CN102716513B - Method for modifying RGD on Ca-P ceramic material surface - Google Patents
Method for modifying RGD on Ca-P ceramic material surface Download PDFInfo
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- CN102716513B CN102716513B CN201210135454.0A CN201210135454A CN102716513B CN 102716513 B CN102716513 B CN 102716513B CN 201210135454 A CN201210135454 A CN 201210135454A CN 102716513 B CN102716513 B CN 102716513B
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- 238000000034 method Methods 0.000 title claims abstract description 47
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 39
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 99
- 239000000919 ceramic Substances 0.000 claims abstract description 86
- 239000000243 solution Substances 0.000 claims abstract description 41
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 33
- 239000007864 aqueous solution Substances 0.000 claims abstract description 31
- 230000004048 modification Effects 0.000 claims abstract description 20
- 238000012986 modification Methods 0.000 claims abstract description 20
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 230000000694 effects Effects 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 9
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 8
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims description 8
- 230000001476 alcoholic effect Effects 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000001506 calcium phosphate Substances 0.000 claims description 6
- 229910000391 tricalcium phosphate Inorganic materials 0.000 claims description 6
- 229940078499 tricalcium phosphate Drugs 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- 238000009423 ventilation Methods 0.000 claims description 4
- 230000001413 cellular effect Effects 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 6
- 230000002708 enhancing effect Effects 0.000 abstract description 2
- 231100000331 toxic Toxicity 0.000 abstract 1
- 230000002588 toxic effect Effects 0.000 abstract 1
- IYMAXBFPHPZYIK-BQBZGAKWSA-N Arg-Gly-Asp Chemical compound NC(N)=NCCC[C@H](N)C(=O)NCC(=O)N[C@@H](CC(O)=O)C(O)=O IYMAXBFPHPZYIK-BQBZGAKWSA-N 0.000 description 48
- 239000000463 material Substances 0.000 description 18
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 11
- 238000010586 diagram Methods 0.000 description 11
- 238000010521 absorption reaction Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 239000004068 calcium phosphate ceramic Substances 0.000 description 5
- 229960004756 ethanol Drugs 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 238000009413 insulation Methods 0.000 description 4
- 238000010306 acid treatment Methods 0.000 description 3
- 125000003368 amide group Chemical group 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 231100000777 Toxicophore Toxicity 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 210000000988 bone and bone Anatomy 0.000 description 2
- 230000010261 cell growth Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000004375 Dextrin Substances 0.000 description 1
- 229920001353 Dextrin Polymers 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000021164 cell adhesion Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 235000019425 dextrin Nutrition 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
- Materials For Medical Uses (AREA)
Abstract
The invention discloses a method for modifying RGD on a Ca-P ceramic material surface, which comprises the following steps: a) providing a Ca-P ceramic; b) placing the Ca-P ceramic in an oxalic acid aqueous solution for reacting the Ca-P ceramic surface and the oxalic acid aqueous solution, removing the Ca-P ceramic after reacting; c) placing the reacted Ca-P ceramic in a EDC/NHS chloroform solution for reacting, and removing the Ca-P ceramic after reacting; and d) placing the Ca-P ceramic which is reacted with the EDC/NHS chloroform solution in a RGD ethanol aqueous solution for reacting to obtain the Ca-P ceramic capable of enhancing the RGD modification effect. According to the embodiment of the invention, RGD is combined with the Ca-P ceramic material surface by chemical bonds, the combination force can be effectively increased; the method of the invention does not introduce a toxic group on the Ca-P ceramic material surface, thereby the usage in the biological and medical fields can not be influenced; and the method for modifying RGD has characteristics of easy operation and reduced cost.
Description
Technical field
The present invention relates to technical field of ceramic material, more specifically, the present invention relates to a kind of method of modifying RGD at Ca-P ceramic material surface.
Background technology
Ca-P ceramic because of its inorganic composition and bone photo like and there is good biocompatibility and be widely used in Bone Defect Repari field.Because the preparation of ceramic material usually will through the process of high temperature sintering, and the material surface poor activity of sintering, be unfavorable for adhesion and the growth of cell, therefore need to carry out finishing to it.Rgd peptide because of its can by the identification of cell cortex protein receptor-specific, thus promote the process such as adhesion, growth of cell and be widely used in the finishing of biomaterial.The finishing of RGD to Ca-P ceramic material is also widely studied, and current research mainly concentrates on simple physical absorption modification and chemical modification two aspect.Modified by physical absorption, the cell adhesion of material surface can be promoted to a certain extent, but cause because intermolecular force is more weak RGD and material surface adhesion also more weak, RGD can not continuously and effectively be played a role; And RGD receives concern by the method that chemical bond is modified, but mainly realized by silane coupler and other organic molecule couplings at present, this modification introduces the organic molecule of certain toxicity, existing defects in medical.
Summary of the invention
The present invention is intended at least one of solve the problems of the technologies described above.
For this reason, one object of the present invention is to propose a kind of raising Ca-P ceramic surface combination power and adhesive capacity, thus strengthens the method for Ca-P ceramic surface RGD modification effect.
According to the method for modifying RGD at Ca-P ceramic material surface of the embodiment of the present invention, comprise the following steps:
A) Ca-P ceramic is provided;
B) described Ca-P ceramic is placed in oxalic acid aqueous solution to make described Ca-P ceramic surface and the reaction of described oxalic acid aqueous solution, after reaction, takes out Ca-P ceramic;
C) chloroformic solution being placed in EDC/NHS with the reacted Ca-P ceramic of described oxalic acid aqueous solution is reacted, after reaction, take out Ca-P ceramic;
D) ethanol water being placed in RGD with the reacted Ca-P ceramic of the chloroformic solution of described EDC/NHS is reacted, the Ca-P ceramic of the RGD modification effect that is enhanced.
According to the method for modifying RGD at Ca-P ceramic material surface of the embodiment of the present invention, RGD is combined with Ca-P ceramic material surface by chemical bond, and adhesion effectively improves; This method of modifying does not introduce toxophore at Ca-P ceramic material surface, does not affect its use in bio-medical field; And operation is simple for the method for modification RGD of the present invention, can reduce costs.
In addition, method of modifying RGD at Ca-P ceramic material surface according to the above embodiment of the present invention, can also have following additional technical characteristic:
According to one embodiment of present invention, described Ca-P ceramic in the form of sheets, block, cellular or Powdered.
According to one embodiment of present invention, described Ca-P ceramic is hydroxyapatite, bata-tricalcium phosphate or its mixture.
According to one embodiment of present invention, described step b) comprises:
B-1) oxalic acid aqueous solution is prepared;
B-2) Ca-P ceramic is put into described oxalic acid aqueous solution to react;
B-3) take out reacted Ca-P ceramic, dry with deionized water rinsing.
According to one embodiment of present invention, the concentration of described oxalic acid aqueous solution is 10
-5~ 10
-3mol/L.
According to one embodiment of present invention, in step b-2) in, make Ca-P ceramic and described oxalic acid aqueous solution react 0.5 ~ 2h.
According to one embodiment of present invention, described step c) comprises:
The NHS of the EDC and 1 ~ 9 weight portion that c-1) take 1 ~ 9 weight portion is dissolved in chloroform, leaves standstill more than 1 hour to dissolve described EDC and NHS under ventilation condition after stirring;
C-2) be placed in the chloroformic solution of described EDC/NHS by with the reacted Ca-P ceramic of described oxalic acid aqueous solution, continuous stirring is fully reacted to make the chloroformic solution of Ca-P ceramic and described EDC/NHS;
C-3) take out reacted Ca-P ceramic, successively rinse with chloroform and acetone, dry.
According to one embodiment of present invention, in step c-2) middle stirring 6 ~ 36h.
According to one embodiment of present invention, described step d) comprises:
D-1) be dissolved in deionized water by dehydrated alcohol, dose volume mark is the ethanol water of 10 ~ 100%;
D-2) RGD is dissolved in described ethanol water, forms the RGD solution that concentration is 1 ~ 5mg/mL;
D-3) react being placed in described RGD solution with the reacted Ca-P ceramic of the chloroformic solution of described EDC/NHS;
D-4) take out reacted Ca-P ceramic, rinse Ca-P ceramic surface with alcoholic solution, dry the Ca-P ceramic of the RGD modification effect that is enhanced.
According to one embodiment of present invention, in steps d-3) in, described Ca-P ceramic reacts 6 ~ 36h in described RGD solution.
Additional aspect of the present invention and advantage will part provide in the following description, and part will become obvious from the following description, or be recognized by practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or additional aspect of the present invention and advantage will become obvious and easy understand from accompanying drawing below combining to the description of embodiment, wherein:
Fig. 1 is the schematic flow sheet of the method for RGD of modifying at Ca-P ceramic material surface according to the embodiment of the present invention;
Fig. 2 is the Fourier transform infrared spectroscopy schematic diagram of lamellar Ca-P ceramic, wherein Fig. 2 (a) represents the Fourier transform infrared spectroscopy schematic diagram modifying the method modification gained Ca-P ceramic surface of RGD at Ca-P ceramic material surface according to the embodiment of the present invention, and Fig. 2 (b) represents the Fourier transform infrared spectroscopy schematic diagram modifying the Ca-P ceramic surface obtained through simple physical absorption;
Fig. 3 is the Fourier transform infrared spectroscopy schematic diagram of block Ca-P ceramic, and wherein Fig. 3 (a) and Fig. 3 (b) represents the Fourier transform infrared spectroscopy schematic diagram in block Ca-P ceramic two faces respectively;
Fig. 4 is the Fourier transform infrared spectroscopy schematic diagram of Powdered Ca-P ceramic, wherein Fig. 4 (a) represents that the method for modifying RGD at Ca-P ceramic material surface according to the embodiment of the present invention modifies the Fourier transform infrared spectroscopy schematic diagram of gained porous calcium phosphate ceramic material surface, Fig. 4 (b) represent through simple physical absorption modifies the porous calcium phosphate ceramic ground material that obtains and the Fourier transform infrared spectroscopy schematic diagram after 60 mesh sieves.
Detailed description of the invention
Be described below in detail embodiments of the invention, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has element that is identical or similar functions from start to finish.Being exemplary below by the embodiment be described with reference to the drawings, only for explaining the present invention, and can not limitation of the present invention being interpreted as.
First, the flow process of the involved in the present invention method of RGD of modifying at Ca-P ceramic material surface is described with reference to figure 1.
Concrete, involved in the present invention comprises the following steps in the method for Ca-P ceramic material surface modification RGD:
A) Ca-P ceramic is provided;
B) described Ca-P ceramic is placed in oxalic acid aqueous solution to make described Ca-P ceramic surface and the reaction of described oxalic acid aqueous solution, after reaction, takes out Ca-P ceramic;
C) chloroformic solution being placed in EDC/NHS with the reacted Ca-P ceramic of described oxalic acid aqueous solution is reacted, after reaction, take out Ca-P ceramic;
D) ethanol water being placed in RGD with the reacted Ca-P ceramic of the chloroformic solution of described EDC/NHS is reacted, the Ca-P ceramic of the RGD modification effect that is enhanced.
Thus, according to the method for modifying RGD at Ca-P ceramic material surface of the embodiment of the present invention, RGD is combined with Ca-P ceramic material surface by chemical bond, and adhesion effectively improves; This method of modifying does not introduce toxophore at Ca-P ceramic material surface, does not affect its use in bio-medical field; And operation is simple for the method for modification RGD of the present invention, can reduce costs.
About described Ca-P ceramic, it is to be appreciated that the shape of described Ca-P ceramic is not particularly limited, such as can in the form of sheets, block, cellular or Powdered.The composition of described Ca-P ceramic mainly comprises hydroxyapatite and bata-tricalcium phosphate, and mass percent shared by wherein said hydroxyapatite is 0 ~ 100%.
The preparation method of described Ca-P ceramic is also not particularly limited, the preparation method of such as lamellar Ca-P ceramic can be: take hydroxyapatite 35g and bata-tricalcium phosphate 65g respectively, add 50mL ethanol and 50mL water, under 110r/min condition, 24h is ground with planetary ball mill, 24h is dried at 70 DEG C, cross 80 mesh sieves, with vulcanizer at 10MPa tableting under pressure, sheet is of a size of
sinter at 1250 DEG C, insulation 2h, obtains Ca-P ceramic material.
Concrete operation method about step b) is not particularly limited, such as, can comprise:
B-1) oxalic acid aqueous solution is prepared;
B-2) Ca-P ceramic is put into described oxalic acid aqueous solution to react;
B-3) take out reacted Ca-P ceramic, dry with deionized water rinsing.
About the compound method of oxalic acid aqueous solution, adopt conventional reagent compound method, the concentration of oxalic acid aqueous solution preferably but be not defined as 10
-5~ 10
-3mol/L.In step b-2) in, in order to make Ca-P ceramic and oxalic acid aqueous solution fully react, its response time can be defined as 0.5 ~ 2h.
Step c) concrete operation step can comprise:
The NHS of the EDC and 1 ~ 9 weight portion that c-1) take 1 ~ 9 weight portion is dissolved in chloroform, leaves standstill more than 1 hour to dissolve described EDC and NHS under ventilation condition after stirring;
C-2) be placed in the chloroformic solution of described EDC/NHS by with the reacted Ca-P ceramic of described oxalic acid aqueous solution, continuous stirring is fully reacted to make the chloroformic solution of Ca-P ceramic and described EDC/NHS;
C-3) take out reacted Ca-P ceramic, successively rinse with chloroform and acetone, dry.
About step c-1) in the control of ventilation condition be not particularly limited, as long as can air circulation be ensured, such as can by described EDC and NHs stirring and dissolving in fume hood.
In order to ensure that the chloroformic solution of Ca-P ceramic and described EDC/NHS can fully react, in step c-2) in can continuous stirring reaction solution 6 ~ 36h.
Steps d) concrete operation step can comprise:
D-1) be dissolved in deionized water by dehydrated alcohol, dose volume mark is the ethanol water of 10 ~ 100%;
D-2) RGD is dissolved in described ethanol water, forms the RGD solution that concentration is 1 ~ 5mg/mL;
D-3) react being placed in described RGD solution with the reacted Ca-P ceramic of the chloroformic solution of described EDC/NHS;
D-4) take out reacted Ca-P ceramic, rinse Ca-P ceramic surface with alcoholic solution, dry the Ca-P ceramic of the RGD modification effect that is enhanced.
Modification effect can be played fully, in steps d-3 to make RGD) in, the response time of described Ca-P ceramic in described RGD solution is preferably 6 ~ 36h.
Thus, the Ca-P ceramic of the RGD modification effect that just can be enhanced.
Below in conjunction with specific embodiment, the method for modifying RGD at Ca-P ceramic material surface according to the embodiment of the present invention is described.
Embodiment 1
Take hydroxyapatite 35g and bata-tricalcium phosphate 65g respectively, add 50mL ethanol and 50mL water, grind 24h with planetary ball mill under 110r/min condition, at 70 DEG C, dry 24h, cross 80 mesh sieves, with vulcanizer at 10MPa tableting under pressure, sheet is of a size of
sinter at 1250 DEG C, insulation 2h, obtains Ca-P ceramic material.
It is 5 × 10 that the Ca-P ceramic material that sintering obtains is placed in concentration
-4process 2h in the oxalic acid aqueous solution of mol/L, deionized water rinsing surface is also dried.
The material that oxalic acid treatment is crossed be placed in 20mL concentration be 1mgEDC+1mgNHS/mL from spoon chloroformic solution, continuous stirring 24h, rinses surface and also dries.
Above-mentioned material to be placed in 10mL solvent be volume fraction be 50% alcoholic solution, concentration is process 24h in the RGD solution of 1mg/mL, rinses surface with the alcoholic solution that volume fraction is 50% and dries.
Fig. 2 be through said method carry out RGD modify Ca-P ceramic material surface (a) that obtains and through simple physical absorption modify obtain the Fourier transform infrared spectroscopy comparison diagram of Ca-P ceramic surface (b).Comparison diagram 2 (a) is visible with Fig. 2 (b), and the method through above-mentioned chemical bonding is modified, material surface 1715cm
-1the C=O peak of place's carboxyl, 1580cm
-1the N-H peak at place, 1640cm
-1there is obvious enhancing at C-N peak in place's amido link, shows that the RGD of material surface obviously increases.Method by chemical bonding is described, the modification effect of material surface RGD strengthens greatly.
Embodiment 2
Take hydroxyapatite 100g, add 50mL ethanol and 50mL water, under 110r/min condition, 24h is ground with planetary ball mill, at 70 DEG C, dry 24h, cross 80 mesh sieves, with vulcanizer at 10MPa pressure block, block is of a size of 10 × 10 × 10mm, sinter at 1250 DEG C, insulation 2h, obtains Ca-P ceramic material.
It is 2 × 10 that the Ca-P ceramic material that sintering obtains is placed in concentration
-5process 2h in mol/L oxalic acid aqueous solution, deionized water rinsing surface is also dried.
Material oxalic acid treatment crossed is placed in the chloroformic solution that 20mL concentration is 1mgEDC+0.75mgNHS/mL, continuous stirring 24h, rinses surface and dries.
Above-mentioned material being placed in 10mL concentration is that the ethanol solution of the RGD of 2mg/mL processes 24h, rinses surface and also dries, and appoints the two sides Fourier transform infrared spectroscopy getting block materials to carry out analyzing to obtain Fig. 2.
As seen from Figure 3, appoint the two sides (Fig. 3 (a), Fig. 3 (b)) of getting all at 1715cm
-1there is the C=O peak of carboxyl in place, 1640cm
-1there is the C-N peak in amido link in place, showing two tested surfaces all has more RGD exist.Namely the method is also applicable to the modification of block materials.
Embodiment 3
Take hydroxyapatite 70g and bata-tricalcium phosphate 30g, add 50mL ethanol, 50mL water and PVA, dextrin and Polyethylene Glycol, under 110r/min condition, grind 24h with planetary ball mill and make slurry, sponge soaking paste, naturally sinter at 1250 DEG C after drying in the shade, insulation 2h, obtains porous calcium phosphate ceramic material.
It is 2 × 10 that the Ca-P ceramic material that sintering obtains is placed in concentration
-4process 2h in the oxalic acid aqueous solution of mol/L, deionized water rinsing surface is also dried.
Material oxalic acid treatment crossed is placed in the chloroformic solution that 20mL concentration is 0.5mgEDC+1mgNHS/mL, continuous stirring 36h, rinses surface and dries.
Above-mentioned material to be placed in 10mL solvent be volume fraction be 20% alcoholic solution, concentration is process 36h in the RGD solution of 3mg/mL, rinses surface with the alcoholic solution that volume fraction is 20% and dries.
Fig. 4 is that said method carries out RGD and modifies the porous calcium phosphate ceramic material that obtains and modify the porous calcium phosphate ceramic ground material that obtains and Fourier transform infrared spectroscopy comparison diagram after crossing 60 mesh sieves through simple physical absorption.As seen from Figure 4, porous material carries out after RGD modification, at 1715cm through said method
-1there is the C=O peak of carboxyl in place, 1640cm
-1there is the C-N peak in amido link in place, illustrates and porous material inner surface has more RGD to exist.Namely the method also can be modified porous material inner surface.
In the description of this description, specific features, structure, material or feature that the description of reference term " embodiment ", " some embodiments ", " example ", " concrete example " or " some examples " etc. means to describe in conjunction with this embodiment or example are contained at least one embodiment of the present invention or example.In this manual, identical embodiment or example are not necessarily referred to the schematic representation of above-mentioned term.And the specific features of description, structure, material or feature can combine in an appropriate manner in any one or more embodiment or example.
Although illustrate and describe embodiments of the invention, those having ordinary skill in the art will appreciate that: can carry out multiple change, amendment, replacement and modification to these embodiments when not departing from principle of the present invention and aim, scope of the present invention is by claim and equivalents thereof.
Claims (6)
1. modify a method of RGD at Ca-P ceramic material surface, it is characterized in that, comprise the following steps:
A) provide Ca-P ceramic, described Ca-P ceramic is hydroxyapatite, bata-tricalcium phosphate or its mixture;
B) described Ca-P ceramic is placed in oxalic acid aqueous solution to make described Ca-P ceramic surface and the reaction of described oxalic acid aqueous solution, take out Ca-P ceramic after reaction, the concentration of described oxalic acid aqueous solution is 10
-5~ 10
-3mol/L, Ca-P ceramic and described oxalic acid aqueous solution react 0.5 ~ 2h;
C) chloroformic solution being placed in EDC/NHS with the reacted Ca-P ceramic of described oxalic acid aqueous solution is reacted, after reaction, take out Ca-P ceramic;
D) reacted by the ethanol water being placed in RGD with the reacted Ca-P ceramic of the chloroformic solution of described EDC/NHS, described Ca-P ceramic reacts 6 ~ 36h in RGD solution, the Ca-P ceramic of the RGD modification effect that is enhanced.
2. according to claim 1ly modify the method for RGD at Ca-P ceramic material surface, it is characterized in that, described Ca-P ceramic in the form of sheets, block, cellular or Powdered.
3. method of modifying RGD at Ca-P ceramic material surface according to claim 1, is characterized in that, described step b) comprising:
B-1) oxalic acid aqueous solution is prepared;
B-2) Ca-P ceramic is put into described oxalic acid aqueous solution to react;
B-3) take out reacted Ca-P ceramic, dry with deionized water rinsing.
4. method of modifying RGD at Ca-P ceramic material surface according to claim 1, is characterized in that, described step c) comprising:
The NHS of the EDC and 1 ~ 9 weight portion that c-1) take 1 ~ 9 weight portion is dissolved in chloroform, leaves standstill more than 1 hour to dissolve described EDC and NHS under ventilation condition after stirring;
C-2) be placed in the chloroformic solution of described EDC/NHS by with the reacted Ca-P ceramic of described oxalic acid aqueous solution, continuous stirring is fully reacted to make the chloroformic solution of Ca-P ceramic and described EDC/NHS;
C-3) take out reacted Ca-P ceramic, successively rinse with chloroform and acetone, dry.
5. method of modifying RGD at Ca-P ceramic material surface according to claim 4, is characterized in that, in step c-2) middle stirring 6 ~ 36h.
6. method of modifying RGD at Ca-P ceramic material surface according to claim 1, is characterized in that, described steps d) comprising:
D-1) be dissolved in deionized water by dehydrated alcohol, dose volume mark is the ethanol water of 10 ~ 100%;
D-2) RGD is dissolved in described ethanol water, forms the RGD solution that concentration is 1 ~ 5mg/mL;
D-3) react being placed in described RGD solution with the reacted Ca-P ceramic of the chloroformic solution of described EDC/NHS;
D-4) take out reacted Ca-P ceramic, rinse Ca-P ceramic surface with alcoholic solution, dry the Ca-P ceramic of the RGD modification effect that is enhanced.
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| CN108785741A (en) * | 2018-06-22 | 2018-11-13 | 苏州市贝克生物科技有限公司 | Bone defect graphene packing material |
| CN111848741B (en) * | 2020-07-22 | 2021-06-15 | 中国人民解放军陆军军医大学第一附属医院 | Peptide, peptide-modified DBM (DBM) scaffold, and preparation method and application thereof |
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2012
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Patent Citations (6)
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| CN1247474A (en) * | 1997-02-20 | 2000-03-15 | 默克专利股份公司 | Bone substitute material with surface coating of peptides having RGD amino acid sequence |
| WO2002040073A1 (en) * | 2000-11-20 | 2002-05-23 | Université De Genève | Endosseous implant |
| JP3771510B2 (en) * | 2001-04-13 | 2006-04-26 | 泰彦 田畑 | Tissue regeneration material |
| CN1631973A (en) * | 2004-11-26 | 2005-06-29 | 中国科学院长春应用化学研究所 | Method for preparing bioceramic and biodegradable aliphatic polyester composite materials |
| CN1919360A (en) * | 2006-09-14 | 2007-02-28 | 同济大学 | Polylactic acid base/nano hydroxyapatite biological material and preparation method thereof |
| CN102085388A (en) * | 2011-01-28 | 2011-06-08 | 浙江大学 | Preparation method of hybrid coating containing polypeptide chain segment |
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| Title |
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| Role of carboxylate chelating agents on the chemical, structural and textural properties of hydroxyapatite;Karima Achelhi et al.;《Dalton Trans》;20100930;10644-10651 * |
| 羟基磷灰石表面改性_功能化及其应用研究;杨春莉;《中国博士学位论文全文数据库》;20101215;19-22 * |
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