoch to organism with high demand, it would be highly desirable to it is raw to develop more activity suitable for implant site
Object material.Bio-medical material develop by direction compound to multiple material, performance complement at present.Process for modifying surface is in life
The application of object material effectively increases the surface quality of medical metal material, improves the implantation effect of implantation material.Therefore, it utilizes
Surface is modified to will be the development trend of medical metal material from now on to improve the performance of medical metal material.
All the time, the self-bone grafting scarce capacity of medical metal implantation bracket be at this stage clinical urgent problem to be solved it
One.Currently, solving the problems, such as that this research is concentrated mainly on one layer of rack surface drug with self-bone grafting ability of imparting implantation and delays
Coating is released, drug degradation polysaccharide coatings are such as loaded with, drug is released as polysaccharide is degraded.But this traditional medicine
There are many limitations for object delivery systme, are such as unable to accurately control to release drug dose, and drug is easy to lose in vivo
Activity.
Compared with conventional medicament delivery systme, drug is controlled specific by outside stimulus response (such as light, electricity, magnetic)
Time, specific position release pre-set given dose drug molecule, are released using the timing of drug, fixed point, quantitative control
It puts, has become the new trend of organizational project and drug release development.Current most of medicine-releasing systems can only realize steady release,
It is strictly a kind of drug sustained release system and is not controlled drug delivery system truly, drug sustained release system generally cannot
It realizes the variation of dosage, therefore cannot achieve real control.
It is furthermore pointed out that although drug therapy is indispensable a part in tissue repair, but drug
Side effect, which is also one, is worth the problem of worrying.For example anticancer drug can not only kill cancer cell, while may also be to tumour
Surrounding normal cell damage and drug resistance.Single physiotherapy (such as electricity treatment) can be to avoid drug side-effect
It influences, but its therapeutic effect is slower.
Summary of the invention
The present invention has electro photoluminescence in order to overcome the shortcomings of the prior art, providing a kind of prepare on medical metal surface
The method for responding composite microcapsule.The present invention, which realizes, is modified medical metal material surface, and a layer function is prepared on its surface and leads
Electric medicament microcapsule, the composite microcapsule can not only pass through electric signal Drug controlled release and by electric signal can direct regulation and control it is dry
Cell differentiation.Under the conditions of same treatment, medicine irritation is mutually cooperateed with physical stimulation, both reduced dependence to drug and
Its side effect, also effectively accelerates Bone Defect Repari.
The present invention is achieved through the following technical solutions:
A method of on medical metal surface, preparation has Electro-stimulate response composite microcapsule, comprising the following steps:
A, on medical metal material surface, formation microsphere template array is spare；
B, it prepares DOPA amine monomers, conductive high polymer monomer and electronegative drug to form electrolyte, the dopamine
The concentration of monomer is 1~20mmol/L, and the conductive high polymer monomer concentration is 0.1~0.5mol/L, the electronegative medicine
The concentration of object is 1~10mmol/L；
C, by step B electrolyte access three-electrode electro Chemical system in, the working electrode, reference electrode with to electricity
Pole constitutes current loop, wherein using the medical metal material with microsphere template as working electrode, sinks on medical metal material
Product obtains the microsphere template of dopamine, conducting polymer and the compound package of drug；
D, the obtained medical metal material of step C is soaked in organic solvent, the microballoon to medical metal material surface
All after dissolution, the coated medical metal material of surface micro-capsule is made, the micro-capsule is by dopamine, conducting polymer and drug
It is compounded to form.
In the preparation method of composite microcapsule coating medical metal material of the present invention, the step A specifically: will be medical
After metal material successively uses acetone and distilled water to be cleaned by ultrasonic, microspheres solution is added dropwise on medical metal material surface, is made after dry
Obtain the medical metal material that surface forms microsphere template array.
In the preparation method of composite microcapsule coating medical metal material of the present invention, with microballoon in the step C
The medical metal material of template is working electrode, and working electrode is connect with electrochemical workstation, is 0.8~2V in voltage range
Oxidizing condition under deposit 0.5~2 hour, be made dopamine, conducting polymer and drug composite coating package microsphere template.
In the preparation method of composite microcapsule coating medical metal material of the present invention, the microballoon is that polystyrene is micro-
Ball or silicon dioxide microsphere.
In the preparation method of composite microcapsule coating medical metal material of the present invention, the conductive high polymer monomer is
Any one of pyrroles, aniline, acetylene and thiophene.
In the preparation method of composite microcapsule coating medical metal material of the present invention, the drug with negative electricity is
Any one of penicillin, nifedipine, dexamethasone, N'-Dimethylguanylguanidine hydrochloride and isoniazid.
In the preparation method of composite microcapsule coating medical metal material of the present invention, the medical metal material is
Any one of titanium, titanium alloy, cobalt alloy, nickel alloy, stainless steel and magnesium alloy.
In the preparation method of composite microcapsule coating medical metal material of the present invention, described is titanium, titanium conjunction to electrode
Any one of gold, cobalt alloy, nickel alloy, stainless steel and platinum.
In the preparation method of composite microcapsule coating medical metal material of the present invention, the reference electrode is that saturation is sweet
It is any in mercury electrode, hydrogen electrode, Ag/AgCl electrode and Hg/HgO electrode.
In the preparation method of composite microcapsule coating medical metal material of the present invention, the organic solvent is tetrahydro furan
It mutters, is any in toluene, chloroform, methylene chloride, vinegar butyl ester and ethylbenzene.
The innovation of the invention consists in that:
1. the present invention has um porous structure in configuration aspects in the composite microcapsule that medical metal surface is prepared, not only
The load capacity of drug can be improved and the microenvironment for being similar to extracellular matrix can be improved for internal cell, be conducive to cell Proliferation
And differentiation.
2. the present invention is doped to conductive polymer with drug under the conditions of electrochemical oxidation using dopamine as pharmaceutical carrier simultaneously
Composite microcapsule is formed in sub- main chain is attached to medical metal material surface；Dopamine (DA) has both in adhesion protein because of its structure
Main component L-3,4- dihydroxyphenylalanine (DOPA) and a small amount of lysine residue, are proved to Adhesion property with super strength,
And dopamine contain a large amount of active function groups may be implemented while making pharmaceutical carrier it is well attached in microsphere template surface.
Meanwhile dopamine (DA) formation poly-dopamine (PDA) process is simple, dopamine can easily be dissolved oxygen in aqueous solution and be aoxidized
Then cause from poly- cross-linking reaction, it is multiple in a kind of substantially any poly-dopamine that solid material surface can form close attachment
Close layer；Poly-dopamine (PDA) has good biocompatibility, and medical metal material surface may be implemented and be modified, improve material
The biocompatibility to osteocyte can be improved to be conducive to sticking for cell in surface hydrophilicity；Poly-dopamine (PDA) table
A large amount of catechols and amino isoreactivity group are contained in face, are also beneficial to the fixation of drug；In addition, poly-dopamine (PDA) is for calcium
The calcification that ion has stronger active force that material surface may be implemented, so that Bone Defect Repari be promoted to treat.
3. the present invention has Electro-stimulate response ability in the composite microcapsule that medical metal surface is prepared；Due in the present invention
The conducting polymer of use has redox characteristic, by taking polypyrrole as an example: polypyrrole is with carbon-carbon single bond and carbon-carbon double bond
The five-ring heterocycles molecule of alternately arranged conjugated structure, conjugated polymer have stronger conductive tendency, therefore to external telecommunications
Number there is better response；The present invention prepares polypyrrole by electrochemical polymerization mode using pyrrole monomer, passes through preparation parameter
Adjustment can prepare the different function polypyrrole material of properity.According to the redox characteristic of polypyrrole: in electrification
It learns under oxidizing condition, polypyrrole main chain is positively charged to need electronegative drug molecule doping to neutralize its electrical property；And electrochemistry also
Under old terms, polypyrrole main chain is not charged, so electronegative drug molecule will release.Therefore, control can be passed through
The size of recovery voltage carrys out the dosage of accurate Drug controlled release.
4. the present invention is conductive due to containing conducting polymer in the composite microcapsule that medical metal surface is prepared, when
When applying voltage to micro-capsule, electric signal can be transmitted to the cell being adhered on micro-capsule by micro-capsule, finally by electric signal tune
Cell differentiation is controlled, reaches and further increases therapeutic effect with drug therapy synergistic effect.
Compared with the prior art, the beneficial effects of the present invention are:
Medical metal material surface is modified 1. the present invention realizes, improves the biocompatibility of medical metal material, especially
Which overcome self-bone grafting scarce capacities existing for existing medical metal implantation bracket, to improve the property of medical metal material
Energy.
2. the present invention provides a kind of new medicine-releasing systems to reach Drug controlled release, improves utilization ratio of drug, reduction machine
Body is chronically at the drug resistance of high drug concentration initiation；The composite microcapsule coating medical metal material that the present invention prepares is being treated
It can be realized using the redox characteristic of conducting polymer in the process and achieve the purpose that Drug controlled release by adjusting voltage.
3. composite microcapsule that the present invention prepares coating medical metal material under the conditions of same treatment by medicine irritation with
Physical stimulation mutually cooperates with, and has both reduced dependence and its side effect to drug, has also played the exclusive advantage of physiotherapy, from
And effectively accelerate Bone Defect Repari.
Detailed description of the invention
Fig. 1 is that the microsphere template array scanning Electronic Speculum of medical metal material surface in the step A of preparation method of the present invention is shown
It is intended to.
Fig. 2 is the composite microcapsule that dopamine made from the step C of preparation method of the present invention, conducting polymer and drug are formed
Coated microsphere template scanning electron microscope schematic diagram.
Fig. 3 is to obtain dopamine, conduction after removing microsphere template using organic solvent in the step D of preparation method of the present invention
The scanning electron microscope schematic diagram on the composite microcapsule coating medical metal material surface that macromolecule and drug are formed.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawing:
Embodiment 1:
A method of on medical metal surface, preparation has Electro-stimulate response composite microcapsule, the specific steps of which are as follows:
A, by medical titanium after over cleaning, polystyrene microsphere solution is added dropwise on its surface, in medical metal material after drying
Expect that surface forms polystyrene microsphere template, will through the above way medical titanium obtained it is spare；
B, DOPA amine monomers, pyrrole monomer and dexamethasone are configured to electrolyte: first by DOPA amine monomers and ground plug rice
Pine mixing, after it is sufficiently reacted, adds pyrrole monomer.In the electrolyte, DOPA amine monomers are 1mmol/L, Bi Kadan
Body 0.1mol/L, the concentration of dexamethasone are 1mmol/L.
C, the B electrolyte walked is put into three-electrode electro Chemical system electrolytic cell: the doctor with polystyrene microsphere template
It is working electrode with titanium, platinum plate is to electrode, and saturated calomel electrode is reference electrode.In the case where voltage is the oxidizing condition of 0.8V
Deposition 0.5 hour, obtains on medical titanium surface by the polystyrene microsphere mould of dopamine, polypyrrole and the compound package of dexamethasone
Plate.
D, medical titanium will be obtained after C step deposition to be soaked in tetrahydrofuran, all dissolve to its surface polystyrene microsphere
The medical titanium that surface is formed composite microcapsule by dopamine, polypyrrole and dexamethasone is obtained afterwards.
Embodiment 2:
A method of on medical metal surface, preparation has Electro-stimulate response composite microcapsule, the specific steps of which are as follows:
A, by medical titanium alloy after over cleaning, polystyrene microsphere solution is added dropwise on its surface, in medical gold after drying
Belong to material surface and form polystyrene microsphere template, will through the above way medical titanium alloy obtained it is spare；
B, DOPA amine monomers, thiophene monomer and chondroitin sulfate are configured to electrolyte: first by DOPA amine monomers and sulfuric acid
Chondroitin mixing, after it is sufficiently reacted, adds thiophene monomer.In the electrolyte, dopamine monomer concentration is 20mmol/
L, the concentration of thiophene is 0.5mol/L, and the concentration of dexamethasone is 10mmol/L.
C, the B electrolyte walked is put into three-electrode electro Chemical system electrolytic cell: the doctor with polystyrene microsphere template
It is working electrode with titanium alloy, platinum plate is to electrode, and saturated calomel electrode is reference electrode.In the oxidizing condition that voltage is 2V
Lower deposition 2 hours, obtains on medical titanium alloy surface by the polystyrene of dopamine, polythiophene and the compound package of chondroitin sulfate
Microsphere template.
D, medical titanium alloy will be obtained after C step deposition to be soaked in methylene chloride, it is whole to its surface polystyrene microsphere
The medical titanium alloy that surface is formed composite microcapsule by dopamine, polythiophene and chondroitin sulfate is obtained after dissolution.
Embodiment: 3:
A method of on medical metal surface, preparation has Electro-stimulate response composite microcapsule, the specific steps of which are as follows:
A, by medical stainless steel after over cleaning, be added dropwise polystyrene microsphere solution on its surface, it is dry after it is medical not
Steel surface of becoming rusty forms polystyrene microsphere template, will through the above way medical stainless steel obtained it is spare；
B, DOPA amine monomers, ethane monomer and penicillin are configured to electrolyte: first mix DOPA amine monomers and penicillin
It closes, after it is sufficiently reacted, adds ethane monomer.In the electrolyte, dopamine monomer concentration is 10mmol/L, acetylene list
The concentration of body is 0.3mol/L, and the concentration of penicillin is 5mmol/L.
C, the B electrolyte walked is put into three-electrode electro Chemical system electrolytic cell: the doctor with polystyrene microsphere template
It is working electrode with stainless steel, platinum plate is to electrode, and saturated calomel electrode is reference electrode.In the oxidation item that voltage is 1.5V
It deposits 1 hour, is obtained on medical stainless steel surface micro- by the polystyrene of dopamine, polyacetylene and the compound package of penicillin under part
Ball template.
D, medical stainless steel will be obtained after C step deposition to be soaked in toluene, all dissolve to its surface polystyrene microsphere
The medical stainless steel that surface is formed composite microcapsule by dopamine, polyacetylene and penicillin is obtained afterwards.
Embodiment 4:
The operation of the present embodiment is substantially the same manner as Example 1, only by conductive high polymer monomer used in example 1 by
Pyrroles changes aniline into.
Embodiment 5:
The operation of the present embodiment is substantially the same manner as Example 1, only by conductive high polymer monomer used in example 1 by
Pyrroles changes acetylene into.
Embodiment 6:
The operation of the present embodiment is substantially the same manner as Example 1, only by conductive high polymer monomer used in example 1 by
Pyrroles changes thiophene into.
Embodiment 7:
The operation of the present embodiment is substantially the same manner as Example 1, only by medical metal material used in example 1 by curing
Medical titanium alloy is changed into titanium.
Embodiment 8:
The operation of the present embodiment is substantially the same manner as Example 1, only by medical metal material used in example 1 by curing
Medical stainless steel is changed into titanium.
Embodiment 9:
The operation of the present embodiment is substantially the same manner as Example 1, only by medical metal material used in example 1 by curing
Medical magnesium alloy is changed into titanium.
Embodiment 10:
The operation of the present embodiment is substantially the same manner as Example 1, only by electronegative drug used in example 1 by ground
Sai meter Song changes penicillin into.
Embodiment 11:
The operation of the present embodiment is substantially the same manner as Example 1, only by electronegative drug used in example 1 by ground
Sai meter Song changes chondroitin sulfate into.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (9)
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| CN114250485B (en) * | 2021-11-26 | 2023-04-07 | 中国华能集团清洁能源技术研究院有限公司 | Nickel-molybdenum-iron hydrogen evolution electrode with ordered porous structure, preparation method and application |
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