CN106563169A - Preparation method for preparing nano silicon dioxide-contained collagen-hydroxyapatite bracket - Google Patents
Preparation method for preparing nano silicon dioxide-contained collagen-hydroxyapatite bracket Download PDFInfo
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- CN106563169A CN106563169A CN201610969079.8A CN201610969079A CN106563169A CN 106563169 A CN106563169 A CN 106563169A CN 201610969079 A CN201610969079 A CN 201610969079A CN 106563169 A CN106563169 A CN 106563169A
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- nano
- silicon dioxide
- collagen
- nano silicon
- hydroxyapatite
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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
- A61L27/446—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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/12—Nanosized materials, e.g. nanofibres, nanoparticles, nanowires, nanotubes; Nanostructured surfaces
Abstract
The invention relates to a preparation method for preparing a nano silicon dioxide-contained collagen-hydroxyapatite bracket. According to the technical scheme of the invention, the nano silicon dioxide is prepared through the liquid-phase reduction reaction. The prepared nano silicon dioxide is uniformly mixed up with a collagen-hydroxyapatite solution, and then a nano silicon dioxide-contained collagen-hydroxyapatite bracket is obtained through the one-step freeze-drying and crosslinking process. The concentration range of the nano silicon dioxide is 10 mug/ml to 50 mug/ml. The particle sizes of the nano silicon dioxide are within the range of 10-30 nm. The materials of the bracket are simple, and the bracket can be prepared without any complicated technical requirements or high-end equipment requirements. Meanwhile, the method is low in cost and easy to popularize. The method provides a reasonable sustained-release system of nano silicon dioxide for wounds. Meanwhile, the method realizes the long-term and effective sustained release of drugs for wounds, and ensures the drug concentration of a wound to be balanced, valid and not excessive.
Description
Technical field
The invention belongs to technical field of biological materials, and in particular to a kind of collagen-hydroxyl phosphorus ash of nano-silica-containing
The preparation method of stone support.
Background technology
Hydroxyapatite and collagen 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 preferably make use of the caking property of collagen and overcome hydroapatite particles with hydroxyapatite compound
Mobility.
Nano silicon has excellent conductivity of heat, electric conductivity, surface-active and catalytic performance, in optics, catalysis, micro-
The fields such as electronics, bio-sensing, antibacterial have huge using value.The nano-silica powder performance of different-shape is different,
As particle diameter is less, narrow particle size distribution spherical nano-silicon dioxide powder has good anti-microbial property and electric conductivity.
Due to the high bioactivity of nano silicon, when applying it in organizational project, the surface of a wound or mesh are discharged into
Mark organ, it preferentially can be captured by the GAP-associated protein GAP in wound exudate or tissue, chlorion and group, cause nano silicon
Particle is in some position high concentration abnormal aggregations, although can effectively participate in antibacterial, but these superfluous nano silicons will be
Aggregation, causes the apoptosis of cell in epidermal cell, macrophage, fibroblast, ultimately results in the disunion of the surface of a wound or prolongs
Healing late.Generally speaking, immoderate use or uncontrolled release nano silicon will certainly run counter to desire, to the surface of a wound
Reparation is no advantage.Therefore, safely and effectively using nano silicon rational slow-releasing system is needed, for the surface of a wound length is provided
Phase effective medicament slow release, keeps the drug concentration of the surface of a wound 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 of nano-silica-containing
Preparation method, is to prepare nano silicon by Liquid reduction reaction process, is then well mixed with collagen-hydroxyapatite solution
Afterwards one-step method is freezed and is crosslinked preparation becomes Metal pylon, and the novel nano silica prepared with antibacterial, safety is biological
Material.
The present invention is achieved by the following technical solutions：
(1) adopting sodium metasilicate and ammonium nitrate and adding soluble starch carries out Liquid reduction reaction process preparation nanometer for dispersant
Silicon dioxide gel；Reaction temperature is 30 DEG C -45 DEG C；
(2) nano silicon dioxide sol heating using microwave in confined conditions is reacted, first under 250～350W microwave powers
2～2.5min of reaction, then 2.5～3min is reacted under 100～150W microwave powers, nanosilica solution is obtained；
(3) NTx albumen ox heel string originated and hydroxyapatite are according to 9：1 mass ratio is dissolved into 0.5mol/L
Acetic acid solution in, with 10ppm as aimed concn add it is a certain amount of mix 4h to after nanosilica solution, be subsequently adding total
The glutaraldehyde of the 0.5% of quality is simultaneously mixed, and obtains the nano-silica-containing collagen-hydroxyapatite that mass fraction is 0.5%
Solution, by nano silicon, collagen-hydroxyapatite solution injects the mould of 4cm × 4cm, freezes 2 hours at -20 DEG C,
Then the collagen-hydroxyapatite support for obtaining the porous nano-silica-containing that thickness is 2mm for 24 hours is freezed.Nano-silica
The concentration range of SiClx is 10ug/ml-50ug/ml, and the particle diameter of nano-silicon dioxide particle is 10-30nm.
Preferably, the condition of heating using microwave 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 nano silicon 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 silicon dioxide particle 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 silicon slow-releasing system for the surface of a wound, provides permanently effective for the surface of a wound
Medicament slow release, keep the drug concentration of the surface of a wound 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 of nano-silica-containing is realized by procedure below
's：
(1) adopting sodium metasilicate and ammonium nitrate and adding soluble starch carries out Liquid reduction reaction process preparation nanometer for dispersant
Silicon dioxide gel；With the addition of soluble starch be the 3% of tetra chlorauric acid quality；Reaction temperature is 40 DEG C；
(2) nano silicon dioxide 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, nanosilica solution is obtained；
(3) NTx albumen ox heel string originated and hydroxyapatite are according to 9：1 mass ratio is dissolved into 0.5mol/L
Acetic acid solution in, with 10ppm as aimed concn add it is a certain amount of mix 4h to after nanosilica solution, be subsequently adding total
The glutaraldehyde of the 0.5% of quality is simultaneously mixed, and obtains the nano-silica-containing collagen-hydroxyapatite that mass fraction is 0.5%
Solution, by nano silicon, collagen-hydroxyapatite solution injects the mould of 4cm × 4cm, freezes 2 hours at -20 DEG C,
Then the collagen-hydroxyapatite support for obtaining the nano-silica-containing that thickness is 2mm for 24 hours is freezed.Nano silicon
Concentration range be 10ug/ml-50ug/ml, the particle diameter of nano-silicon dioxide particle is 10-30nm.
Embodiment 2
A kind of preparation method of the collagen-hydroxyapatite support of nano-silica-containing is realized by procedure below
's：
(1) adopting sodium metasilicate and ammonium nitrate and adding soluble starch carries out Liquid reduction reaction process preparation nanometer for dispersant
Silicon dioxide gel；With the addition of soluble starch be the 3% of tetra chlorauric acid quality；Reaction temperature is 30 DEG C；
(2) nano silicon dioxide 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, nanosilica solution is obtained；
(3) NTx albumen ox heel string originated and hydroxyapatite are according to 9：1 mass ratio is dissolved into 0.5mol/L
Acetic acid solution in, with 10ppm as aimed concn add it is a certain amount of mix 4h to after nanosilica solution, be subsequently adding total
The glutaraldehyde of the 0.5% of quality is simultaneously mixed, and obtains nano-silica-containing, collagen-hydroxyapatite that mass fraction is 0.5%
Solution, by nano silicon, collagen-hydroxyapatite solution the mould of 4cm × 4cm is injected, and is freezed 2 hours at -20 DEG C,
Then the collagen-hydroxyapatite support for obtaining the porous nano-silica-containing that thickness is 2mm for 24 hours is freezed.Nano-silica
The concentration range of SiClx is 10ug/ml-50ug/ml, and the particle diameter of nano-silicon 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 of nano-silica-containing, is characterized in that, step is as follows：
(1) sodium metasilicate and ammonium nitrate are adopted and is added soluble starch and is carried out Liquid reduction reaction process for dispersant and prepare nano-silica
SiClx colloidal sol；Reaction temperature is 30 DEG C -45 DEG C；
(2) nano silicon dioxide sol heating using microwave in confined conditions is reacted, is first reacted under 250～350W microwave powers
2～2.5min, then 2.5～3min is reacted under 100～150W microwave powers, nanosilica solution is obtained；
(3) by ox 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 nanosilica solution for aimed concn and mixes 4h, be subsequently adding gross mass 0.5% glutaraldehyde simultaneously
Mix, obtain nano-silica-containing, collagen-hydroxyapatite solution that mass fraction is 0.5%, by nano silicon,
Collagen-hydroxyapatite solution injects the mould of 4cm × 4cm, freezes at -20 DEG C 2 hours, then freezes and obtains thickness in 24 hours
Spend the collagen-hydroxyapatite support of the porous nano-silica-containing for 2mm.
2. the preparation method of the collagen-hydroxyapatite support of a kind of nano-silica-containing according to claim 1, its
It is characterized in that：The concentration range of nano silicon is 10ug/ml-50ug/ml, and the particle diameter of nano-silicon dioxide particle is 10-
30nm。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610969079.8A CN106563169A (en) | 2016-11-04 | 2016-11-04 | Preparation method for preparing nano silicon dioxide-contained collagen-hydroxyapatite bracket |
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| CN201610969079.8A CN106563169A (en) | 2016-11-04 | 2016-11-04 | Preparation method for preparing nano silicon dioxide-contained collagen-hydroxyapatite bracket |
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| CN106563169A true CN106563169A (en) | 2017-04-19 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107296976A (en) * | 2017-06-27 | 2017-10-27 | 郑州汉东科技有限公司 | A kind of Medical multifunctional bleeding-stopping dressing and preparation method thereof |
| CN107661540A (en) * | 2017-10-31 | 2018-02-06 | 华南理工大学 | A kind of method that high-strength hydroxylapatite chitosan SiO 2 hybrid support is prepared using 3D printing |
-
2016
- 2016-11-04 CN CN201610969079.8A patent/CN106563169A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107296976A (en) * | 2017-06-27 | 2017-10-27 | 郑州汉东科技有限公司 | A kind of Medical multifunctional bleeding-stopping dressing and preparation method thereof |
| CN107661540A (en) * | 2017-10-31 | 2018-02-06 | 华南理工大学 | A kind of method that high-strength hydroxylapatite chitosan SiO 2 hybrid support is prepared using 3D printing |
| CN107661540B (en) * | 2017-10-31 | 2020-12-22 | 华南理工大学 | Method for preparing high-strength hydroxyapatite-chitosan-silicon dioxide hybrid scaffold by using 3D printing |
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