CN1562894A - Method for forming osteolith class layer on surface of calcium phosphate ceramics - Google Patents
Method for forming osteolith class layer on surface of calcium phosphate ceramics Download PDFInfo
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- CN1562894A CN1562894A CN 200410033613 CN200410033613A CN1562894A CN 1562894 A CN1562894 A CN 1562894A CN 200410033613 CN200410033613 CN 200410033613 CN 200410033613 A CN200410033613 A CN 200410033613A CN 1562894 A CN1562894 A CN 1562894A
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- calcium phosphate
- phosphate ceramic
- body fluid
- simulated body
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Abstract
In the invention, calcium phosphate ceramics is soaked by 1-12 mole sodium hydroxide solution, then is soaked and processed by iimitate body fluid with different density to form bone-like kietyoite layer on the surface of calcium phosphate ceramics.
Description
Technical field
The invention belongs to calcium phosphate ceramic surface-active-treatment technical field, particularly a kind of method that makes the calcium phosphate ceramic surface form bone like apatite layer.
Background technology
The inorganic components of the chemical constitution of calcium phosphate ceramic and human body bone is close, has excellent biological compatibility, is the very important bone impairment renovation material of a class.The preparation method of calcium phosphate ceramic mainly contains synthetic method, coral conversion method and nature bone calcination method etc., all to handle in the method for preparing process through the high temperature sintering about 1000 ℃, thereby the biological activity of calcium phosphate ceramic is reduced, implant as medical material, influenced cell and adhesion, propagation and the growth organized thereon.Activity is carried out on the calcium phosphate biological ceramic surface handle, make its surface form the bone like apatite layer close with inorganic components with the human body bone structure, the application in clinical medicine has important practical value for calcium phosphate ceramic.At present, at " biomedical engineering magazine " 2002 the 19th volumes the 2nd phase 186-190 page or leaf, Duan Yourong etc. have delivered exercise question and have been " the influence research that fine and close CaP ceramic surface pattern forms bone like apatite layer in dynamic simulation body fluid ", in this article, reported calcium phosphate ceramic has been soaked, formed the method for bone like apatite layer on the calcium phosphate ceramic surface with flow simulating body fluid.The device that this method is used is comparatively complicated, technology cost height; The speed that forms osteoid apatite on the calcium phosphate ceramic surface is slow, and quantity is few, and osteoid apatite is inhomogeneous in the calcium phosphate ceramic surface arrangement, has influenced the practical application of calcium phosphate ceramic in clinical medicine.
Summary of the invention
The objective of the invention is in order to overcome the deficiency that above-mentioned calcium phosphate ceramic surface forms the osteoid apatite layer method, provide a kind of calcium phosphate ceramic to form the method for osteoid apatite, before employing is soaked with simulated body fluid calcium phosphate ceramic, earlier with 1～12 mole of different concns aqueous sodium hydroxide solution to the calcium phosphate ceramic surface preparation, and then, make the calcium phosphate ceramic surface form bone like apatite layer through the simulated body fluid immersion treatment.
Technology of the present invention may further comprise the steps:
(1) calcium phosphate ceramic is cleaned up in deionized water or distilled water, in 80～100 ℃ of oven dry;
(2) with analytical pure sodium hydroxide reagent and the deionized water or distilled water preparation 1～12 molar sodium hydroxide aqueous solution;
(3) in 1000 ml deionized water or distilled water, add sodium-chlor (NaCl) 8.00～24.00 grams, sodium bicarbonate (NaHCO
3) 0.35～1.01 gram, Repone K (KCl) 0.23～0.69 gram, dipotassium hydrogen phosphate (K
2HPO
43H
2O) 0.23～0.69 gram, magnesium chloride (MgCl
26H
2O) 0.31～0.93 gram, calcium chloride (CaCl
22H
2O) 0.28g～0.84 gram, sodium sulfate (Na
2SO
4) 0.07～0.21 gram, Tutofusin tris ((CH
2OH)
2CNH
2) 6.06～18.18 grams, prepare simulated body fluid, and the pH value of simulated body fluid is transferred to 7.2～7.4 with 1 mole hydrochloride solution;
(4) the cleaned calcium phosphate ceramic of step (1) is placed Glass Containers, add 1～12 molar sodium hydroxide aqueous solution of step (2) preparation, and calcium phosphate ceramic is fully immersed in the aqueous sodium hydroxide solution, normal temperature was placed 2～6 days down;
(5) with the calcium phosphate ceramic after step (4) immersion treatment, clean repeatedly, after the pH value of scavenging solution is 6.5～7.5, in 80～100 ℃ of oven dry with deionized water or distilled water;
(6) calcium phosphate ceramic after step (5) cleaning, the oven dry is placed Glass Containers, the simulated body fluid that adds step (3) preparation, and calcium phosphate ceramic is fully immersed in the simulated body fluid, 36～38 ℃ of temperature, under the condition of humidity 60～90%, immersion treatment 2～20 days, during every 24～48 hours, remove old liquid, change the fresh simulated body fluid of same concentrations;
(7) calcium phosphate ceramic after step (6) processing is taken out, clean up with deionized water or distilled water, in 80～100 ℃ of oven dry.
Characteristics of the present invention:
Treatment process is simple, and cost is low.
Adopt aqueous sodium hydroxide solution that calcium phosphate ceramic is soaked pre-treatment, and then use the simulated body fluid immersion treatment, because the calcium phosphate ceramic surface has great amount of hydroxy group, make calcium ion, phosphate anions etc. are adsorbed on the calcium phosphate ceramic surface easily, thereby make osteoid apatite fast in its surperficial sedimentation velocity, quantity is many, be evenly distributed, the surfactivity height of calcium phosphate ceramic implants this calcium phosphate ceramic, is convenient to osteocyte and new organization in the calcium phosphate ceramic surface adhesion, propagation and growth, also help calcium phosphate ceramic implant back and the combining of body osseous tissue, the growth of promotion new bone tissue and from the reconstruction of body bone.
Calcium phosphate ceramic after the present invention handles is mainly used in damaged reparation of bone and bone tissue engineering stent material, also can use as the tooth dental repair material.
Embodiment
Embodiment 1
(1) porous calcium phosphate ceramic with the preparation of synthetic method cleans up in deionized water or distilled water, in 80 ℃ of oven dry;
(2) prepare the 12 molar sodium hydroxide aqueous solution with analytical pure sodium hydroxide reagent and deionized water or distilled water;
(3) in 1000 ml deionized water or distilled water, add sodium-chlor (NaCl) 24.00 grams, sodium bicarbonate (NaHCO
3) 1.01 grams, Repone K (KCl) 0.69 gram, dipotassium hydrogen phosphate (K
2HPO
43H
2O) 0.69 gram, magnesium chloride (MgCl
26H
2O) 0.93 gram, calcium chloride (CaCl
22H
2O) 0.84 gram, sodium sulfate (Na
2SO
4) 0.21 gram, Tutofusin tris ((CH
2OH)
3CNH
2) 18.18 grams, prepare simulated body fluid, and the pH value of simulated body fluid is transferred to 7.2～7.4, the preparation simulated body fluid with 1 mole hydrochloride solution;
(4) the cleaned calcium phosphate ceramic of step (1) is placed Glass Containers, add the 12 molar sodium hydroxide aqueous solution of step (2) preparation, and calcium phosphate ceramic is fully immersed in the aqueous sodium hydroxide solution, normal temperature was placed 6 days down;
(5) with the calcium phosphate ceramic after step (4) immersion treatment, clean repeatedly, after the pH value of scavenging solution is 6.5～7.5, in 80 ℃ of oven dry with deionized water or distilled water;
(6) calcium phosphate ceramic after step (5) cleaning, the oven dry is placed Glass Containers, the simulated body fluid that adds step (3) preparation, and calcium phosphate ceramic is fully immersed in the simulated body fluid, be placed on 36～37 ℃ of temperature, in the thermostat container of humidity 60～70%, immersion treatment 18 days, during every 48 hours, remove old liquid, change the fresh simulated body fluid of same concentrations;
(7) set by step after handle (6), calcium phosphate ceramic is taken out, clean up,,, show on the calcium phosphate ceramic surface to have formed bone like apatite layer by scanning electron microscopic observation and Infrared spectroscopy in 80 ℃ of oven dry with deionized water or distilled water.
Embodiment 2
(1) porous calcium phosphate ceramic with the preparation of coral conversion method cleans up in deionized water or distilled water, in 90 ℃ of oven dry;
(2) prepare the 8 molar sodium hydroxide aqueous solution with analytical pure sodium hydroxide reagent and deionized water or distilled water;
(3) in 1000 ml deionized water or distilled water, add sodium-chlor (NaCl) 12.00 grams, sodium bicarbonate (NaHCO
3) 0.525 gram, Repone K (KCl) 0.345 gram, dipotassium hydrogen phosphate (K
2HPO
43H
2O) 0.345 gram, magnesium chloride (MgCl
26H
2O) 0.465 gram, calcium chloride (CaCl
22H
2O) 0.42 gram, sodium sulfate (Na
2SO
4) 0.105 gram, Tutofusin tris ((CH
2OH)
3CNH
2) 9.09 grams, prepare simulated body fluid, and the pH value of simulated body fluid is transferred to 7.2～7.4 with 1 mole hydrochloride solution; The preparation simulated body fluid;
(4) the cleaned calcium phosphate ceramic of step (1) is placed Glass Containers, add the 8 molar sodium hydroxide aqueous solution of step (2) preparation, and calcium phosphate ceramic is fully immersed in the aqueous sodium hydroxide solution, normal temperature was placed 4 days down;
(5) with the calcium phosphate ceramic after step (4) immersion treatment, clean repeatedly, after the pH value of scavenging solution is 6.5～7.5, in 90 ℃ of oven dry with deionized water or distilled water;
(6) with the calcium phosphate ceramic after step (5) cleaning, the oven dry, place Glass Containers, the simulated body fluid that adds step (3) preparation, and calcium phosphate ceramic is fully immersed in the simulated body fluid, be placed on 36～37 ℃ of temperature, in the thermostat container of humidity 70～80%, immersion treatment 10 days, every 36 hours, remove old liquid during this time, change the fresh simulated body fluid of same concentrations;
(7) set by step after handle (6), calcium phosphate ceramic is taken out, clean up,,, show on the calcium phosphate ceramic surface to have formed bone like apatite layer by scanning electron microscopic observation and Infrared spectroscopy in 90 ℃ of oven dry with deionized water or distilled water.
Embodiment 3
(1) porous calcium phosphate ceramic with the preparation of nature bone calcination method cleans up in deionized water or distilled water, in 100 ℃ of oven dry;
(2) prepare the 1 molar sodium hydroxide aqueous solution with analytical pure sodium hydroxide reagent and deionized water or distilled water;
(3) in 1000 ml deionized water or distilled water, add sodium-chlor (NaCl) 8.00 grams, sodium bicarbonate (NaHCO
3) 0.35 gram, Repone K (KCl) 0.23 gram, dipotassium hydrogen phosphate (K
2HPO
43H
2O) 0.23 gram, magnesium chloride (MgCl
26H
2O) 0.31 gram, calcium chloride (CaCl
22H
2O) 0.28g gram, sodium sulfate (Na
2SO
4) 0.07 gram, Tutofusin tris ((CH
2OH)
3CNH
2) 6.06 grams, prepare simulated body fluid, and the pH value of simulated body fluid is transferred to 7.2～7.4, the preparation simulated body fluid with 1 mole hydrochloride solution;
(4) the cleaned calcium phosphate ceramic of step (1) is placed Glass Containers, add the 1 molar sodium hydroxide aqueous solution of step (2) preparation, and calcium phosphate ceramic is fully immersed in the aqueous sodium hydroxide solution, normal temperature was placed 2 days down;
(5) with the calcium phosphate ceramic after step (4) immersion treatment, clean repeatedly, after the pH value of scavenging solution is 6.5～7.5, in 100 ℃ of oven dry with deionized water or distilled water;
(6) the calcium phosphate ceramic material after step (5) cleaning, the oven dry is placed Glass Containers, the simulated body fluid that adds step (3) preparation, and calcium phosphate ceramic is fully immersed in the simulated body fluid, be placed on 36～37 ℃ of temperature, in the thermostat container of humidity 80～90%, immersion treatment 3 days, during every 24 hours, remove old liquid, change the fresh simulated body fluid of same concentrations;
(7) set by step after handle (6), calcium phosphate ceramic is taken out, clean up,,, show on the calcium phosphate ceramic surface to have formed bone like apatite layer by scanning electron microscopic observation and Infrared spectroscopy in 100 ℃ of oven dry with deionized water or distilled water.
Scleroblast is inoculated in the calcium phosphate ceramic of resulting surface generation bone like apatite layer among above-mentioned three embodiment, vitro culture 7 days, competence for added value with the mtt assay test cell, vitro culture 14 days, measure alkaline phosphatase activities (ALP), the result is as shown in table 1, this shows, the competence for added value of cell and alkaline phosphatase activities all than under the similarity condition without the present invention handle to calcium phosphate ceramic height in the same old way.
The MTT absorbance of the compound cultivation of table 1 calcium phosphate ceramic/scleroblast and ALP value
| Embodiment 1 | Embodiment 2 | Embodiment 3 | To in the same old way | |
| Mtt assay records absorbance | 1.245 | ??0.823 | ??2.014 | ??0.508 |
| Alkaline phosphatase (ALP) (U/L) | 16.451 | ??15.523 | ??18.264 | ??10.825 |
Claims (1)
1. calcium phosphate ceramic surface forms the method for bone like apatite layer, calcium phosphate ceramic is soaked with simulated body fluid, before it is characterized in that calcium phosphate ceramic soaks with simulated body fluid, earlier calcium phosphate ceramic is carried out surface preparation with the aqueous sodium hydroxide solution of 1～12 mole of different concns, soak through simulated body fluid, technology may further comprise the steps again:
(1) calcium phosphate ceramic is cleaned up in deionized water or distilled water, in 80～100 ℃ of oven dry;
(2) with analytical pure sodium hydroxide reagent and the deionized water or distilled water preparation 1～12 molar sodium hydroxide aqueous solution;
(3) in 1000 ml deionized water or distilled water, add sodium-chlor (NaCl) 8.00～24.00 grams, sodium bicarbonate (NaHCO
3) 0.35～1.01 gram, Repone K (KCl) 0.23～0.69 gram, dipotassium hydrogen phosphate (K
2HPO
43H
2O) 0.23～0.69 gram, magnesium chloride (MgCl
26H
2O) 0.31～0.93 gram, calcium chloride (CaCl
22H
2O) 0.28g～0.84 gram, sodium sulfate (Na
2SO
4) 0.07～0.21 gram, Tutofusin tris ((CH
2OH)
3CNH
2) 6.06～18.18 grams, prepare simulated body fluid, and the pH value of simulated body fluid is transferred to 7.2～7.4 with 1 mole hydrochloride solution;
(4) the cleaned calcium phosphate ceramic of step (1) is placed Glass Containers, add 1～12 molar sodium hydroxide aqueous solution of step (2) preparation, and calcium phosphate ceramic is fully immersed in the aqueous sodium hydroxide solution, normal temperature was placed 2～6 days down;
(5) with the calcium phosphate ceramic after step (4) immersion treatment, clean repeatedly, after the pH value of scavenging solution is 6.5～7.5, in 80～100 ℃ of oven dry with deionized water or distilled water;
(6) calcium phosphate ceramic after step (5) cleaning, the oven dry is placed Glass Containers, the simulated body fluid that adds step (3) preparation, and calcium phosphate ceramic is fully immersed in the simulated body fluid, 36～38 ℃ of temperature, under the condition of humidity 60～90%, immersion treatment 2～20 days, during every 24～48 hours, remove old liquid, change the fresh simulated body fluid of same concentrations;
(7) calcium phosphate ceramic after step (6) processing is taken out, clean up with deionized water or distillation, in 80～100 ℃ of oven dry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410033613 CN1241879C (en) | 2004-04-13 | 2004-04-13 | Method for forming osteolith class layer on surface of calcium phosphate ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410033613 CN1241879C (en) | 2004-04-13 | 2004-04-13 | Method for forming osteolith class layer on surface of calcium phosphate ceramics |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1562894A true CN1562894A (en) | 2005-01-12 |
| CN1241879C CN1241879C (en) | 2006-02-15 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410033613 Expired - Fee Related CN1241879C (en) | 2004-04-13 | 2004-04-13 | Method for forming osteolith class layer on surface of calcium phosphate ceramics |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102497891A (en) * | 2009-06-23 | 2012-06-13 | 盖斯特里希医药公司 | Bone substitute material |
| CN103341206A (en) * | 2013-06-09 | 2013-10-09 | 四川大学 | Calcium phosphate/collagen/bone-like apatite three-level bionic bone tissue engineering scaffold and preparation method thereof |
| CN107050508A (en) * | 2017-01-19 | 2017-08-18 | 深圳清华大学研究院 | Injectable bone repair material and preparation method thereof |
| CN107141022A (en) * | 2017-04-14 | 2017-09-08 | 华南理工大学 | A kind of whitlockite coating built in calcium phosphate bioceramic matrix surface and preparation method thereof |
| CN107397977A (en) * | 2017-08-03 | 2017-11-28 | 广东工业大学 | Method that 3D printing metal base surface is modified, 3D printing Metal Substrate bioceramic scaffold and preparation method thereof |
-
2004
- 2004-04-13 CN CN 200410033613 patent/CN1241879C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102497891A (en) * | 2009-06-23 | 2012-06-13 | 盖斯特里希医药公司 | Bone substitute material |
| US8734524B2 (en) | 2009-06-23 | 2014-05-27 | Geistlich Pharma Ag | Bone substitute material |
| CN102497891B (en) * | 2009-06-23 | 2015-05-27 | 盖斯特里希医药公司 | Bone substitute material |
| CN103341206A (en) * | 2013-06-09 | 2013-10-09 | 四川大学 | Calcium phosphate/collagen/bone-like apatite three-level bionic bone tissue engineering scaffold and preparation method thereof |
| CN103341206B (en) * | 2013-06-09 | 2014-11-19 | 四川大学 | Calcium phosphate/collagen/bone-like apatite three-level bionic bone tissue engineering scaffold and preparation method thereof |
| CN107050508A (en) * | 2017-01-19 | 2017-08-18 | 深圳清华大学研究院 | Injectable bone repair material and preparation method thereof |
| CN107050508B (en) * | 2017-01-19 | 2020-12-18 | 深圳清华大学研究院 | Injectable bone repair material and preparation method thereof |
| CN107141022A (en) * | 2017-04-14 | 2017-09-08 | 华南理工大学 | A kind of whitlockite coating built in calcium phosphate bioceramic matrix surface and preparation method thereof |
| CN107141022B (en) * | 2017-04-14 | 2020-08-18 | 华南理工大学 | Whitlockite coating constructed on surface of calcium phosphate biological ceramic matrix and preparation method thereof |
| CN107397977A (en) * | 2017-08-03 | 2017-11-28 | 广东工业大学 | Method that 3D printing metal base surface is modified, 3D printing Metal Substrate bioceramic scaffold and preparation method thereof |
| CN107397977B (en) * | 2017-08-03 | 2021-01-26 | 广东工业大学 | 3D printing metal matrix surface modification method, 3D printing metal matrix biological ceramic support and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1241879C (en) | 2006-02-15 |
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