CN106552291A - A kind of preparation method of the collagen hydroxyapatite support containing nano nickel sulphide - Google Patents

A kind of preparation method of the collagen hydroxyapatite support containing nano nickel sulphide Download PDF

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CN106552291A
CN106552291A CN201610962861.7A CN201610962861A CN106552291A CN 106552291 A CN106552291 A CN 106552291A CN 201610962861 A CN201610962861 A CN 201610962861A CN 106552291 A CN106552291 A CN 106552291A
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nano nickel
nickel sulphide
collagen
sulphide
solution
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王淑芳
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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
    • A61L2300/10—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
    • 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
    • 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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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Transplantation (AREA)
  • Epidemiology (AREA)
  • Dermatology (AREA)
  • Animal Behavior & Ethology (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Medicinal Preparation (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The present invention relates to a kind of preparation method of the collagen hydroxyapatite support containing nano nickel sulphide, nano nickel sulphide is obtained by Liquid reduction reaction process, after which is mixed homogeneously with collagen hydroxyapatite solution one-step method lyophilizing and crosslinking prepare, wherein the concentration range of nano nickel sulphide is 10ug/ml 50ug/ml, and the particle diameter of nano nickel sulphide particle is 10 30nm.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, rational nano nickel sulphide slow-releasing system is provided for wound surface, permanently effective medicament slow release is provided for wound surface, keep the drug level of wound surface balanced effective and not superfluous.

Description

A kind of preparation method of the collagen-hydroxyapatite support containing nano nickel sulphide
Technical field
The invention belongs to technical field of biological materials, and in particular to a kind of collagen-hydroxyapatite containing nano nickel sulphide The preparation method of 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 nickel sulphide has excellent conductivity of heat, electric conductivity, surface activity and catalytic performance, in optics, catalysis, micro- electricity The fields such as son, bio-sensing, antibacterial have huge using value.The nano nickel sulphide mealiness of different-shape can be different, such as grain Footpath is less, the ball shaped nano of narrow particle size distribution sulfuration nikel powder has good anti-microbial property and electric conductivity.
Due to the high bioactivity of nano nickel sulphide, when applying it in organizational project, wound surface or target are discharged into Organ, it preferentially can be captured by the associated protein in wound exudate or tissue, chloride ion and group, cause nano nickel sulphide granule In some position high concentration abnormal aggregations, although can effectively participate in antibacterial, but these superfluous nano nickel sulphides will be thin in epidermis Born of the same parents, macrophage, the interior aggregation of fibroblast, cause the apoptosis of cell, ultimately result in disunion or the delayed union of wound surface. Generally speaking, immoderate use or uncontrolled release nano nickel sulphide will certainly run counter to desire, and wound repair is not had Benefit.Therefore, safely and effectively rational slow-releasing system is needed using nano nickel sulphide, provide permanently effective medicine for wound surface Thing 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 system of the collagen-hydroxyapatite support containing nano nickel sulphide Preparation Method, is to prepare nano nickel sulphide by Liquid reduction reaction process, is then mixed homogeneously with collagen-hydroxyapatite solution latter Footwork lyophilizing is simultaneously crosslinked preparation and becomes Metal pylon, prepares the novel nano nickel sulfide biomaterial with antibacterial, safety.
The present invention is achieved by the following technical solutions：
(1) nickel acetate and thiourea are adopted and is added glycerol and Liquid reduction reaction process is carried out for dispersant prepare nano nickel sulphide Colloidal sol；Reaction temperature is 30 DEG C -45 DEG C；
(2) it is by the microwave heating reaction in confined conditions of nano nickel sulphide colloidal sol, first anti-under 250～350W microwave powers 2～2.5min is answered, then 2.5～3min is reacted under 100～150W microwave powers, nano nickel sulphide 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 solution to nano nickel sulphide as aimed concn with 10ppm, be subsequently adding total matter The glutaraldehyde of the 0.5% of amount is simultaneously mixed, and obtains the solution of collagen-hydroxyapatite containing nano nickel sulphide that mass fraction is 0.5%, Nano nickel sulphide, collagen-hydroxyapatite solution are injected into the mould of 4cm × 4cm, is freezed 2 hours at -20 DEG C, is then frozen It is dry to obtain within 24 hours collagen-hydroxyapatite support of the porous containing nano nickel sulphide that thickness is 2mm.The concentration of nano nickel sulphide Scope is 10ug/ml-50ug/ml, and the particle diameter of nano nickel sulphide 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 nickel sulphide using microwave-hydrothermal method, with process is simple, life Cycle is short, energy-conserving and environment-protective are produced, the features such as having a safety feature.
2. the nano nickel sulphide 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 nickel sulphide slow-releasing system for wound surface, provides permanently effective for wound surface Medicament slow release, keeps 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 nickel sulphide is realized by procedure below：
(1) nickel acetate and thiourea are adopted and is added glycerol and Liquid reduction reaction process is carried out for dispersant prepare nano nickel sulphide Colloidal sol；Plus the addition of glycerol is the 3% of tetra chlorauric acid quality；Reaction temperature is 40 DEG C；
(2) nano nickel sulphide colloidal sol stirring 10min is taken, microwave heating treatment (selects the auspicious swan HX- in Beijing under airtight condition 300A computer microwaves ultrasound combinatorial compound instrument is microwave source), 2.25min is reacted under 300W microwave powers first, then it is micro- in 120W 2.75min is reacted under wave power, obtain nano nickel sulphide 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 solution to nano nickel sulphide as aimed concn with 10ppm, be subsequently adding total matter The glutaraldehyde of the 0.5% of amount is simultaneously mixed, and obtains the solution of collagen-hydroxyapatite containing nano nickel sulphide that mass fraction is 0.5%, Nano nickel sulphide, collagen-hydroxyapatite solution are injected into the mould of 4cm × 4cm, is freezed 2 hours at -20 DEG C, is then frozen It is dry to obtain within 24 hours the collagen-hydroxyapatite support containing nano nickel sulphide that thickness is 2mm.The concentration range of nano nickel sulphide For 10ug/ml-50ug/ml, the particle diameter of nano nickel sulphide particle is 10-30nm.
Embodiment 2
A kind of preparation method of the collagen-hydroxyapatite support containing nano nickel sulphide is realized by procedure below：
(1) nickel acetate and thiourea are adopted and is added glycerol and Liquid reduction reaction process is carried out for dispersant prepare nano nickel sulphide Colloidal sol；Plus the addition of glycerol is the 3% of tetra chlorauric acid quality；Reaction temperature is 30 DEG C；
(2) nano nickel sulphide colloidal sol stirring 10min is taken, microwave heating treatment (selects the auspicious swan HX- in Beijing under airtight condition 300A computer microwaves ultrasound combinatorial compound instrument is microwave source), 2.5min is reacted under 250W microwave powers first, then in 150W microwaves 2.5min is reacted under power, obtain nano nickel sulphide 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 solution to nano nickel sulphide as aimed concn with 10ppm, be subsequently adding total matter The glutaraldehyde of the 0.5% of amount is simultaneously mixed, obtain mass fraction be 0.5% it is molten containing nano nickel sulphide, collagen-hydroxyapatite Nano nickel sulphide, collagen-hydroxyapatite solution are injected the mould of 4cm × 4cm by liquid, freezing 2 hours at -20 DEG C, then Lyophilizing obtains collagen-hydroxyapatite support of the porous containing nano nickel sulphide that thickness is 2mm for 24 hours.Nano nickel sulphide it is dense Degree scope is 10ug/ml-50ug/ml, and the particle diameter of nano nickel sulphide 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 nickel sulphide, is characterized in that, step is as follows：
(1) nickel acetate and thiourea are adopted and is added glycerol and is carried out for dispersant Liquid reduction reaction process to prepare nano nickel sulphide molten Glue；Reaction temperature is 30 DEG C -45 DEG C；
(2) by the microwave heating reaction in confined conditions of nano nickel sulphide colloidal sol, first 2 are reacted under 250～350W microwave powers ～2.5min, then 2.5～3min is reacted under 100～150W microwave powers, nano nickel sulphide 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 nano nickel sulphide solution for aimed concn, is subsequently adding the 0.5% of gross mass glutaraldehyde and mixes Even, it is 0.5% containing nano nickel sulphide, collagen-hydroxyapatite solution, by nano nickel sulphide, collagen-hydroxyl to obtain mass fraction Base apatite solution injects the mould of 4cm × 4cm, freezes 2 hours at -20 DEG C, and then lyophilizing obtains thickness for 24 hours for 2mm Porous containing nano nickel sulphide collagen-hydroxyapatite support.
2. the preparation method of a kind of collagen-hydroxyapatite support containing nano nickel sulphide according to claim 1, which is special Levying is：The concentration range of nano nickel sulphide is 10ug/ml-50ug/ml, and the particle diameter of nano nickel sulphide particle is 10-30nm.
CN201610962861.7A 2016-11-04 2016-11-04 A kind of preparation method of the collagen hydroxyapatite support containing nano nickel sulphide Pending CN106552291A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110697803A (en) * 2019-09-05 2020-01-17 东南大学 Preparation method of high-performance nickel sulfide-graphene composite electrode material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110697803A (en) * 2019-09-05 2020-01-17 东南大学 Preparation method of high-performance nickel sulfide-graphene composite electrode material

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