CN106581766A - Preparation method of collagen-hydroxyapatite stent containing nanometer manganese dioxide - Google Patents
Preparation method of collagen-hydroxyapatite stent containing nanometer manganese dioxide Download PDFInfo
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- CN106581766A CN106581766A CN201610961711.4A CN201610961711A CN106581766A CN 106581766 A CN106581766 A CN 106581766A CN 201610961711 A CN201610961711 A CN 201610961711A CN 106581766 A CN106581766 A CN 106581766A
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L27/44—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix
- A61L27/446—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix with other specific inorganic fillers other than those covered by A61L27/443 or A61L27/46
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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
- A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L27/44—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix
- A61L27/46—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix with phosphorus-containing inorganic fillers
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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
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
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- A—HUMAN NECESSITIES
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- 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
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- 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
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- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention relates to a preparation method of a collagen-hydroxyapatite stent containing nanometer manganese dioxide. The nanometer manganese dioxide is prepared through a liquid phase reduction reaction; and the nanometer manganese dioxide and a collagen-hydroxyapatite solution are uniformly mixed, and are subjected to one-step freeze drying and crosslinking to prepare and obtain the collagen-hydroxyapatite stent, wherein the concentration range of the nanometer manganese dioxide is 10 ug/ml to 50ug/ml; and the particle diameter of the nanometer manganese dioxide is 10 to 30nm. The stent provided by the invention has the advantages that required materials are simple; no complicated technical requirements and no high-end equipment requirements are needed; the cost is low; the popularization is easy; a reasonable nanometer manganese dioxide slow-release system is provided for a wound surface; the long-time effective medicine slow release is provided for the wound surface; and the medicine concentration on the wound surface keeps balanced, effective and non-superfluous.
Description
Technical field
The invention belongs to technical field of biological materials, and in particular to a kind of ash of the collagen-hydroxyl phosphorus containing nano-manganese dioxide
The preparation method of stone support.
Background technology
Hydroxyapatite and collagen protein are topmost inorganic and organic principles in nature bone, and all have good life
Thing characteristic, but there is when being used alone different defects again, it is difficult to meet requirement of the organizational project to biomaterial performance, with
Collagen protein preferably make use of the caking property of collagen protein and overcome hydroapatite particles with hydroxyapatite compound
Mobility.
Nano-manganese dioxide has excellent conductivity of heat, electric conductivity, surface activity and catalytic performance, in optics, catalysis, micro-
The fields such as electronics, bio-sensing, antibacterial have huge using value.The nano-manganese dioxide mealiness of different-shape can be different,
As particle diameter is less, narrow particle size distribution ball shaped nano manganese dioxide powder has good anti-microbial property and electric conductivity.
Due to the high bioactivity of nano-manganese dioxide, when applying it in organizational project, wound surface or mesh are discharged into
Mark organ, it preferentially can be captured by the associated protein in wound exudate or tissue, chloride ion and group, cause nano-manganese dioxide
Granule is in some position high concentration abnormal aggregations, although can effectively participate in antibacterial, but these superfluous nano-manganese dioxides will be
In epidermis cell, macrophage, fibroblast, aggregation, causes the apoptosis of cell, ultimately results in the disunion of wound surface or prolong
Heal late.Generally speaking, immoderate use or uncontrolled release nano-manganese dioxide will certainly run counter to desire, to wound surface
Reparation is no advantage.Therefore, safely and effectively rational slow-releasing system is needed using nano-manganese dioxide, provide length for wound surface
Phase effective medicament slow release, keeps the drug level of wound surface balanced effective and not superfluous.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of collagen-hydroxyapatite support containing nano-manganese dioxide
Preparation method, is to prepare nano-manganese dioxide by Liquid reduction reaction process, is then mixed homogeneously with collagen-hydroxyapatite solution
One-step method lyophilizing it is crosslinked preparation and becomes Metal pylon afterwards, the novel nano manganese dioxide prepared with antibacterial, safety is biological
Material.
The present invention is achieved by the following technical solutions：
(1) manganese sulfate and potassium peroxydisulfate are adopted and is added soluble starch and is carried out for dispersant Liquid reduction reaction process and prepare and received
Rice sol of manganese dioxide；Reaction temperature is 30 DEG C -45 DEG C；
(2) by the microwave heating reaction in confined conditions of nano-manganese dioxide colloidal sol, first under 250～350W microwave powers
2～2.5min of reaction, then 2.5～3min is reacted under 100～150W microwave powers, nanometer titanium dioxide manganese solution is obtained；
(3) NTx albumen and the hydroxyapatite that cattle heel string is originated is according to 9：1 mass ratio is dissolved into 0.5mol/L
Acetic acid solution in, mix 4h after adding a certain amount of manganese solution to nanometer titanium dioxide as aimed concn with 10ppm, be subsequently adding total
The glutaraldehyde of the 0.5% of quality is simultaneously mixed, and obtains the collagen-hydroxyapatite containing nano-manganese dioxide that mass fraction is 0.5%
Nano-manganese dioxide, collagen-hydroxyapatite solution are injected the mould of 4cm × 4cm, are freezed 2 hours at -20 DEG C by solution,
Then lyophilizing obtains collagen-hydroxyapatite support of the porous containing nano-manganese dioxide that thickness is 2mm for 24 hours.Nano-silica
The concentration range for changing manganese is 10ug/ml-50ug/ml, and the particle diameter of nano-manganese dioxide particle is 10-30nm.
Preferably, in the step (2), the condition of microwave heating reaction is：First react under 300W microwave powers
2.25min, then 2.75min is reacted under 120W microwave powers.
The present invention has the advantages that：
1. the present invention replaces traditional hydro-thermal method to prepare nano-manganese dioxide using microwave-hydrothermal method, with process is simple,
With short production cycle, energy-conserving and environment-protective, the features such as having a safety feature.
2. the nano-manganese dioxide granule using the method preparation is spherical in shape, uniform in size, good dispersion.
3. the support material requested of the present invention is simple, without the need for complicated technical requirements and high-end device requirement, low cost,
It is easy to spread.
4. support of the present invention provides rational nano-manganese dioxide slow-releasing system for wound surface, provides permanently effective for wound surface
Medicament slow release, keep the drug level of wound surface balanced effective and not superfluous.
Specific embodiment
The present invention is further illustrated with reference to embodiment.
Embodiment 1
A kind of preparation method of the collagen-hydroxyapatite support containing nano-manganese dioxide is realized by procedure below
's：
(1) manganese sulfate and potassium peroxydisulfate are adopted and is added soluble starch and is carried out for dispersant Liquid reduction reaction process and prepare and received
Rice sol of manganese dioxide；With the addition of soluble starch be the 3% of tetra chlorauric acid quality；Reaction temperature is 40 DEG C；
(2) nano-manganese dioxide colloidal sol stirring 10min is taken, microwave heating treatment (selects the auspicious swan in Beijing under airtight condition
HX-300A computer microwaves ultrasound combinatorial compound instrument is microwave source), 2.25min is reacted under 300W microwave powers first, then in 120W
2.75min is reacted under microwave power, obtain nanometer titanium dioxide manganese solution；
(3) NTx albumen and the hydroxyapatite that cattle heel string is originated is according to 9：1 mass ratio is dissolved into 0.5mol/L
Acetic acid solution in, mix 4h after adding a certain amount of manganese solution to nanometer titanium dioxide as aimed concn with 10ppm, be subsequently adding total
The glutaraldehyde of the 0.5% of quality is simultaneously mixed, and obtains the collagen-hydroxyapatite containing nano-manganese dioxide that mass fraction is 0.5%
Nano-manganese dioxide, collagen-hydroxyapatite solution are injected the mould of 4cm × 4cm, are freezed 2 hours at -20 DEG C by solution,
Then lyophilizing obtains the collagen-hydroxyapatite support containing nano-manganese dioxide that thickness is 2mm for 24 hours.Nano-manganese dioxide
Concentration range be 10ug/ml-50ug/ml, the particle diameter of nano-manganese dioxide particle is 10-30nm.
Embodiment 2
A kind of preparation method of the collagen-hydroxyapatite support containing nano-manganese dioxide is realized by procedure below
's：
(1) manganese sulfate and potassium peroxydisulfate are adopted and is added soluble starch and is carried out for dispersant Liquid reduction reaction process and prepare and received
Rice sol of manganese dioxide；With the addition of soluble starch be the 3% of tetra chlorauric acid quality；Reaction temperature is 30 DEG C；
(2) nano-manganese dioxide colloidal sol stirring 10min is taken, microwave heating treatment (selects the auspicious swan in Beijing under airtight condition
HX-300A computer microwaves ultrasound combinatorial compound instrument is microwave source), 2.5min is reacted under 250W microwave powers first, then in 150W
2.5min is reacted under microwave power, obtain nanometer titanium dioxide manganese solution；
(3) NTx albumen and the hydroxyapatite that cattle heel string is originated is according to 9：1 mass ratio is dissolved into 0.5mol/L
Acetic acid solution in, mix 4h after adding a certain amount of manganese solution to nanometer titanium dioxide as aimed concn with 10ppm, be subsequently adding total
The glutaraldehyde of the 0.5% of quality is simultaneously mixed, and it is 0.5% containing nano-manganese dioxide, collagen-hydroxyapatite to obtain mass fraction
Nano-manganese dioxide, collagen-hydroxyapatite solution are injected the mould of 4cm × 4cm, are freezed 2 hours at -20 DEG C by solution,
Then lyophilizing obtains collagen-hydroxyapatite support of the porous containing nano-manganese dioxide that thickness is 2mm for 24 hours.Nano-silica
The concentration range for changing manganese is 10ug/ml-50ug/ml, and the particle diameter of nano-manganese dioxide particle is 10-30nm.
Although above-mentioned be described to the specific embodiment of the present invention in conjunction with the embodiments, not to present invention protection
The restriction of scope, one of ordinary skill in the art should be understood that on the basis of technical scheme, those skilled in the art
The various modifications made by creative work need not be paid or deformation are still within protection scope of the present invention.
Claims (2)
1. a kind of preparation method of the collagen-hydroxyapatite support containing nano-manganese dioxide, is characterized in that, step is as follows：
(1) adopting manganese sulfate and potassium peroxydisulfate and adding soluble starch carries out Liquid reduction reaction process preparation nanometer two for dispersant
Manganese oxide colloidal sol；Reaction temperature is 30 DEG C -45 DEG C；
(2) by the microwave heating reaction in confined conditions of nano-manganese dioxide colloidal sol, first react under 250～350W microwave powers
2～2.5min, then 2.5～3min is reacted under 100～150W microwave powers, nanometer titanium dioxide manganese solution is obtained；
(3) by cattle NTx albumen and shitosan according to 9：1 mass ratio is dissolved in the acetic acid solution of 0.5mol/L, with
10ppm mixes 4h after being added to nanometer titanium dioxide manganese solution for aimed concn, be subsequently adding gross mass 0.5% glutaraldehyde simultaneously
Mix, obtain mass fraction be 0.5% containing nano-manganese dioxide, collagen-hydroxyapatite solution, by nano-manganese dioxide,
Collagen-hydroxyapatite solution injects the mould of 4cm × 4cm, freezes 2 hours at -20 DEG C, and then lyophilizing obtains thickness in 24 hours
Spend collagen-hydroxyapatite support of the porous containing nano-manganese dioxide for 2mm.
2. the preparation method of a kind of collagen-hydroxyapatite support containing nano-manganese dioxide according to claim 1, its
It is characterized in that：The concentration range of nano-manganese dioxide is 10ug/ml-50ug/ml, and the particle diameter of nano-manganese dioxide particle is 10-
30nm。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108636375A (en) * | 2018-06-11 | 2018-10-12 | 四会市恒星智能科技有限公司 | Absorption carrier and preparation method thereof for metal recovery in waste and old lithium ion battery |
| CN112807488A (en) * | 2019-11-18 | 2021-05-18 | 中国科学院上海硅酸盐研究所 | Ion adsorption type manganese dioxide coating with function of promoting bone differentiation and preparation method and application thereof |
| CN113952919A (en) * | 2021-11-19 | 2022-01-21 | 西北师范大学 | Preparation method of manganese oxide coated hydroxyapatite nanowire |
| CN115444981A (en) * | 2021-06-09 | 2022-12-09 | 中国科学院上海硅酸盐研究所 | Hydroxyapatite-manganese dioxide composite coating with biological oxidation resistance and bone-promoting performance and preparation method and application thereof |
-
2016
- 2016-11-04 CN CN201610961711.4A patent/CN106581766A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108636375A (en) * | 2018-06-11 | 2018-10-12 | 四会市恒星智能科技有限公司 | Absorption carrier and preparation method thereof for metal recovery in waste and old lithium ion battery |
| CN112807488A (en) * | 2019-11-18 | 2021-05-18 | 中国科学院上海硅酸盐研究所 | Ion adsorption type manganese dioxide coating with function of promoting bone differentiation and preparation method and application thereof |
| CN112807488B (en) * | 2019-11-18 | 2022-04-08 | 中国科学院上海硅酸盐研究所 | Ion adsorption type manganese dioxide coating with function of promoting bone differentiation and preparation method and application thereof |
| CN115444981A (en) * | 2021-06-09 | 2022-12-09 | 中国科学院上海硅酸盐研究所 | Hydroxyapatite-manganese dioxide composite coating with biological oxidation resistance and bone-promoting performance and preparation method and application thereof |
| CN115444981B (en) * | 2021-06-09 | 2023-11-10 | 中国科学院上海硅酸盐研究所 | Hydroxyapatite-manganese dioxide composite coating with biological antioxidation and bone promoting properties, and preparation method and application thereof |
| CN113952919A (en) * | 2021-11-19 | 2022-01-21 | 西北师范大学 | Preparation method of manganese oxide coated hydroxyapatite nanowire |
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