CN108355166A - A kind of mesopore bioactive glass/metal organic frame timbering material and preparation method - Google Patents
A kind of mesopore bioactive glass/metal organic frame timbering material and preparation method Download PDFInfo
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- CN108355166A CN108355166A CN201810459567.3A CN201810459567A CN108355166A CN 108355166 A CN108355166 A CN 108355166A CN 201810459567 A CN201810459567 A CN 201810459567A CN 108355166 A CN108355166 A CN 108355166A
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
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- A61L27/18—Macromolecular materials obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- A—HUMAN NECESSITIES
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/10—Ceramics or glasses
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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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- 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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- 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
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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
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Abstract
The invention discloses a kind of mesopore bioactive glass/metal organic frame compound support frame materials and preparation method thereof.The preparation method includes the steps that preparing mesopore bioactive glass/metal organic frame composite printing ink；With CAD/CAM computer-aided software engineering timbering materials appearance and internal structure the step of；Low temperature 3D printing technique prepares the step of mesopore bioactive glass/metal organic frame compound support frame material.Mesopore bioactive glass prepared by the present invention/metal organic frame compound support frame material has three-dimensional communication and controllable macroporous structure, mechanical strength is high, biocompatibility is good and can promote proliferation, differentiation and the skeletonization of human bone marrow's interstital stem cell, is expected to provide new strategy for the repairing and treating of clinically large segmental bone defect.
Description
Technical field
The invention belongs to materialogy fields, are related to a kind of bone tissue engineering stent material, and in particular to a kind of mesoporous biological
Activity glass/metal organic frame compound support frame material.
Background technology
The repairing and treating of large segmental bone defect as caused by bone tumour, traffic accident etc. is the huge challenge clinically faced.
Currently, using bone tissue engineering stent material come repairing and treating bone defect be considered as solve relevant issues effective ways it
One.Under normal conditions, bone tissue engineering stent material needs to have the porous structure of three-dimensional communication, good mechanical support
The basic demands such as energy, biodegradability and bioactivity.Therefore, design prepares the bone tissue work for meeting above-mentioned basic demand
Engineering support material is the Important Problems of repairing and treating bone defect.
Mesopore bioactive glass (MBG) has the mesopore orbit of big specific surface area and high-sequential, than common biology
Glass has higher bioactivity, while its meso-hole structure assigns drug efficiently loading and slow release characteristic, has situ drug
Slow-release function.Studies have shown that although MBG can also promote the proliferation of osteoblast, differentiation, new osteanagenesis is induced, it is dropped
It solves product inducing peripheral basic environment to increase, is unfavorable for osteocyte response.Metal organic frame (Metal-Organic
Framework, english abbreviation MOF) it is the porous crystalline substance formed by Coordinate self-assembly by metal ion or cluster and organic ligand
Body material, which part iron-based, zinc-base and zirconium base MOF materials have biocompatibility, biodegradability, are led in biological medicine
Domain shows bright application prospect；Meanwhile the aobvious faintly acid of organic ligand in MOF material degradation products, and the metal degraded
Ion can promote osteocyte to respond in a certain range.Therefore, it is prepared in conjunction with mesoporous bioglass and metal organic frame simultaneous
Structural mechanics, bioactivity, pH microenvironments and the porous compound support frame material of osteocyte response are cared for, large segmental bone defect is expected to be used for
Repairing and treating application.
Low temperature 3D printing technique can accurately control the outside of timbering material as emerging rapid shaping technique means
Shape, internal structure and the connectivity in hole.Compared to other 3D printing techniques, low temperature 3D printing simple operation does not need high temperature,
It is small to the damage of material, it can be effectively used for the preparation for carrying medicine compound support frame material.
Against the background of the prior art, to prepare mesoporous bioglass/metal organic frame with low temperature 3D printing technique compound
Timbering material is expected to provide new strategy for the repairing and treating of clinically large segmental bone defect.
Invention content
For the preparation problem of bone tissue engineering stent material, the present invention provides a kind of mesopore bioactive glass/gold
Belong to organic frame compound support frame material and preparation method thereof, the preparation method of this compound support frame material solves existing
The bone tissue engineering stent material prepared in technology is unable to the internal structure of accuracy controlling timbering material, mechanical property, pH micro-loops
The problems such as border regulates and controls and bioactivity is less desirable.
The present invention provides a kind of preparation method of mesopore bioactive glass/metal organic frame compound support frame material,
Include the following steps：
1) the step of preparing mesopore bioactive glass/metal organic frame composite printing ink, by mesopore bioactive
Glass and metal organic frame powder are uniformly mixed by certain mass ratio, are crossed the sieve of 200~600 mesh, are then taken certain mass
Mixed powder be added in the chloroform soln of polycaprolactone,
It is uniformly mixing to obtain marking ink, is then sealed；
2) CAD/CAM computer-aided software engineering mesopore bioactive glass/metal organic frame timbering material is used
Appearance and internal structure the step of, the size of timbering material model is 15 × 15 × 15
Cm and within any size and shape, internal aperture be 50~1500 μm, it is 0 ° that adjacent two layers ink, which moves towards angle,
~180 °；
3) low temperature 3D printing technique prepares the step of mesopore bioactive glass/metal organic frame timbering material, will match
The marking ink made is put into the barrel of 3D printer, and a diameter of 100~1000 μm of syringe needle, 4~8 DEG C of precoolings are then loaded onto
5-15 minutes；3D printing program is run, printer air pressure is adjusted to 1.2~5.0bar, and print speed is 2.0~8.0mm/s；It will be black
Waterline prints in the glass culture dish of article carrying platform, and precise forming obtains required mesoporous biological in the way of layer upon layer
Activity glass/metal organic frame compound support frame material, it is spare after 12-24 hours dry in 37 DEG C.
Further, the mass ratio of the mesopore bioactive glass and metal organic frame powder ranging from 99:1 to
30:Arbitrary proportion between 70.
Further, the mass volume ratio between the polycaprolactone and chloroform is 0.1g/mL to 0.15g/mL, is situated between
The mass volume ratio of hole bioactive glass/between metal organic frame mixed powder and polycaprolactone solution be 0.1g/mL extremely
1g/mL。
Further, the metal organic frame powder body material includes iron-based MOF materials MIL-100 (Fe), MIL-88
(Fe), zinc-base MOF materials ZIF-8 (Zn), ZIF-90 (Zn), appointing in zirconium base MOF materials Uio-66 (Zr), PCN-223 (Zr)
Meaning is a kind of.
The present invention also provides a kind of mesopore bioactive glass/metal organic frames being prepared using the above method
Compound support frame material.
Mesopore bioactive glass/metal organic frame timbering material of the present invention will be situated between using low temperature 3D printing technique
The excellent bioactivity of hole bioactive glass and the degradability of metal organic frame are combined, and prepare bioactive composite support
Frame material.Timbering material, which has three-dimensional communication and controllable, to be shown to the timbering material physicochemical property and biology performance detection
Macroporous structure, mechanical strength is high, biocompatibility it is good and can promote the proliferation of human bone marrow's interstital stem cell, differentiation and
Skeletonization.
The present invention is compared with prior art, and technological progress is significant.The present invention provides a kind of mesopore bioactives
The 3D printing preparation method of glass/metal organic frame timbering material.The mesopore bioactive that method through the invention obtains
Glass/metal organic frame timbering material is expected to provide new strategy for the repairing and treating of clinically large segmental bone defect.
Description of the drawings
Fig. 1 is the optical photograph of mesopore bioactive glass/metal organic frame timbering material prepared by embodiment 1
Fig. 2 is the scanning electron microscope of mesopore bioactive glass/metal organic frame timbering material prepared by embodiment 1
(SEM) figure.
Fig. 3 is mesopore bioactive glass/metal organic frame of human bone marrow's interstital stem cell prepared by embodiment 1
Scanning electron microscope (SEM) figure after being inoculated with 3 days on timbering material.
Specific implementation mode
In order to make related field researcher be better understood from technical scheme of the present invention, with reference to specific example to this
Invention is described further.
Embodiment 1
A kind of preparation method of mesopore bioactive glass/metal organic frame compound support frame material, includes the following steps：
Step 1 prepares mesopore bioactive glass/metal organic frame (MBG/MOF) composite printing ink.By MBG and
MOF powders are 90 in mass ratio:10 are uniformly mixed, and cross the sieve of 400 mesh, 0.7 gram of mixed powder is then taken to be added to 2.0 milliliters
In polycaprolactone (PCL)/chloroform soln (0.15g/mL), stirs evenly, be then sealed.
Step 2, with the appearance and internal junction of CAD/CAM computer-aided software engineering MBG/MOF compound support frame materials
Structure, timbering material model be cylinder (H=10mm), internal aperture is 400 μm, and adjacent two layers ink moves towards angle
It is 60 °.
Step 3, low temperature 3D printing technique prepare MBG/MOF compound support frame materials.Prepared marking ink is put into 3D
In the barrel of printer, a diameter of 400 microns of syringe needle is then loaded onto, 4 DEG C are pre-chilled 10 minutes；Run 3D printing program, printing
Machine air pressure is adjusted to 1.8~2.4bar, and print speed is 4.6~6.2mm/s；Ink line is printed to the glass culture of article carrying platform
In ware, precise forming obtains required MBG/MOF compound support frame materials in the way of layer upon layer, 12 hours dry in 37 DEG C
It is spare afterwards.
Embodiment 2
A kind of preparation method of mesopore bioactive glass/metal organic frame compound support frame material, includes the following steps：
Step 1 prepares MBG/MOF composite printing inks.It is 70 in mass ratio by MBG and MOF powders:30 are uniformly mixed,
The sieve of 400 mesh is crossed, 0.7 gram of polycaprolactone for being added to 3.0 milliliters (PCL)/chloroform soln (0.1g/mL) is then taken
In, it stirs evenly, is then sealed.
Step 2, the appearance with the computer-aided software engineering MBG/MOF compound support frame materials such as CAD/CAM and inside
Structure, timbering material model be cylinder (H=10mm), internal aperture is 300 μm, and adjacent two layers ink moves towards folder
Angle is 60 °.
Step 3, low temperature 3D printing technique prepare MBG/MOF compound support frame materials.Prepared marking ink is put into 3D
In the barrel of printer, a diameter of 300 microns of syringe needle is then loaded onto, 8 DEG C are pre-chilled 15 minutes；Run 3D printing program, printing
Machine air pressure is adjusted to 1.8~2.0bar, and print speed is 4.0~5.6mm/s；Ink line is printed to the glass culture of article carrying platform
In ware, precise forming obtains required MBG/MOF compound support frame materials in the way of layer upon layer, 12 hours dry in 37 DEG C
It is spare afterwards.
Embodiment 3
A kind of preparation method of mesopore bioactive glass/metal organic frame compound support frame material, includes the following steps：
Step 1 prepares MBG/MOF composite printing inks.It is 50 in mass ratio by MBG and MOF powders:50 are uniformly mixed,
The sieve of 300 mesh is crossed, 0.7 gram of polycaprolactone for being added to 3.0 milliliters (PCL)/chloroform soln (0.1g/ml) is then taken
In, it stirs evenly, is then sealed.
Step 2, with the appearance and internal junction of CAD/CAM computer-aided software engineering MBG/MOF compound support frame materials
Structure, timbering material model be cylinder (H=10mm), internal aperture is 200 μm, and adjacent two layers ink moves towards angle
It is 90 °.
Step 3, low temperature 3D printing technique prepare MBG/MOF compound support frame materials.Prepared marking ink is put into 3D
In the barrel of printer, a diameter of 200 microns of syringe needle is then loaded onto, 4 DEG C are pre-chilled 15 minutes；Run 3D printing program, printing
Machine air pressure is adjusted to 1.9~2.2bar, and print speed is 4.4~5.6mm/s；Ink line is printed to the glass culture of article carrying platform
In ware, precise forming obtains required MBG/MOF compound support frame materials in the way of layer upon layer, 12 hours dry in 37 DEG C
It is spare afterwards.
4 cell adherence test case of embodiment
Mesopore bioactive glass/metal organic frame of human bone marrow's interstital stem cell prepared by embodiment 1 is compound
Case study is adhered on timbering material, is included the following steps：
Step 1, extract according to the literature human bone marrow interstital stem cell [Matsubara T, Suardita K,
Ishii M,et al.Alveolar bone marrow as a cell source for regenerative
medicine:differences between alveolar and iliac bone marrow stromal
Cells.Journal of Bone and Mineral Research, 2005,20,399-409], cell used in subsequent experimental
All it is cell of the secondary culture to the 5th generation.
MBG/MOF compound support frame materials prepared by embodiment 1 are irradiated 24 hours and are sterilized by step 2 in the UV lamp,
It is subsequently placed into 24 well culture plates, after the wetting in advance of the l milliliters of DMEM cell culture mediums containing 10% fetal calf serum being added 24 hours
Remove culture medium.Then, 1 × 10 will be contained5100 microlitres of culture solution of human bone marrow's interstital stem cell is added drop-wise to each holder
On material, after allowing cell to adhere in advance 4 hours be added 1 milliliter contain 10% fetal calf serum DMEM cell culture mediums, and 37 DEG C,
5%CO2It is cultivated in the incubator of atmosphere.
Step 3 after cell cultivates 3 days on timbering material, is first washed three times with PBS buffer solution at 37 DEG C, is then used
PBS containing 2.5% glutaraldehyde fixes 1 hour, and fixative is removed by the buffer solution PBS containing 4% sucrose, is then passed through
PBS buffer solutions containing 1% osmium tetroxide are fixed, then by graded ethanol solutions (50%, 70%, 90%,
95%, 100%) and hexamethyldisilazane solution (HMDS) dehydration.
Step 4, the adherency situation with scanning electron microscope (FEI Quanta 450) observation cell on timbering material surface, branch
Frame material sample is adhesive in conduction on metal base, and metal spraying is carried out before observing and is handled within 60 seconds.
The results are shown in Figure 3, and human bone marrow's interstital stem cell adheres to good and complete on MBG/MOF compound support frame materials
Full drawout shows that MBG/MOF compound support frame materials are conducive to cell adherence, has good biocompatibility.
Above-mentioned preparation process can be printed by changing the mass ratio of MBG and MOF powders, the type of organic solvent, adjusting
Parameter, design different stent materials model, prepare heterogeneity content, the MBG/MOF compound rest materials of different internal structure
Material.
Physicochemical property and biology performance are carried out to the compound support frame material analysis shows, it is mesoporous prepared by the present invention
Bioactivity glass/metal organic frame timbering material has three-dimensional communication and controllable macroporous structure, and mechanical strength meets pine
Matter bone strength (2-12MPa), biocompatibility it is good and can promote the proliferation of human bone marrow's interstital stem cell, differentiation and at
Bone.Therefore, mesopore bioactive glass/metal organic frame timbering material prepared by the present invention is expected to as clinically big section of bone
The treatment zone of defect carrys out new technology.
The above content is in conjunction with specific embodiments to the further description of the invention done, and it cannot be said that the present invention
It is confined to these embodiments.Therefore, the modification and replacement in the case where not departing from present general inventive concept should belong to the guarantor of the present invention
Within the scope of shield.
Claims (6)
1. a kind of preparation method of mesopore bioactive glass/metal organic frame compound support frame material, it is characterised in that including
Following steps：
1) the step of preparing mesopore bioactive glass/metal organic frame composite printing ink, by mesopore bioactive glass
It is uniformly mixed by certain mass ratio with metal organic frame powder, crosses the sieve of 200~600 mesh, then take the mixed of certain mass
It closes powder to be added in the chloroform soln of polycaprolactone, is uniformly mixing to obtain marking ink, is then sealed；
2) the outer of CAD/CAM computer-aided software engineering mesopore bioactive glass/metal organic frame timbering material is used
See and the step of internal structure, the size of timbering material model be 15 × 15 × 15cm and within any size and shape, inside
Aperture is 50~1500 μm, and it is 0 °~180 ° that adjacent two layers ink, which moves towards angle,；
3) low temperature 3D printing technique prepares the step of mesopore bioactive glass/metal organic frame timbering material, will prepare
Marking ink put into the barrel of 3D printer, then load onto a diameter of 100~1000 μm of syringe needle, 4~8 DEG C of precooling 5-15
Minute；3D printing program is run, printer air pressure is adjusted to 1.2~5.0bar, and print speed is 2.0~8.0mm/s；By ink line
In the glass culture dish for printing to article carrying platform, precise forming obtains required mesopore bioactive in the way of layer upon layer
Glass/metal organic frame compound support frame material, it is spare after 12-24 hours dry in 37 DEG C.
2. a kind of preparation of mesopore bioactive glass/metal organic frame compound support frame material according to claim 1
Method, it is characterised in that：The mass ratio of mesopore bioactive glass and metal organic frame powder ranging from 99:1 to 30:70 it
Between arbitrary proportion.
3. a kind of preparation of mesopore bioactive glass/metal organic frame compound support frame material according to claim 1
Method, it is characterised in that：Mass volume ratio between polycaprolactone and chloroform is 0.1g/mL-0.15g/mL.
4. a kind of preparation of mesopore bioactive glass/metal organic frame compound support frame material according to claim 1
Method, it is characterised in that：The quality of mesopore bioactive glass/between metal organic frame mixed powder and polycaprolactone solution
Volume ratio is 0.1g/mL to 1g/mL.
5. a kind of preparation of mesopore bioactive glass/metal organic frame compound support frame material according to claim 1
Method, it is characterised in that：The metal organic frame powder body material includes iron-based MOF materials MIL-100 (Fe), MIL-88
(Fe), zinc-base MOF materials ZIF-8 (Zn), ZIF-90 (Zn), appointing in zirconium base MOF materials Uio-66 (Zr), PCN-223 (Zr)
Meaning is a kind of.
6. a kind of mesopore bioactive glass/metal organic frame compound support frame material, it is characterised in that：Use claim 1
It is prepared to 5 any one the methods.
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