CN1329087C - Medical beta phase tricalcium phosphate/collagen cmposite material and its preparing method - Google Patents
Medical beta phase tricalcium phosphate/collagen cmposite material and its preparing method Download PDFInfo
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- CN1329087C CN1329087C CNB2005100490177A CN200510049017A CN1329087C CN 1329087 C CN1329087 C CN 1329087C CN B2005100490177 A CNB2005100490177 A CN B2005100490177A CN 200510049017 A CN200510049017 A CN 200510049017A CN 1329087 C CN1329087 C CN 1329087C
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Abstract
The present invention discloses medical beta phase tricalcium phosphate/collagen composite material and a preparing method thereof. The composite material is composed of the ingredients of the mass percentage: 50% to 67% of nanometer beta phase tricalcium phosphate and 50% to 33% of collagen. Beta phase tricalcium phosphate powder is deposited on collagen matrices through the original position complexation of the collagen and the beta phase tricalcium phosphate, and the mechanical strength of the composite material is enhanced under the action of glutaraldehyde. The beta phase tricalcium phosphate/collagen composite material prepared by the method of the present invention has the characteristics of uniform ingredients, tight combination, favorable biocompatibility, proper pore size, etc. and is suitable for being used as bone repairing material in medical treatment.
Description
Technical field
The present invention relates to a kind of medical β phase tricalcium phosphate/collagen composite materials and preparation method thereof, belong to the bio-medical technical field.
Background technology
Thunder bolt or disease make sclerous tissues such as people's skeleton, tooth produce damage or disappearance, thereby have formed the great market of medical repair materials.Usually, autotransplantation and homogeneous allogenic bone transplantation are used as the damaged scheme of treatment bone.But the source from the body bone is limited, can not be used for large-scale treatment; Though there is immunoreation in the allograph bone wide material sources, even viral communication may take place.Bone renovating material research has at present covered a plurality of fields that comprise metal, pottery, macromolecule and composite thereof, but these materials respectively have deficiency: what have retains for a long time in vivo, be easy to generate biological repelling effect, in time the increase in vivo that has, mechanical properties decrease is too fast, can not satisfy the requirement of bone renovating material.
Along with going deep into of research, people recognize that biodegradable bone renovating material is the trend of Future Development.Can be absorbed by the body fluid environment step by step after this material implants along with the prolongation of time, become the organic component of tissue alive, the risk of having avoided second operation to take out, and also the composition in the material can promote the generation organized.
Summary of the invention
The purpose of this invention is to provide a kind of β phase tricalcium phosphate finely dispersed degradable biological medical calcium phosphate/collagen composite materials and preparation method thereof in the collagen matrix.
Medical β phase tricalcium phosphate/collagen composite materials of the present invention is made up of nano beta phase tricalcium phosphate and collagen, and wherein the mass percentage content of β phase tricalcium phosphate is 50%～67%, and the mass percentage content of collagen is 50%～33%.
The preparation method of medical β phase tricalcium phosphate/collagen composite materials comprises the following steps:
1) be 1 * 10 with concentration
-4～10 * 10
-3The collagenolysis of g/ml stirs in pH value is 2～3 acid solution simultaneously, until forming milky white solution;
2) stirring evenly joins β phase tricalcium phosphate powder in the collagen solution down, and the β phase tricalcium phosphate of adding is 1: 1～2: 1 with the ratio of the quality of collagen;
3) stir that dropwise to add mass concentration down be 1% glutaraldehyde, the glutaraldehyde of adding is 1: 10 with the ratio of the quality of collagen;
4) continue stirring white cotton-shaped suspended material to occur in solution, stop to stir and leaving standstill, treat that flocculent substance all after the deposition, continues agitating solution, and dropwise drips aqueous slkali, is to stop to drip in 6～7 o'clock until pH value;
5) with solution left standstill, remove supernatant after, put into mould, freezing then, dry, put into ethanol and soak repeatedly, lyophilization once more, sterilization gets final product.
Among the present invention, the particle size of said β phase tricalcium phosphate is 200nm-500nm.The acid that is used to dissolve collagen can be hydrochloric acid or acetic acid.The aqueous slkali that drips can be NaOH, NH40H or KOH.Step 5) is put into ethanol and is soaked repeatedly, and general 3～6 times, each 12～24h.
In order to reduce the cryodesiccated time of material, usually to adopt mould that the surface has a micropore for well.
The present invention has prepared medical β phase tricalcium phosphate/collagen composite materials in the mode of original position complexation, this material relies on the intermolecular group complexation to form by nanometer β phase tricalcium phosphate and tropocollagen molecule, on the collagen matrix, deposit β phase tricalcium phosphate powder, and under the effect of glutaraldehyde, increase the mechanical strength of composite.On micro-scale, have the characteristics that are evenly distributed.Under the freeze drying process condition, can prepare the bone renovating material of aperture size by this good biocompatibility, the β phase tricalcium phosphate/collagen composite materials of degrading completely, can be used as bio-medical material and aspect medical, be used widely in 10 μ m～150 μ m, hole internal communication.
The bone renovating material that adopts method of the present invention to prepare have uniform component distribution, β phase tricalcium phosphate and collagen in conjunction with closely, characteristics such as biocompatibility is good, finally degraded fully in vivo, do not have residuals to exist, can be used as embedded material and be applied in bio-medical fields such as bone tissue engineer.
Description of drawings
Fig. 1 is the stereoscan photograph of medical β phase tricalcium phosphate/collagen composite materials of making of embodiment 2.
The specific embodiment
Used collagen is the type i collagen that sigma company extracts from cattle root tendon in the following example.
Embodiment 1
1g collagen is dissolved in the hydrochloric acid solution of 300ml 0.01M, stir simultaneously, treat evenly to join 1.5g β phase tricalcium phosphate powder in the collagen solution after milky white solution forms, the glutaraldehyde solution that adds 10ml 1% then, continue to stir up to the cotton-shaped suspended material of white and occur, treat that it deposits back adding NaOH solution to pH value fully is 6, remove supernatant after leaving standstill 24h, the gained material is put into the surface has the mould of plastics of micropore to cool off 10min at liquid nitrogen, put into the dry 72h of freezer dryer then, put into ethanol after material takes out and soak 24h * 3 time, put into the dry 48h of freezer dryer once more, take out the back 2h that in oxirane steam, sterilizes.
Embodiment 2
0.4g collagen is dissolved in the acetic acid solution of 100ml 0.5M, stir simultaneously, treat evenly to join 0.8g β phase tricalcium phosphate powder in the collagen solution behind the milky white solution, the glutaraldehyde solution that adds 8ml 0.5% then, continuous stirring occurs up to the cotton-shaped suspended material of white, treats that it deposits the back fully and adds NH
4OH solution to pH value is 7, remove supernatant after leaving standstill 36h, the gained material is put into the surface has the mould of plastics of micropore to cool off 30min at liquid nitrogen, put into the dry 72h of freezer dryer then, put into ethanol after material takes out and soak 24h * 3 time, put into the dry 48h of freezer dryer once more, 3h sterilizes in oxirane steam after taking out.This example products therefrom is through sem test, and the material internal pattern is shown in legend 1, and from scheming as seen, the hole of the medical β phase tricalcium phosphate/collagen composite materials inside that makes is connected.
Embodiment 3
0.5g β phase tricalcium phosphate powder is evenly joined in the 400ml collagen solution, collagen solution concentration is 0.5mg/ml, the glutaraldehyde solution that adds 25ml 0.2% then, continue to stir up to the cotton-shaped suspended material of white and occur, treat that it deposits back adding KOH solution to pH value fully is 7, remove supernatant after leaving standstill 48h, the gained material is put into the surface has the mould of plastics of micropore to cool off 60min at liquid nitrogen, put into the dry 96h of freezer dryer then, put into ethanol after material takes out and soak 24h * 3 time, put into the dry 60h of freezer dryer once more, 1h sterilizes in oxirane steam after taking out.
Claims (1)
1. the preparation method of medical β phase tricalcium phosphate/collagen composite materials is characterized in that comprising the following steps:
1) be 1 * 10 with concentration
-4～10 * 10
-3The collagenolysis of g/ml stirs in pH value is 2～3 acid solution simultaneously, until forming milky white solution;
2) stirring is down that the β phase tricalcium phosphate powder of 200nm-500nm evenly joins in the collagen solution with particle size, and the β phase tricalcium phosphate of adding is 1: 1～2: 1 with the ratio of the quality of collagen;
3) stir that dropwise to add mass concentration down be 1% glutaraldehyde, the glutaraldehyde of adding is 1: 10 with the ratio of the quality of collagen;
4) continue stirring white cotton-shaped suspended material to occur in solution, stop to stir and leaving standstill, treat that flocculent substance all after the deposition, continues agitating solution, and dropwise drips aqueous slkali, is to stop to drip in 6～7 o'clock until pH value;
5) with solution left standstill, remove supernatant after, put into mould, freezing then, dry, put into ethanol and soak repeatedly, lyophilization once more, sterilization gets final product.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100490177A CN1329087C (en) | 2005-02-01 | 2005-02-01 | Medical beta phase tricalcium phosphate/collagen cmposite material and its preparing method |
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| CNB2005100490177A CN1329087C (en) | 2005-02-01 | 2005-02-01 | Medical beta phase tricalcium phosphate/collagen cmposite material and its preparing method |
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| CN1647826A CN1647826A (en) | 2005-08-03 |
| CN1329087C true CN1329087C (en) | 2007-08-01 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101822852B (en) * | 2009-03-03 | 2013-04-10 | 北京化工大学 | Biomimetic calcium phosphate fiber composite bracket material and preparation method thereof |
| CN103055352B (en) * | 2013-01-22 | 2014-12-10 | 四川大学 | Calcium phosphate/collagen composite biologic ceramic material and preparation method thereof |
| CN107185040B (en) * | 2017-05-24 | 2020-07-14 | 成都大学 | Preparation method, application and use of nano tricalcium phosphate-hydrogel-I type collagen biological material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1338315A (en) * | 2001-10-12 | 2002-03-06 | 清华大学 | Process for preparing nm-crysal collagen-based calcium phosphate composition used for repairing bone |
| CN1654543A (en) * | 2005-01-27 | 2005-08-17 | 浙江大学 | Biodegradable calcium phosphate/collagen composite materials for medical use and method for preparation thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1338315A (en) * | 2001-10-12 | 2002-03-06 | 清华大学 | Process for preparing nm-crysal collagen-based calcium phosphate composition used for repairing bone |
| CN1654543A (en) * | 2005-01-27 | 2005-08-17 | 浙江大学 | Biodegradable calcium phosphate/collagen composite materials for medical use and method for preparation thereof |
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