CN107929807A - The compound polycaprolactone material of strontium-doped hydroxyapatite and its preparation and application - Google Patents
The compound polycaprolactone material of strontium-doped hydroxyapatite and its preparation and application Download PDFInfo
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- CN107929807A CN107929807A CN201711221079.0A CN201711221079A CN107929807A CN 107929807 A CN107929807 A CN 107929807A CN 201711221079 A CN201711221079 A CN 201711221079A CN 107929807 A CN107929807 A CN 107929807A
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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
- A61L27/02—Inorganic materials
- A61L27/12—Phosphorus-containing materials, e.g. apatite
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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
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/047—Other specific metals or alloys not covered by A61L27/042 - A61L27/045 or A61L27/06
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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
- A61L27/14—Macromolecular materials
- A61L27/18—Macromolecular materials obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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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
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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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
- A61L27/50—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
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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
- A61L27/50—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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y80/00—Products made by additive manufacturing
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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
- 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
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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
- 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
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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
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
Abstract
The present invention provides a kind of compound polycaprolactone material of strontium-doped hydroxyapatite and its preparation and application.The compound polycaprolactone material of the strontium-doped hydroxyapatite, it is characterised in that formed by mixing strontium nanometer hydroxyapatite and polycaprolactone.The method of the present invention is easy to operate, and using the synthetic material with good biocompatibility, SrHA's mixes that strontium amount can select, the compositely proportional of SrHA and PCL can be adjusted, stent micro-structure can regulate and control for the stent of preparation；SrHA/PCL stents prepared by the present invention can sustained release strontium element, have the bioactivity stent be expected to be used for clinically bulk bone defect healing.
Description
Technical field
The invention belongs to the preparation field of tissue engineering bracket, more particularly to a kind of strontium-doped hydroxyapatite is compound gathers in oneself
Ester material and its preparation and the application in 3D printing bone stent.
Background technology
Bone tissue engineer is planted the seed cell of in vitro culture in synthesis using biology and the technology of organizational engineering
Or on natural extracellular matrix carriers, and multiple correlation inducible factor, implant and achieve the purpose that bone defect position is repaired,
To solve the problems, such as that bone defect healing provides broader practice prospect.A key issue for limiting its development is exactly to be difficult to make
Preferable carrier bracket is produced, and the development of 3D printing technique makes this problem be expected to be resolved.3D printing technique can be very
The controllability of the porosity of stent, aperture, pore volume, space arrangement and other surfaces characteristic is realized in big degree, it is thus possible to
Realize the preparation of excellent bone tissue engineering scaffold, be to realize various bone surgery individuations, the effective means of precision.However,
The 3D printing bone repairing support clinically used at present is mostly metallic support, can not be degraded in vivo；Hydrogel 3D printing
Although stent has a good biocompatibility and superior biological degradability, but in mechanical property there is it is certain the defects of.
Therefore, it is still a challenging research to explore a kind of new 3D printing material to be used for orthopaedics repairing and treating.
The micro- such as growth of strontium, magnesium to bone in human body has very important effect.It is micro in human body
The element such as growth to bone such as strontium, magnesium has very important effect.Congeners of the strontium as calcium, in alternative hydroxyapatite
Calcium be used for bone tissue engineer as saamite solid solution.Influence of the strontium to bone metabolism has gradually obtained the accreditation of researcher,
Its mechanism of action is that can influence the duplication and differentiation of preosteoblast, on this basis promoting bone growing, while can suppress again
Osteoclast breaks up, and promotes its apoptosis, so as to suppress bone information, and does not influence the effect of bone mineralising.PCL has had been found good
Histocompatbility, biodegradation and permeability, be easy to plasticity, it is cheap, in osteoblast and HA/PCL 3D printing stents
Find that osteoblast is easier to be attached on the features such as being grown on HA/PCL 3D printing stents in compound in vitro culture, but stent
Repairing and treating is in the form of a single.Therefore, prepare strontium-doped hydroxyapatite/polycaprolactone composite material and be used for the artificial bone tissue of 3D printing
It is worthy of expecting that stent is used for personalized treatment research.
The content of the invention
The purpose of the present invention is just to provide for a kind of material available for bone defect healing 3D printing stent and its preparation
And application.
In order to achieve the above object, the present invention provides a kind of compound polycaprolactone material of strontium-doped hydroxyapatite, it is special
Sign is, is formed by mixing strontium nanometer hydroxyapatite and polycaprolactone.
Present invention also offers a kind of 3D printing bone stent, it is characterised in that compound by above-mentioned strontium-doped hydroxyapatite
Polycaprolactone material is made.
Present invention also offers the preparation method of above-mentioned 3D printing bone stent, it is characterised in that including：
Step 1：Prepare the compound polycaprolactone material of strontium-doped hydroxyapatite；
Step 2：By compound polycaprolactone material use melting rapid shaping processing technology (FDM) system of strontium-doped hydroxyapatite
Standby 3D printing bone stent.
Preferably, the preparation method of the compound polycaprolactone material of the strontium-doped hydroxyapatite includes：Hydro-thermal method synthesizes
Strontium nanometer hydroxyapatite (SrHA) is mixed, then is washed through ethanol and removes impurity, centrifugation, after drying grinding, the strontium of mixing of gained is received
Rice hydroxyapatite is added in solvent with polycaprolactone, and stirring makes it fully mix, and is removed solvent, is obtained mixing strontium hydroxy-apatite
The compound polycaprolactone material (SrHA/PCL) of stone.
It is highly preferred that the solvent is tetrahydrofuran.
Preferably, mix the strontium nanometer hydroxyapatite and the mass ratio of polycaprolactone are 10%-50%.
Preferably, the content of strontium mixed in strontium nanometer hydroxyapatite is 5%-10%.
Preferably, mix the strontium nanometer hydroxyapatite and the mass ratio of polycaprolactone are 1: 9-5: 5.
Preferably, mix the strontium nanometer hydroxyapatite and the mass ratio of polycaprolactone are 1: 9,3: 7 or 5: 5.
Preferably, the 3D printing bone stent is loose structure.
Preferably, the melting rapid shaping processing technology is included the compound polycaprolactone material of strontium-doped hydroxyapatite
Adding heating in the melter of Flashmelt rapid shaping instrument makes its melting, and curing accumulation in layer by syringe needle extrusion prepares 3D
Print bone stent.
The 3D printing stent of the present invention is supervised by mixing strontium nanometer hydroxyapatite (SrHA) powder and U.S.'s food and medicine
Superintend and direct biological medical polymer material polycaprolactone (PCL) composition of management board (FDA) approval.
Strontium nanometer hydroxyapatite is mixed using what hydro-thermal method prepared that difference mixes strontium ratio；Described is mixed into strontium nano hydroxyapatite
Lime stone prepares composite material by certain mass ratio with polycaprolactone and is used for 3D printing；Using melting rapid shaping processing technology
(FDM) preparing the composite material has porous controllable composite material bracket.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) present invention is easy to operate, and the composite material that can prepare different proportion is used to prepare 3D printing bone repairing support；
(2) material that preparation method of the present invention uses all is the good biomaterial of biocompatibility, to the nontoxic pair of body
Effect, and releasable strontium element in vivo, reach more preferable therapeutic effect；
(3) macropore stent prepared by the present invention has excellent operability.
(4) the method for the present invention is easy to operate, and the stent of preparation uses the synthetic material with good biocompatibility,
SrHA's mixes that strontium amount can select, the compositely proportional of SrHA and PCL can be adjusted, stent micro-structure can regulate and control；Present invention system
Standby SrHA/PCL stents can sustained release strontium element, the stent with the bioactivity is expected to be used for clinically bulk bone and lacks
Damage is repaired.
Brief description of the drawings
Fig. 1 is the biomaterial SrHA phenograms available for bone defect healing prepared by hydro-thermal method, and A is the TEM of Sr0HA
Picture B is the TEM of Sr10HA, and C is its XRD diagram piece.
Fig. 2 is the SEM pictures for printing the 3D printing stent that SrHA/PCL ratios are 1: 9, and wherein A is surface, and B is section,
The strontium nanometer hydroxyapatite of mixing added is Sr10HA。
Fig. 3 is the Sr release conditions of different composite material 3D printing stent sample under conditions in vitro, and strontium nanometer is mixed in addition
Hydroxyapatite is Sr10HA.Wherein PCL-50SrHA is that PCL/SrHA mass ratioes are that 5: 5, PCL-30SrHA is PCL/SrHA matter
Amount is than being that PCL/SrHA mass ratioes are 9: 1 for 7: 3, PCL-10SrHA.
Fig. 4 is the 3D printing stent displaying of different printing apertures and structure.
Embodiment
With reference to specific embodiment, the present invention is further explained.It is to be understood that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Scope.
Embodiment 1
A kind of 3D printing bone stent is made of the compound polycaprolactone material of strontium-doped hydroxyapatite.Described mixes strontium hydroxyl phosphorus
The compound polycaprolactone material of lime stone is formed by mixing strontium nanometer hydroxyapatite and polycaprolactone.
The preparation method of above-mentioned 3D printing bone stent includes：
Step 1：Prepare the compound polycaprolactone material of strontium-doped hydroxyapatite：Strontium nanometer hydroxyapatite is mixed in hydro-thermal method synthesis
Sr10HA, specific preparation process are as follows：Prepare Sr (NO respectively first3)2, Ga (NO3)2·4H2O and NH4H2PO40.5mol/L
Aqueous solution it is spare, with containing NH3Solution pH value is adjusted for 25~28% ammonium hydroxide, makes Sr (NO3)2Solution and Ga (NO3)2·4H2O
Solution PH >=11, and NH4H2PO4Solution PH >=10；Sr (the NO of 10mL are added in reaction vessel3)2The Ga of solution and 90mL
(NO3)2·4H2O solution first reacts 1h in 80 DEG C of magnetic agitation 400rpm/min so that Sr (NO3)2Solution and Ga (NO3)2·
4H2O solution is sufficiently mixed, and obtains mixed solution.By NH under stirring condition4H2PO4Solution is slowly dropped to above-mentioned mixed solution
In, ensure that n (Ga+Sr)/n (P)=1.67, n is molal quantity, sustained response 6h.After reaction, reaction product is by second three times
Alcohol is washed, washed, and 6000rpm centrifugation 10min, by the whiteness being collected into, grinding obtains mixing strontium hydroxyl phosphorus after 60 DEG C of drying
Lime stone powder sample, be finally collected into 50mL centrifuge tubes be placed on it is spare in drying box；The Sr of gained10The TEM and XRD diagram piece of HA
Respectively as shown in Figure 1B and C.
By 1g Sr10HA is added to 10mL tetrahydrochysenes with 9g polycaprolactones (Sigma-Aldrich, Mn=45000)
In furans, stirring makes it fully mix, and tetrahydrofuran is removed in fume hood, obtains the compound polycaprolactone material of strontium-doped hydroxyapatite
Expect (SrHA/PCL).
Step 2：By compound polycaprolactone material use melting rapid shaping processing technology (FDM) system of strontium-doped hydroxyapatite
Standby 3D printing bone stent, concretely comprises the following steps：It is rapid-result soon that the compound polycaprolactone material of strontium-doped hydroxyapatite is added into Flashmelt
95 DEG C are heated in the melter of type instrument makes its melting, and curing accumulation in layer by 21G syringe needles extrusion prepares porous 3D printing
Bone stent, as shown in Figure 2 and Figure 4.
Embodiment 2
Similar to embodiment, difference lies in, in the step 1, Sr10The mass ratio of HA and polycaprolactone is 5: 5.
Embodiment 3
Similar to embodiment, difference lies in, in the step 1, Sr10The mass ratio of HA and polycaprolactone is 3: 7.
The 3D printing stent of 10mg is weighed, is placed in the PBS buffer (containing 0.02%NaN3) that the pH containing 10mL is 7.4
In centrifuge tube, it is placed in the constant-temperature table that temperature is 37 DEG C and rotating speed is 100rpm.Until the time point of setting, in taking-up
The liquid 5mL in face simultaneously suctions out surplus liquid, then adds the PBS buffer (containing 0.02%NaN3) that fresh pH is 7.4.Most
The sustained-release liquid being collected into is detected by inductively coupled plasma courtyard emission spectrometer (ICP-AES) afterwards, calculates Sr2+
Total burst size and draw elution profiles, as shown in Figure 3.
Comparative example 1
Prepare the compound polycaprolactone material of strontium-doped hydroxyapatite：Hydro-thermal method synthesis nanometer hydroxyapatite Sr0HA：Specifically
Step is with reference to Sr10HA synthesis steps, by the Sr (NO of 10mL3)2Solution changes the Ga (NO of 10mL into3)2·4H2O solution, that is, 100mL
Ga (NO3)2·4H2O solution, Sr is synthesized according to n (Ga)/n (P)=1.670HA)；The Sr of gained0The TEM and XRD diagram piece point of HA
Not as shown in Figure 1A and C.
Claims (9)
1. a kind of compound polycaprolactone material of strontium-doped hydroxyapatite, it is characterised in that by mixing strontium nanometer hydroxyapatite and gathering
Caprolactone forms.
2. a kind of 3D printing bone stent, it is characterised in that be made of the above-mentioned compound polycaprolactone material of strontium-doped hydroxyapatite.
3. the preparation method of the 3D printing bone stent described in claim 2, it is characterised in that including：
Step 1：Prepare the compound polycaprolactone material of strontium-doped hydroxyapatite；
Step 2：The compound polycaprolactone material use melting rapid shaping processing technology of strontium-doped hydroxyapatite is prepared into 3D printing
Bone stent.
4. the preparation method of 3D printing bone stent as claimed in claim 3, it is characterised in that the strontium-doped hydroxyapatite
The preparation method of compound polycaprolactone material includes：Strontium nanometer hydroxyapatite is mixed in hydro-thermal method synthesis, then is washed and removed through ethanol
Impurity, centrifugation, after drying grinding, the strontium nanometer hydroxyapatite of mixing of gained are added in solvent with polycaprolactone, stirring makes
It is fully mixed, and is removed solvent, is obtained the compound polycaprolactone material of strontium-doped hydroxyapatite.
5. the preparation method of 3D printing bone stent as claimed in claim 4, it is characterised in that the solvent is tetrahydrochysene furan
Mutter.
6. the preparation method of 3D printing bone stent as claimed in claim 3, it is characterised in that described mixes strontium nano hydroxyapatite
The mass ratio of lime stone and polycaprolactone is 1: 9-5: 5.
7. the preparation method of 3D printing bone stent as claimed in claim 3, it is characterised in that described mixes strontium nano hydroxyapatite
The mass ratio of lime stone and polycaprolactone is 1: 9,3: 7 or 5: 5.
8. the preparation method of 3D printing bone stent as claimed in claim 3, it is characterised in that the 3D printing bone stent is
Loose structure.
9. the preparation method of 3D printing bone stent as claimed in claim 3, it is characterised in that the melting rapid shaping adds
Work technology includes adding strontium-doped hydroxyapatite compound polycaprolactone material in the melter of Flashmelt rapid shaping instrument and adds
Heat makes its melting, and curing accumulation in layer by syringe needle extrusion prepares 3D printing bone stent.
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| CN110665057A (en) * | 2019-11-07 | 2020-01-10 | 上海健康医学院 | Preparation method of hydroxyapatite/PLGA double-layer stent |
| CN111991618A (en) * | 2020-09-01 | 2020-11-27 | 上海交通大学医学院附属第九人民医院 | Bioactive three-dimensional nanofiber scaffold and application thereof |
| CN115105644A (en) * | 2022-07-19 | 2022-09-27 | 南京屹特博医学科技发展有限公司 | 3D printing artificial bone repair material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110665057A (en) * | 2019-11-07 | 2020-01-10 | 上海健康医学院 | Preparation method of hydroxyapatite/PLGA double-layer stent |
| CN111991618A (en) * | 2020-09-01 | 2020-11-27 | 上海交通大学医学院附属第九人民医院 | Bioactive three-dimensional nanofiber scaffold and application thereof |
| CN115105644A (en) * | 2022-07-19 | 2022-09-27 | 南京屹特博医学科技发展有限公司 | 3D printing artificial bone repair material and preparation method thereof |
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