CN106581767A - Preparation method of collagen-hydroxyapatite stent containing nanometer fluorapatite - Google Patents
Preparation method of collagen-hydroxyapatite stent containing nanometer fluorapatite Download PDFInfo
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- CN106581767A CN106581767A CN201610962865.5A CN201610962865A CN106581767A CN 106581767 A CN106581767 A CN 106581767A CN 201610962865 A CN201610962865 A CN 201610962865A CN 106581767 A CN106581767 A CN 106581767A
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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
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/455—Phosphates containing halogen
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/112—Phosphorus-containing compounds, e.g. phosphates, phosphonates
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/60—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special physical form
- A61L2300/602—Type of release, e.g. controlled, sustained, slow
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- Oral & Maxillofacial Surgery (AREA)
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- Engineering & Computer Science (AREA)
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- Animal Behavior & Ethology (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
The invention relates to a preparation method of a collagen-hydroxyapatite stent containing nanometer fluorapatite. The nanometer fluorapatite is prepared through a liquid phase reduction reaction; and the nanometer fluorapatite 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 fluorapatite is 10 ug/ml to 50ug/ml; and the particle diameter of the nanometer fluorapatite 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 fluorapatite 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 nanometer fluor-apatite
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 different defects again when being used alone, 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.
Nanometer fluor-apatite 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 nanometer fluor-apatite mealiness of different-shape can be different,
As particle diameter is less, narrow particle size distribution ball shaped nano fluor-apatite powder has good anti-microbial property and electric conductivity.
Due to the high bioactivity of nanometer fluor-apatite, 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 a nanometer fluor-apatite
Granule is in some position high concentration abnormal aggregations, although can effectively participate in antibacterial, but the nanometer fluor-apatite of these surpluses will be
Aggregation, causes the apoptosis of cell in epidermis cell, macrophage, fibroblast, ultimately results in the disunion of wound surface or prolongs
Healing late.Generally speaking, immoderate use or uncontrolled release nanometer fluor-apatite will certainly run counter to desire, to wound surface
Reparation is no advantage.Therefore, safely and effectively using nanometer fluor-apatite rational slow-releasing system is needed, for wound surface length is provided
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 nanometer fluor-apatite
Preparation method, is to prepare nanometer fluor-apatite by Liquid reduction reaction process, is then mixed homogeneously with collagen-hydroxyapatite solution
One-step method lyophilizing and it is crosslinked preparation and becomes Metal pylon afterwards, the novel nano fluor-apatite prepared with antibacterial, safety is biological
Material.
The present invention is achieved by the following technical solutions：
(1) adopting ammonium fluoride and diammonium phosphate, calcium nitrate and adding glucose carries out Liquid reduction reaction process for dispersant
Prepare nanometer fluor-apatite colloidal sol；Reaction temperature is 30 DEG C -45 DEG C；
(2) by the microwave heating reaction in confined conditions of nanometer fluor-apatite 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 fluor-apatite solution is obtained；
(3) NTx albumen cattle heel string originated and hydroxyapatite are according to 9：1 mass ratio is dissolved into 0.5mol/L
Acetic acid solution in, added as aimed concn with 10ppm and mix 4h after a certain amount of fluor-apatite solution to nanometer, be subsequently adding total
The glutaraldehyde of the 0.5% of quality is simultaneously mixed, and obtains the collagen-hydroxyapatite of fluor-apatite containing nanometer that mass fraction is 0.5%
Solution, by nanometer fluor-apatite, collagen-hydroxyapatite solution injects the mould of 4cm × 4cm, freezes 2 hours at -20 DEG C,
Then lyophilizing obtains collagen-hydroxyapatite support of the porous containing nanometer fluor-apatite that thickness is 2mm for 24 hours.Nanometer fluorine phosphorus
The concentration range of lime stone is 10ug/ml-50ug/ml, and the particle diameter of nanometer fluor-apatite particle is 10-30nm.
Preferably, the condition of microwave heating reaction is in the step (2)：First react under 300W microwave powers
2.25min, then react 2.75min under 120W microwave powers.
The present invention has the advantages that：
1. the present invention replaces traditional hydro-thermal method to prepare nanometer fluor-apatite 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 nanometer fluor-apatite 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 nanometer fluor-apatite 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 nanometer fluor-apatite is realized by procedure below
's：
(1) adopting ammonium fluoride and diammonium phosphate, calcium nitrate and adding glucose carries out Liquid reduction reaction process for dispersant
Prepare nanometer fluor-apatite colloidal sol；Plus the addition of glucose is the 3% of tetra chlorauric acid quality；Reaction temperature is 40 DEG C；
(2) a nanometer fluor-apatite 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), first 2.25min is reacted under 300W microwave powers, then in 120W
2.75min is reacted under microwave power, a nanometer fluor-apatite solution is obtained；
(3) NTx albumen cattle heel string originated and hydroxyapatite are according to 9：1 mass ratio is dissolved into 0.5mol/L
Acetic acid solution in, added as aimed concn with 10ppm and mix 4h after a certain amount of fluor-apatite solution to nanometer, be subsequently adding total
The glutaraldehyde of the 0.5% of quality is simultaneously mixed, and obtains the collagen-hydroxyapatite of fluor-apatite containing nanometer that mass fraction is 0.5%
Solution, by nanometer fluor-apatite, collagen-hydroxyapatite solution injects the mould of 4cm × 4cm, freezes 2 hours at -20 DEG C,
Then lyophilizing obtains the collagen-hydroxyapatite support containing nanometer fluor-apatite that thickness is 2mm for 24 hours.Nanometer fluor-apatite
Concentration range be 10ug/ml-50ug/ml, the particle diameter of nanometer fluor-apatite particle is 10-30nm.
Embodiment 2
A kind of preparation method of the collagen-hydroxyapatite support containing nanometer fluor-apatite is realized by procedure below
's：
(1) adopting ammonium fluoride and diammonium phosphate, calcium nitrate and adding glucose carries out Liquid reduction reaction process for dispersant
Prepare nanometer fluor-apatite colloidal sol；Plus the addition of glucose is the 3% of tetra chlorauric acid quality；Reaction temperature is 30 DEG C；
(2) a nanometer fluor-apatite 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), first 2.5min is reacted under 250W microwave powers, then in 150W
2.5min is reacted under microwave power, a nanometer fluor-apatite solution is obtained；
(3) NTx albumen cattle heel string originated and hydroxyapatite are according to 9：1 mass ratio is dissolved into 0.5mol/L
Acetic acid solution in, added as aimed concn with 10ppm and mix 4h after a certain amount of fluor-apatite solution to nanometer, be subsequently adding total
The glutaraldehyde of the 0.5% of quality is simultaneously mixed, and obtains fluor-apatite containing nanometer, collagen-hydroxyapatite that mass fraction is 0.5%
Solution, by nanometer fluor-apatite, collagen-hydroxyapatite solution the mould of 4cm × 4cm is injected, and is freezed 2 hours at -20 DEG C,
Then lyophilizing obtains collagen-hydroxyapatite support of the porous containing nanometer fluor-apatite that thickness is 2mm for 24 hours.Nanometer fluorine phosphorus
The concentration range of lime stone is 10ug/ml-50ug/ml, and the particle diameter of nanometer fluor-apatite 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 nanometer fluor-apatite, is characterized in that, step is as follows：
(1) adopting ammonium fluoride and diammonium phosphate, calcium nitrate and adding glucose carries out Liquid reduction reaction process preparation for dispersant
Nanometer fluor-apatite colloidal sol；Reaction temperature is 30 DEG C -45 DEG C；
(2) by the microwave heating reaction in confined conditions of nanometer fluor-apatite colloidal sol, first react under 250～350W microwave powers
2～2.5min, then 2.5～3min is reacted under 100～150W microwave powers, nanometer fluor-apatite 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 is added to after nanometer fluor-apatite solution for aimed concn and mixes 4h, be subsequently adding gross mass 0.5% glutaraldehyde simultaneously
Mix, obtain fluor-apatite containing nanometer, collagen-hydroxyapatite solution that mass fraction is 0.5%, by nanometer fluor-apatite,
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 nanometer fluor-apatite for 2mm.
2. the preparation method of a kind of collagen-hydroxyapatite support containing nanometer fluor-apatite according to claim 1, its
It is characterized in that：The concentration range of nanometer fluor-apatite is 10ug/ml-50ug/ml, and the particle diameter of nanometer fluor-apatite particle is 10-
30nm。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610962865.5A CN106581767A (en) | 2016-11-04 | 2016-11-04 | Preparation method of collagen-hydroxyapatite stent containing nanometer fluorapatite |
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| CN201610962865.5A CN106581767A (en) | 2016-11-04 | 2016-11-04 | Preparation method of collagen-hydroxyapatite stent containing nanometer fluorapatite |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112158820A (en) * | 2020-09-06 | 2021-01-01 | 桂林理工大学 | Preparation method and application of fluorapatite solid solution |
-
2016
- 2016-11-04 CN CN201610962865.5A patent/CN106581767A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112158820A (en) * | 2020-09-06 | 2021-01-01 | 桂林理工大学 | Preparation method and application of fluorapatite solid solution |
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