CN108714251A - The method that two-step method prepares the chitosan-based synthetism plate material of high hydroxyapatite content - Google Patents

The method that two-step method prepares the chitosan-based synthetism plate material of high hydroxyapatite content Download PDF

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CN108714251A
CN108714251A CN201810576446.7A CN201810576446A CN108714251A CN 108714251 A CN108714251 A CN 108714251A CN 201810576446 A CN201810576446 A CN 201810576446A CN 108714251 A CN108714251 A CN 108714251A
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chitosan
hydroxyapatite
content
solution
plate material
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王征科
方雯
杨玲
胡巧玲
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Zhejiang University ZJU
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Zhejiang University ZJU
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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
    • 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
    • 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
    • A61L27/58—Materials at least partially resorbable by the body
    • 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
    • A61L2300/412—Tissue-regenerating or healing or proliferative 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
    • A61L2430/00—Materials or treatment for tissue regeneration
    • A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Medicinal Chemistry (AREA)
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  • Oral & Maxillofacial Surgery (AREA)
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  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Composite Materials (AREA)
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Abstract

The method that a kind of two-step method disclosed by the invention prepares the chitosan-based synthetism plate material of high hydroxyapatite content, step include：Anhydrous calcium chloride powder is added in chitosan acid solution, urea is added, stirring forms transparent uniform mixed liquor, standing and defoaming.Mixed solution is injected in single radial cut flat plate mold, gel is prepared using two-step method, is first dipped in NaOH coagulating baths and transfers to Na2HPO4In conversion bath, is dried after demoulding washing, the high chitosan-based synthetism plate material of hydroxyapatite content is made.Present invention uses urea as additive, is achieved the homogeneous phase solution system of high-calcium ionic content, and hydroxyapatite content may be up to 95% in gained composite material, has good biocompatibility, degradability and bone growth inducing.Inorganic content through-thickness distribution gradient, can induce osteocyte migration, promotes osteoacusis and wound healing, have good actual application value as bone renovating material.

Description

The method that two-step method prepares the chitosan-based synthetism plate material of high hydroxyapatite content
Technical field
The present invention relates to a kind of methods that two-step method prepares the chitosan-based synthetism plate material of high hydroxyapatite content.
Background technology
Not with bone defects diseases such as the development of global aging trend and bone wound, congenital abnormality, arthritis Disconnected to occur, Bone Defect Repari problem is always one of the great difficult problem that medical field is faced.The autologous bone being often used in traditional medicine is moved It plants and allogenic bone transplantation technology has that source is narrow and the limitations such as immunological rejection, therefore, to existing bone grafting material Modification is optimized, and it is Orthopedic Clinical urgent problem to develop novel bone renovating material.
Human body bone is mainly collectively formed by organic bone matrix structure and inorganic bone salts frame structure, and hydroxy-apatite Stone is its host inorganic mineralogical composition.Hydroxyapatite has good biocompatibility, bioactivity and bone conduction effect, plants It can combine closely in a short time with the bone tissue of human body after entering human body, thus be widely used as bone alternate material.But pure hydroxyl Base Apatite materials brittleness is big, and toughness is low, and mechanical property is poor, it usually needs is used in combination with other materials.
Chitosan (CS) be used as a kind of amino-containing natural polysaccharide of richness, with good biocompatibility, non-immunogenicity, The advantages that biodegradability, is widely used in biomedical sector, such as chitosan-based hemostatic film, nerve rehabilitating tube, artificial Skin etc..By by chitosan with it is hydroxyapatite hybridized, the bone renovating material of excellent combination property can be made.Based on human body High inorganic content and the basis of reality of organic-inorganic Material cladding in bone, prepare hydroxyapatite/shell of high mineral content Polysaccharide composite material has certain facilitation to the development of bone renovating material, has good reality in clinical orthopaedics field Application prospect.
Invention content
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to which providing a kind of two-step method prepares high hydroxyapatite content The method of chitosan-based synthetism plate material.
The method that a kind of two-step method of the present invention prepares the chitosan-based synthetism plate material of high hydroxyapatite content, including such as Lower step：
1) it is molten to weigh the chitosan that certain mass viscosity average molecular weigh is 10,000-120 ten thousand, deacetylation is 60%-95% Matter, using volume fraction for 2%-20% aqueous acetic acid as solvent, stir to being completely dissolved, be configured to 2wt.%-10wt.% Chitosan solution A；
2) certain mass anhydrous calcium chloride powder is weighed, formation mixture stoste B in chitosan solution A is added it to, The addition of calcium chloride is with hydroxyapatite (HA) mass ratio theoretical value corresponding to chitosan (CS) quality and calcium ion Metering, can make m (CS):M (HA) is 60:40-4:96；A certain amount of urea is added, until mixed solution is via WGT-S type mist degree instrument The light transmittance measured is more than 90%, obtains homogeneous mixed solution C；
3) composite hydrogel is prepared by two-step method, the specific steps are：Solution C is injected in single radial cut flat plate mold, first It immerses in the coagulating bath that c (NaOH) is 2wt.%-10wt.%, until solution gels completion, then transfers them to c (Na2HPO4) bathed for the conversion of 2wt.%-10wt.%, realize conversion of the calcium hydroxide crystals to hydroxyapatite；
4) the chitosan-based plural gel of gained is demoulded, and is washed repeatedly to neutrality with deionized water, drying obtains high hydroxyl The chitosan-based synthetism plate material of base apatite content.
During the mineral content in all kinds of method products therefroms using hydrogel as template-mediated mineralising can only achieve at present Etc. levels, and high mineral content relatively difficult to achieve is horizontal.Present invention uses urea as additive, is achieved high-calcium ionic and contains The homogeneous phase solution system of amount, hydroxyapatite content may be up to 95% in the chitosan-based composite material of gained, and with good Biocompatibility, degradability and bone growth inducing, the distribution of inorganic content through-thickness gradient, inducible osteocyte move It moves, promotes osteoacusis and wound healing, there is good actual application value as bone renovating material.
Specific implementation mode
It is further illustrated the present invention below in conjunction with specific example.
Embodiment 1：
1) 1g chitosans (viscosity average molecular weigh be 10,000, deacetylation 60%) are weighed to be added in 100mL beakers, then are added Enter the aqueous acetic acid that 9mL volume fractions are 2%, the chitosan solution A of 10wt.% is obtained after stirring evenly；
2) certain mass anhydrous calcium chloride powder is weighed, adds it to and forms mixture stoste B in chitosan solution A. Institute's addition is measured with hydroxyapatite (HA) mass ratio theoretical value corresponding to chitosan (CS) quality and calcium ion, m (CS):M (HA) is 4:96.A certain amount of urea is added, until mixed solution is more than via the light transmittance that WGT-S type mist degree instrument measures 90%, obtain homogeneous mixed solution C；
3) composite hydrogel is prepared by two-step method, the specific steps are：Solution C is injected in single radial cut flat plate mold, first It immerses in the coagulating bath that c (NaOH) is 2wt.%, until solution gels completion, then transfers them to c (Na2HPO4) be The conversion of 2wt.% is bathed, and realizes conversion of the calcium hydroxide crystals to hydroxyapatite；
4) the chitosan-based plural gel of gained is demoulded, and is washed repeatedly to neutrality with deionized water, drying obtains high hydroxyl The chitosan-based synthetism plate material of base apatite content.
The high chitosan-based bone plate Materials Inorganic object content of hydroxyapatite content made from this example is 95.8%.
Embodiment 2：
1) 1g chitosans (viscosity average molecular weigh be 200,000, deacetylation 70%) are weighed to be added in 100mL beakers, then are added Enter the aqueous acetic acid that 11.5mL volume fractions are 5%, the chitosan solution A of 8wt.% is obtained after stirring evenly；；
2) certain mass anhydrous calcium chloride powder is weighed, adds it to and forms mixture stoste B in chitosan solution A. Institute's addition is measured with hydroxyapatite (HA) mass ratio theoretical value corresponding to chitosan (CS) quality and calcium ion, m (CS):M (HA) is 15:85.A certain amount of urea is added, until mixed solution is big via the light transmittance that WGT-S type mist degree instrument measures In 90%, homogeneous mixed solution C is obtained；
3) composite hydrogel is prepared by two-step method, the specific steps are：Solution C is injected in single radial cut flat plate mold, first It immerses in the coagulating bath that c (NaOH) is 4wt.%, until solution gels completion, then transfers them to c (Na2HPO4) be The conversion of 4wt.% is bathed, and realizes conversion of the calcium hydroxide crystals to hydroxyapatite；
4) the chitosan-based plural gel of gained is demoulded, and is washed repeatedly to neutrality with deionized water, drying obtains high hydroxyl The chitosan-based synthetism plate material of base apatite content.
The high chitosan-based bone plate Materials Inorganic object content of hydroxyapatite content made from this example is 84.4%.
Embodiment 3：
1) 1g chitosans (viscosity average molecular weigh be 500,000, deacetylation 80%) are weighed to be added in 100mL beakers, then are added Enter the aqueous acetic acid that 19mL volume fractions are 10%, the chitosan solution A of 5wt.% is obtained after stirring evenly；
2) certain mass anhydrous calcium chloride powder is weighed, adds it to and forms mixture stoste B in chitosan solution A. Institute's addition is measured with hydroxyapatite (HA) mass ratio theoretical value corresponding to chitosan (CS) quality and calcium ion, m (CS):M (HA) is 25:75.A certain amount of urea is added, until mixed solution is big via the light transmittance that WGT-S type mist degree instrument measures In 90%, homogeneous mixed solution C is obtained；
3) composite hydrogel is prepared by two-step method, the specific steps are：Solution C is injected in single radial cut flat plate mold, first It immerses in the coagulating bath that c (NaOH) is 5wt.%, until solution gels completion, then transfers them to c (Na2HPO4) be The conversion of 5wt.% is bathed, and realizes conversion of the calcium hydroxide crystals to hydroxyapatite；
4) the chitosan-based plural gel of gained is demoulded, and is washed repeatedly to neutrality with deionized water, drying obtains high hydroxyl The chitosan-based synthetism plate material of base apatite content.
The high chitosan-based bone plate Materials Inorganic object content of hydroxyapatite content made from this example is 73.6%.
Embodiment 4：
1) 1g chitosans (viscosity average molecular weigh be 1,000,000, deacetylation 90%) are weighed to be added in 100mL beakers, then The aqueous acetic acid that 24mL volume fractions are 15% is added, the chitosan solution A of 4wt.% is obtained after stirring evenly；；
2) certain mass anhydrous calcium chloride powder is weighed, adds it to and forms mixture stoste B in chitosan solution A. Institute's addition is measured with hydroxyapatite (HA) mass ratio theoretical value corresponding to chitosan (CS) quality and calcium ion, m (CS):M (HA) is 35:65.A certain amount of urea is added, until mixed solution is big via the light transmittance that WGT-S type mist degree instrument measures In 90%, homogeneous mixed solution C is obtained；
3) composite hydrogel is prepared by two-step method, the specific steps are：Solution C is injected in single radial cut flat plate mold, first It immerses in the coagulating bath that c (NaOH) is 8wt.%, until solution gels completion, then transfers them to c (Na2HPO4) be The conversion of 8wt.% is bathed, and realizes conversion of the calcium hydroxide crystals to hydroxyapatite；
4) the chitosan-based plural gel of gained is demoulded, and is washed repeatedly to neutrality with deionized water, drying obtains high hydroxyl The chitosan-based synthetism plate material of base apatite content.
The high chitosan-based bone plate Materials Inorganic object content of hydroxyapatite content made from this example is 64.5%.
Embodiment 5：
1) 1g chitosans (viscosity average molecular weigh be 1,200,000, deacetylation 95%) are weighed to be added in 100mL beakers, then The aqueous acetic acid that 49mL volume fractions are 20% is added, the chitosan solution A of 2wt.% is obtained after stirring evenly；；
2) certain mass anhydrous calcium chloride powder is weighed, adds it to and forms mixture stoste B in chitosan solution A. Institute's addition is measured with hydroxyapatite (HA) mass ratio theoretical value corresponding to chitosan (CS) quality and calcium ion, m (CS):M (HA) is 60:40.A certain amount of urea is added, until mixed solution is big via the light transmittance that WGT-S type mist degree instrument measures In 90%, homogeneous mixed solution C is obtained；
3) composite hydrogel is prepared by two-step method, the specific steps are：Solution C is injected in single radial cut flat plate mold, first It immerses in the coagulating bath that c (NaOH) is 10wt.%, until solution gels completion, then transfers them to c (Na2HPO4) be The conversion of 10wt.% is bathed, and realizes conversion of the calcium hydroxide crystals to hydroxyapatite；
4) the chitosan-based plural gel of gained is demoulded, and is washed repeatedly to neutrality with deionized water, drying obtains high hydroxyl The chitosan-based synthetism plate material of base apatite content.
The high chitosan-based bone plate Materials Inorganic object content of hydroxyapatite content made from this example is 38.6%.
Embodiment 6：
1) 1g chitosans (viscosity average molecular weigh be 10,000, deacetylation 60%) are weighed to be added in 100mL beakers, then are added Enter the aqueous acetic acid that 9mL volume fractions are 2%, the chitosan solution A of 10wt.% is obtained after stirring evenly；
2) certain mass anhydrous calcium chloride powder is weighed, adds it to and forms mixture stoste B in chitosan solution A. Institute's addition is measured with hydroxyapatite (HA) mass ratio theoretical value corresponding to chitosan (CS) quality and calcium ion, m (CS):M (HA) is 4:96.There is precipitation to generate in mixed solution B, muddy gel state is presented, is stirred being added without urea mixing In the case of mixing, follow-up precipitating in situ is cannot achieve, fails the operations such as subsequently to be solidified, convert, dry.If can be seen that not Add urea to adjust, will be unable to that the high chitosan-based synthetism plate material of hydroxyapatite content is made.

Claims (2)

1. a kind of method that two-step method prepares the chitosan-based synthetism plate material of high hydroxyapatite content, which is characterized in that including Following steps：
1) it is solute to weigh the chitosan that certain mass viscosity average molecular weigh is 10,000-120 ten thousand, deacetylation is 60%-95%, with The aqueous acetic acid that volume fraction is 2%-20% is solvent, stirs to being completely dissolved, is configured to the shell of 2wt.%-10wt.% Glycan solution A；
2) certain mass anhydrous calcium chloride powder is weighed, formation mixture stoste B, chlorination in chitosan solution A are added it to The addition of calcium is measured with hydroxyapatite (HA) mass ratio theoretical value corresponding to chitosan (CS) quality and calcium ion, It can make m (CS):M (HA) is 60:40-4:96；A certain amount of urea is added, until mixed solution is measured via WGT-S type mist degree instrument Light transmittance be more than 90%, obtain homogeneous mixed solution C；
3) composite hydrogel is prepared by two-step method, the specific steps are：Solution C is injected in single radial cut flat plate mold, c is submerged initially in (NaOH) in the coagulating bath for being 2wt.%-10wt.%, until solution gels completion, then c (Na are transferred them to2HPO4) be The conversion of 2wt.%-10wt.% is bathed, and realizes conversion of the calcium hydroxide crystals to hydroxyapatite；
4) the chitosan-based plural gel of gained is demoulded, and is washed repeatedly to neutrality with deionized water, drying obtains high hydroxyl phosphorus The chitosan-based synthetism plate material of lime stone content.
2. the method that two-step method according to claim 1 prepares the chitosan-based synthetism plate material of high hydroxyapatite content, It is characterized in that：The mass fraction of hydroxyapatite is up in the chitosan-based synthetism plate material of high hydroxyapatite content 40%-95%.
CN201810576446.7A 2018-06-06 2018-06-06 The method that two-step method prepares the chitosan-based synthetism plate material of high hydroxyapatite content Pending CN108714251A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113332498A (en) * 2021-05-20 2021-09-03 湖北赛罗生物材料有限公司 Silk fibroin/hydroxyapatite composite material and preparation method and application thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1389503A (en) * 2002-07-15 2003-01-08 浙江大学 In-situ compounding process of synthesizing nano composite chitosan/hydroxyapatite material

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1389503A (en) * 2002-07-15 2003-01-08 浙江大学 In-situ compounding process of synthesizing nano composite chitosan/hydroxyapatite material

Non-Patent Citations (1)

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Title
陈中科: "壳聚糖基质中碳酸钙结晶生长的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113332498A (en) * 2021-05-20 2021-09-03 湖北赛罗生物材料有限公司 Silk fibroin/hydroxyapatite composite material and preparation method and application thereof
CN113332498B (en) * 2021-05-20 2022-05-13 湖北赛罗生物材料有限公司 Silk fibroin/hydroxyapatite composite material and preparation method and application thereof

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