CN107050506A - A kind of bone tissue engineering stent material of fibre-reinforced Injectable in-situ solidification and pore-forming and preparation method thereof - Google Patents
A kind of bone tissue engineering stent material of fibre-reinforced Injectable in-situ solidification and pore-forming and preparation method thereof Download PDFInfo
- Publication number
- CN107050506A CN107050506A CN201710303911.5A CN201710303911A CN107050506A CN 107050506 A CN107050506 A CN 107050506A CN 201710303911 A CN201710303911 A CN 201710303911A CN 107050506 A CN107050506 A CN 107050506A
- Authority
- CN
- China
- Prior art keywords
- bone tissue
- tissue engineering
- polylactide
- hydroxyapatite
- bracket material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/06—Flowable or injectable implant compositions
-
- 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
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Transplantation (AREA)
- Dermatology (AREA)
- Medicinal Chemistry (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Materials For Medical Uses (AREA)
Abstract
Solidify bone tissue engineering stent material with pore-forming and preparation method thereof the invention belongs to field of medical materials, more particularly to a kind of fibre-reinforced Injectable in-situ.The injectable bone tissue engineering bracket material that the present invention is provided includes：Polylactide, hydroxyapatite, polyglycollide fibre and organic solvent；The ratio of the polylactide, hydroxyapatite and polyglycollide fibre gross mass and organic solvent volume is (5~10) g：(10~50) mL.The present invention, as the solute component of injectable bone tissue engineering bracket material, has been obviously improved the mechanical strength after injection solidification using polylactide, hydroxyapatite and polyglycollide fibre.Test result indicates that, compression strength >=15MPa after the injectable bone tissue engineering bracket material curing molding that the present invention is provided, modulus of elasticity >=15MPa.
Description
Technical field
The invention belongs to the bone of field of medical materials, more particularly to a kind of fibre-reinforced Injectable in-situ solidification and pore-forming
Tissue engineering bracket material and preparation method thereof.
Background technology
According to statistics, Cranial defect patient of the China every year caused by disease, wound, tumour etc. becomes more than 1,000,000, and in rising
Gesture.Autologous bone transplanting and homogeneous allogenic bone transplantation are the main methods of current treatment Cranial defect.However, autologous bone limited source,
And cause new defect to donor site, using being restricted.Homogeneous allogenic bone self-bone grafting ability is poor compared with autologous bone, and there is row
Reprimand reaction and the danger of transmission.In recent years, increasing Inorganic synthese material or organic synthesis high polymer material quilt
Research and development is progressively applied to clinic as bone tissue engineering scaffold or bone renovating material.
At present, clinically conventional bone tissue engineering scaffold or bone renovating material is mainly the moulding hard of external preparation
Property graft materials, such as decalcification bone (DBM)/collagen-based composite.However, clinically being controlled using moulding rigid graft materials
Problems with is frequently run onto when treating Cranial defect：1. defect lacuna is often irregular, and graft materials can not be attached closely with host bone,
The stress growth creeped with bone tissue of Gegenbaur's cell is influenceed, and material easily comes off from defect；2. wound is big, bone
Defect surrounding soft tissue includes blood vessel, muscle etc. and is often damaged than more serious, and routine operation cuts Cranial defect neoplasty again
The further damage of soft tissue can be caused, the bridge joint of final influence bone and fusion.3. operating time is longer, adds postoperative infection
Risk and operation cost.
The problem of to solve to run into during rigid graft materials treatment Cranial defect, injectable bone tissue engineering bracket material is opened
Issue.Injectable bone tissue engineering bracket material is mainly made up of high molecular polymer and organic solvent, conventional macromolecule
Polymer includes the biodegradable polymer such as PLA (PLA) or polylactide-co-glycolide (PLGA), and conventional is organic
Solvent includes METHYLPYRROLIDONE (NMP) etc..Injectable bone tissue engineering bracket material is being injected into Cranial defect position
Afterwards, organic solvent is replaced rapidly by the water in bone tissue, the shaping of high molecular polymer in-situ solidifying, and bone can be filled up completely with rapidly and is lacked
Position is damaged, realizes that graft materials are matched with the complete of host's Cranial defect, effectively the growth of stress of guiding or stimulation bone tissue.This
Outside, because injectable bone tissue engineering bracket material can't cause big wound when treating Cranial defect, it is to avoid Cranial defect
The damage again of position surrounding soft tissue, operating time is short.But existing injectable bone tissue engineering bracket material is after hardening
Mechanical strength it is generally relatively low, seriously constrain its application in bone defect healing.
The content of the invention
In view of this, it is an object of the invention to provide a kind of fibre-reinforced Injectable in-situ solidification and the bone group of pore-forming
Engineering scaffold material and preparation method thereof is knitted, is had after the injectable bone tissue engineering bracket material solidification that the present invention is provided higher
Mechanical strength.
The invention provides a kind of injectable bone tissue engineering bracket material, including：Polylactide-co-glycolide, hydroxyl phosphorus
Lime stone, polyglycollide fibre and organic solvent；
The ratio of the polylactide-co-glycolide, hydroxyapatite and polyglycollide fibre gross mass and organic solvent volume
For (5~10) g：(10~50) mL.
It is preferred that, the weight average molecular weight of the polylactide-co-glycolide is 50000~500000.
It is preferred that, the mol ratio of lactide segment and glycolide segment is (50~90) in the polylactide-co-glycolide：
(50~10).
It is preferred that, the hydroxyapatite be hydroapatite particles, the hydroapatite particles a length of 50~
200nm；A width of 10~50nm of the hydroapatite particles.
It is preferred that, the average length of the polyglycollide fibre is 10~1000 μm；The polyglycollide fibre is averaged
A diameter of 1~100 μm.
It is preferred that, the organic solvent includes METHYLPYRROLIDONE, dimethyl sulfoxide (DMSO), tetraethylene glycol and ethyl acetate
In one or more.
It is preferred that, the mass ratio of the polylactide-co-glycolide and hydroxyapatite is 1：(5~15)；Described poly- third hands over
The ratio of ester-glycolide and hydroxyapatite gross mass and organic solvent volume is 1g：(1~10) mL；The polylactide-second is handed over
The mass ratio (1~9) of ester and hydroxyapatite total amount and polyglycollide fibre：(9~1).
The invention provides a kind of preparation method of injectable bone tissue engineering bracket material described in above-mentioned technical proposal, bag
Include following steps：
A), polylactide-co-glycolide, hydroxyapatite, polyglycollide fibre and organic solvent are mixed, and obtain noting
Penetrate bone tissue engineering stent material.
It is preferred that, the step a) is specifically included：
A1 after), hydroxyapatite and organic solvent are mixed, then mix with polylactide-co-glycolide, mixed
Liquid；
A2), the mixed liquor is mixed with polyglycollide fibre, obtains injectable bone tissue engineering bracket material.
Compared with prior art, the invention provides a kind of fibre-reinforced Injectable in-situ solidification and the bone tissue of pore-forming
Engineering scaffold material and preparation method thereof.The injectable bone tissue engineering bracket material that the present invention is provided includes：Polylactide-second
Lactide, hydroxyapatite, polyglycollide fibre and organic solvent；The polylactide-co-glycolide, hydroxyapatite and poly- second are handed over
The ratio of ester fiber gross mass and organic solvent volume is (5~10) g：(10~50) mL.The present invention with polylactide-co-glycolide,
Hydroxyapatite and polyglycollide fibre have been obviously improved injection as the solute component of injectable bone tissue engineering bracket material
Mechanical strength after agent solidification.Test result indicates that, the injectable bone tissue engineering bracket material curing molding that the present invention is provided
Compression strength >=15MPa afterwards, modulus of elasticity >=15MPa.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
The embodiment of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can also basis
The accompanying drawing of offer obtains other accompanying drawings.
Fig. 1 is the PGA single scanning electron microscope (SEM) photographs that the embodiment of the present invention 1 is provided；
Fig. 2 is the PGA chopped fiber scanning electron microscope (SEM) photographs that the embodiment of the present invention 1 is provided；
Fig. 3 is the bone tissue engineering scaffold scanning electron microscope (SEM) photograph that the embodiment of the present invention 1 is provided；
Fig. 4 is the compression strength block diagram that the embodiment of the present invention 4 is provided；
Fig. 5 is the modulus of elasticity block diagram that the embodiment of the present invention 4 is provided.
Embodiment
The technical scheme in the embodiment of the present invention is clearly and completely described below, it is clear that described embodiment
Only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area
The every other embodiment that art personnel are obtained under the premise of creative work is not made, belongs to the model that the present invention is protected
Enclose.
The invention provides a kind of injectable bone tissue engineering bracket material, including：Polylactide-co-glycolide, hydroxyl phosphorus
Lime stone, polyglycollide fibre and organic solvent；
The ratio of the polylactide-co-glycolide, hydroxyapatite and polyglycollide fibre gross mass and organic solvent volume
For (5~10) g：(10~50) mL.
The injectable bone tissue engineering bracket material that the present invention is provided includes polylactide-co-glycolide, hydroxyapatite, gathered
Glycolide fiber and organic solvent.Wherein, the polylactide-co-glycolide is also known as Poly(D,L-lactide-co-glycolide, English letter
Referred to as PLGA.The weight average molecular weight (Mw) of the polylactide-co-glycolide is not particularly limited the present invention, may be selected but does not limit
In 50000~500000, specifically may be selected to be 100000,150000,200000,250000,300000,350000,400000,
450000 or 500000.The present invention is to lactide segment (english abbreviation LA) in the polylactide-co-glycolide and glycolide chain
The mol ratio of section (english abbreviation GA) is not particularly limited, and may be selected but is not limited to (50~90)：(50~10), it is specific to may be selected
For (60~80)：(40~20) or 70：30.
In the present invention, the hydroxyapatite abbreviation HA, it is the main inorganic composition of bone and tooth.In the present invention
In one embodiment of offer, the hydroxyapatite is hydroapatite particles.The present invention is to the hydroapatite particles
Length be not particularly limited, may be selected but be not limited to 50~200nm, specifically may be selected 60nm, 70nm, 80nm, 90nm,
100nm, 110nm, 120nm, 130nm, 140nm, 150nm, 160nm, 170nm, 180nm or 190nm.The present invention is to the hydroxyl
The width of apatite particle is not particularly limited, may be selected but be not limited to 10~50nm, specifically may be selected 15nm, 20nm, 25nm,
30nm, 35nm, 40nm or 45nm.
In the present invention, the polyglycollide fibre abbreviation PGA fibers.Length of the present invention to the polyglycollide fibre
It is not particularly limited, the average length of the polyglycollide fibre may be selected but be not limited to 10~1000 μm, specifically optional 50 μ
m、60μm、70μm、80μm、90μm、95μm、100μm、105μm、110μm、115μm、120μm、130μm、140μm、150μm、
160μm、170μm、180μm、190μm、200μm、210μm、220μm、230μm、240μm、250μm、300μm、350μm、400μ
M, 450 μm, 500 μm, 550 μm, 600 μm, 650 μm, 700 μm, 750 μm, 800 μm, 850 μm, 900 μm or 950 μm.The present invention is right
The width of the polyglycollide fibre is not particularly limited, and the mean breadth of the polyglycollide fibre may be selected but be not limited to 1
~100 μm, specific optional 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, 5.5 μm, 6 μm, 6.5 μm, 7 μm, 7.5 μm, 8 μm, 8.5 μm, 9 μ
m、9.5μm、10μm、10.5μm、11μm、11.5μm、12μm、12.5μm、13μm、13.5μm、14μm、14.5μm、15μm、15.5
μm、16μm、16.5μm、17μm、17.5μm、18μm、18.5μm、19μm、19.5μm、20μm、21μm、22μm、23μm、24μm、
25μm、26μm、27μm、28μm、29μm、30μm、35μm、40μm、45μm、50μm、55μm、60μm、65μm、70μm、75μm、80
μm, 85 μm, 90 μm or 95 μm.In one embodiment for providing of the present invention, the polyglycollide fibre length it is minimum-greatly
It is worth for 9.64~694.42 μm, quartile (Q1~Q3) is 46.18~131.85 μm, and median is 76.36 μm, and average value is
103.16 μm, standard deviation is 92.41 μm.In one embodiment that the present invention is provided, the pole of the polyglycollide fibre diameter
Minimum-maximum property is 0.07~191.11 μm, and quartile (Q1~Q3) is 6.13~12.56 μm, and median is 9.48 μm, average
It is worth for 12.69 μm, standard deviation is 18.85 μm.The source of the polyglycollide fibre is not particularly limited the present invention, preferably adopts
Prepare using the following method：
I), PGA raw material carries out melt spinning, obtains polyglycollide fibre line；
II), the polyglycollide fibre line carries out mechanical breaking, obtains polyglycollide fibre.
The present invention provide it is above-mentioned prepare the mode of polyglycollide fibre, the PGA raw material is preferably poly- second
Lactide particles material.The melt spinning is carried out in melt spinning machine, and the spinning disc rotating speed of the melt spinning machine is preferably 500
It is~2000 revs/min, specific to may be selected 1000 revs/min；The spinning disc temperature of the melt spinning machine is preferably 200~300 DEG C, tool
Body may be selected to be 250 DEG C.In the present invention, the PGA raw material is preferably being dried before melt spinning is carried out
Processing, to remove moisture contained in PGA raw material.The temperature of the drying is limited to 40~70 DEG C, specifically may be selected 50
DEG C or 60 DEG C；The time of the drying is preferably 0.5~5h, and 1h, 2h or 3h specifically may be selected.
In the present invention, the organic solvent is organic solvent that can be miscible with water, including but not limited to N- methyl -2- pyrroles
One or more in pyrrolidone, dimethyl sulfoxide (DMSO), tetraethylene glycol and ethyl acetate.
In the present invention, the polylactide-co-glycolide, hydroxyapatite and polyglycollide fibre gross mass with it is organic molten
The ratio of agent volume is (5~10) g：(10~50) mL, preferably 10g：(12~30) mL, specifically may be selected to be 10g：20mL or
10g：28mL.In one embodiment that the present invention is provided, the mass ratio of the polylactide-co-glycolide and hydroxyapatite is
1：(5~15), are specifically chosen as 1：6、1：7、1：8、1：9、1：10、1：11、1：12、1：13 or 1：14.There is provided in the present invention
In one embodiment, the ratio of polylactide-co-glycolide and the hydroxyapatite gross mass and organic solvent volume is 1g：(1~
10) mL, is specifically chosen as 1g：2mL、1g：3mL、1g：4mL、1g：5mL、1g：6mL、1g：7mL、1g：8mL or 1g：9mL.At this
Invent in the one embodiment provided, the matter of polylactide-co-glycolide and the hydroxyapatite total amount and polyglycollide fibre
Amount is than (1~9)：(9~1), be preferably (2~8)：(8~2), more preferably (3~7)：(7~3), specifically may be selected to be 4：6、
5：5 or 6：4.
The present invention is used as injectable bone organizational project using polylactide-co-glycolide, hydroxyapatite and polyglycollide fibre
The solute component of timbering material, has been obviously improved the mechanical property after injection solidification.Test result indicates that, what the present invention was provided
Compression strength >=15MPa after injectable bone tissue engineering bracket material curing molding, modulus of elasticity >=15MPa.
The invention provides a kind of preparation method of injectable bone tissue engineering bracket material described in above-mentioned technical proposal, bag
Include following steps：
A), polylactide-co-glycolide, hydroxyapatite, polyglycollide fibre and organic solvent are mixed, and obtain noting
Penetrate bone tissue engineering stent material.
It is directly that polylactide-co-glycolide, hydroxyapatite, PGA is fine in the preparation method that the present invention is provided
Peacekeeping organic solvent is well mixed, you can obtain injectable bone tissue engineering bracket material.The process is specifically included：
A1 after), hydroxyapatite and organic solvent are mixed, then mix with polylactide-co-glycolide, mixed
Liquid；
A2), the mixed liquor is mixed with polyglycollide fibre, obtains injectable bone tissue engineering bracket material.
In the above-mentioned preparation method that the present invention is provided, hydroxyapatite and organic solvent are mixed first.Wherein,
The mode of the mixing is preferably ultrasonic mixing, and the ultrasonic frequency is preferably 20~60KHz, specifically may be selected to be 40KHz；
The time of the mixing is preferably 10min~2h, specifically may be selected to be 20min, 30min, 40min, 1h or 1.5h.Mixing is finished
Afterwards, suspension is obtained.
Obtain after the suspension, the suspension and polylactide-co-glycolide are mixed.Wherein, the suspension and
The mode that polylactide-co-glycolide is mixed preferably mechanical agitation；The mixing temperature is preferably 60~80 DEG C, specifically may be used
For 70 DEG C.After polylactide-co-glycolide is completely dissolved in suspension, mixing is finished, and obtains mixed liquor.
Obtain after mixed liquor, the mixed liquor is mixed with polyglycollide fibre.Wherein, the polyglycollide fibre is next
Source hereinbefore by the agency of, will not be repeated here.In the present invention, the mixed liquor is mixed with polyglycollide fibre
Mode preferably first carries out mechanical agitation, is emulsified again after stirring.The mixture during mechanical agitation in the present invention
The temperature of system is preferably controlled in 60~80 DEG C, specifically can be controlled in 70 DEG C；The time of the emulsification is preferably 3~5min；It is described
The emulsifier rotating speed of emulsification is preferably 5000~10000rpm, specifically may be selected to be 8000rpm.Mixed liquor and polyglycollide fibre
After well mixed, the injectable bone tissue engineering bracket material that the present invention is provided is obtained.
The present invention is used as injectable bone organizational project using polylactide-co-glycolide, hydroxyapatite and polyglycollide fibre
The solute component of timbering material, has been obviously improved the mechanical property after the injection solidification being made.Test result indicates that, using this
Compression strength >=15MPa after the injectable bone tissue engineering bracket material curing molding that the method that invention is provided is made, elasticity
Modulus >=15MPa.
The invention provides a kind of bone tissue engineering scaffold, as the injectable bone organizational project branch described in above-mentioned technical proposal
Formed after frame material solidification.
In the present invention, it is organic molten in injection after the injectable bone tissue engineering bracket material is expelled in water
Agent is replaced rapidly by water, and the high molecular polymer in injection gradually solidifies during above-mentioned displacement, after the curing be complete,
Form bone tissue engineering scaffold.
In one embodiment that the present invention is provided, the injectable bone tissue engineering bracket material is expelled in tissue
Afterwards, the organic solvent in injection is replaced rapidly by the water in tissue, and the high molecular polymer in injection is in above-mentioned displacement
During gradually solidify, after the curing be complete, formed bone tissue engineering scaffold.
It is fine that the bone tissue engineering scaffold that the present invention is provided includes polylactide-co-glycolide, hydroxyapatite and PGA
Dimension, with excellent mechanical property.Test result indicates that, the present invention provide bone tissue engineering scaffold compression strength >=
15MPa, modulus of elasticity >=15MPa.
For the sake of becoming apparent from, it is described in detail below by following examples.
Embodiment 1
1) PLGA/HA solution, is prepared：1g HA particles (being about 100nm, wide about 20nm) are added to 40mL nmp solvents
In, ultrasonic (supersonic frequency after fully stirring evenly：40KHz) 30min, 9g PLGA (LA are added into suspension:GA=80:20 (rub
You compare), Mw=200000), 70 DEG C of stirring in water bath are placed in, are completely dissolved to PLGA.
2) PGA fibers, are prepared：50 DEG C of drying 2h of PGA particles, then add the PGA particles of drying to melt spinning machine
Rotating metallic disk in, and pass through temperature measurer measure rotating metallic disk temperature.When metal dish is heated to 250 DEG C, this is kept
Temperature obtains the liquid PGA of melting for 5 minutes.The rotating speed for adjusting metal dish is 1000 revs/min, and the PGA materials of thawing are because of centrifugal force
Effect sprayed from the hole on the metal dish side of rotation, to form continuous PGA singles because ambient temperature declines, and turned
Speed is received by 100 revs/min of peripheral collector unit.
3), by PGA fibers by pulverizer mechanical breaking, the PGA chopped fibers crushed are obtained, by PGA chopped fibers according to
PGA:(PLGA+HA)=3:7 mass ratio is added in PLGA/HA solution, after 70 DEG C of stirring in water bath are uniform, emulsifier emulsification 3
~5min (emulsifier rotating speed 8000rpm), obtains injectable bone tissue engineering bracket material.
To step 2) obtain PGA singles be scanned electron microscopic observation, as a result as shown in Figure 1.Fig. 1 is implementation of the present invention
The PGA single scanning electron microscope (SEM) photographs that example 1 is provided.
To step 3) obtain PGA chopped fibers be scanned electron microscopic observation, as a result as shown in Figure 2.Fig. 2 is implementation of the present invention
The PGA chopped fiber scanning electron microscope (SEM) photographs that example 1 is provided.
500 PGA chopped fibers are measured on scanning electron microscope (SEM) photograph with Image J softwares, as a result as shown in table 1：
The PGA chopped fiber Size Distribution tables of table 1
It can be seen from Table 1 that, the length average value for the PGA chopped fibers that the present embodiment is produced is 103.16 μm, and diameter is put down
Average is 12.69 μm.
By step 3) obtain injectable bone tissue engineering bracket material be expelled in water, curing molding obtains bone tissue
Engineering rack, is scanned electron microscopic observation, as a result as shown in Figure 3 to the bone tissue engineering scaffold.Fig. 3 is the embodiment of the present invention 1
The bone tissue engineering scaffold scanning electron microscope (SEM) photograph of offer.
Embodiment 2
1) PLGA/HA solution, is prepared：1g HA particles (being about 100nm, wide about 20nm) are added to 40mL nmp solvents
In, ultrasonic (supersonic frequency after fully stirring evenly：40KHz) 30min, 9g PLGA (LA are added into suspension:GA=80:20 (rub
You compare), Mw=200000), 70 DEG C of stirring in water bath are placed in, are completely dissolved to PLGA.
2) PGA fibers, are prepared：50 DEG C of drying 2h of PGA particles, then add the PGA particles of drying to melt spinning machine
Rotating metallic disk in, and pass through temperature measurer measure rotating metallic disk temperature.When metal dish is heated to 250 DEG C, this is kept
Temperature obtains the liquid PGA of melting for 5 minutes.The rotating speed for adjusting metal dish is 1000 revs/min, and the PGA materials of thawing are because of centrifugal force
Effect sprayed from the hole on the metal dish side of rotation, to form continuous PGA singles because ambient temperature declines, and turned
Speed is received by 100 revs/min of peripheral collector unit.
3), by PGA fibers by pulverizer mechanical breaking, the PGA chopped fibers crushed are obtained, by PGA chopped fibers according to
PGA:(PLGA+HA)=5:5 mass ratio is added in PLGA/HA solution, after 70 DEG C of stirring in water bath are uniform, emulsifier emulsification 3
~5min (emulsifier rotating speed 8000rpm), obtains injectable bone tissue engineering bracket material.
Embodiment 3
1) PLGA/HA solution, is prepared：1g HA particles (being about 100nm, wide about 20nm) are added to 40mL nmp solvents
In, ultrasonic (supersonic frequency after fully stirring evenly：40KHz) 30min, 9g PLGA (LA are added into suspension:GA=80:20 (rub
You compare), Mw=200000), 70 DEG C of stirring in water bath are placed in, are completely dissolved to PLGA.
2) PGA fibers, are prepared：50 DEG C of drying 2h of PGA particles, then add the PGA particles of drying to melt spinning machine
Rotating metallic disk in, and pass through temperature measurer measure rotating metallic disk temperature.When metal dish is heated to 250 DEG C, this is kept
Temperature obtains the liquid PGA of melting for 5 minutes.The rotating speed for adjusting metal dish is 1000 revs/min, and the PGA materials of thawing are because of centrifugal force
Effect sprayed from the hole on the metal dish side of rotation, to form continuous PGA singles because ambient temperature declines, and turned
Speed is received by 100 revs/min of peripheral collector unit.
3), by PGA fibers by pulverizer mechanical breaking, the PGA chopped fibers crushed are obtained, by PGA chopped fibers according to
PGA:(PLGA+HA)=7:3 mass ratio is added in PLGA/HA solution, after 70 DEG C of stirring in water bath are uniform, emulsifier emulsification 3
~5min (emulsifier rotating speed 8000rpm), obtains injectable bone tissue engineering bracket material.
Comparative example
1) PLGA/HA solution, is prepared：1g HA particles (being about 100nm, wide about 20nm) are added to 40mL nmp solvents
In, ultrasonic (supersonic frequency after fully stirring evenly：40KHz) 30min, 9g PLGA (LA are added into suspension:GA=80:20 (rub
You compare), Mw=200000), 70 DEG C of stirring in water bath are placed in, are completely dissolved to PLGA, injectable bone tissue engineering bracket material is obtained
Material.
Embodiment 4
Mechanics Performance Testing
Injectable bone tissue engineering bracket material made from embodiment 1~3 and comparative example is expelled in water, in injection
Organic solvent replaced by water rapidly, the high molecular polymer in injection gradually solidifies during above-mentioned displacement, has treated
After all solidstate, bone tissue engineering scaffold is formed.Wherein, the bone tissue engineering scaffold of comparative example formation is marked as 1, embodiment 1~3
The bone tissue engineering scaffold of formation is successively marked as 2~4.
With electronic type universal testing machine (Britain of Instron 1121), in the environment of room temperature (20 DEG C) and 47% humidity,
Establishing criteria GB/T 1041-1992, test the compression strength and modulus of elasticity of bone tissue engineering scaffold 1,2,3 and 4 respectively, plus
Load speed is 2mm/min, shown in result figure 4 and Fig. 5.Fig. 4 is the compression strength block diagram that the embodiment of the present invention 4 is provided, and Fig. 5 is
The modulus of elasticity block diagram that the embodiment of the present invention 4 is provided.In Fig. 4, the corresponding concrete numerical value of 4 post bars is respectively 7.81 ±
0.25,15.20±1.04,22.14±1.44,30.92±2.16MPa；In Fig. 5, the corresponding concrete numerical value of 4 post bars is respectively
10.05±3.61,15.30±2.72,27.35±2.37,69.62±8.98MPa.This hair can be seen that by Fig. 4 and Fig. 5
The excellent in mechanical performance for the bone tissue engineering scaffold that bright embodiment is provided, its compression strength >=15MPa, modulus of elasticity >=15MPa.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of injectable bone tissue engineering bracket material, including：Polylactide-co-glycolide, hydroxyapatite, PGA are fine
Peacekeeping organic solvent；
The ratio of the polylactide-co-glycolide, hydroxyapatite and polyglycollide fibre gross mass and organic solvent volume is (5
~10) g：(10~50) mL.
2. injectable bone tissue engineering bracket material according to claim 1, it is characterised in that the polylactide-second
The weight average molecular weight of lactide is 50000~500000.
3. injectable bone tissue engineering bracket material according to claim 1, it is characterised in that the polylactide-second
The mol ratio of lactide segment and glycolide segment is (50~90) in lactide：(50~10).
4. injectable bone tissue engineering bracket material according to claim 1, it is characterised in that the hydroxyapatite is
Hydroapatite particles, a length of 50~200nm of the hydroapatite particles；A width of the 10 of the hydroapatite particles~
50nm。
5. injectable bone tissue engineering bracket material according to claim 1, it is characterised in that the polyglycollide fibre
Average length be 10~1000 μm；The average diameter of the polyglycollide fibre is 1~100 μm.
6. injectable bone tissue engineering bracket material according to claim 1, it is characterised in that the organic solvent includes
One or more in METHYLPYRROLIDONE, dimethyl sulfoxide (DMSO), tetraethylene glycol and ethyl acetate.
7. the injectable bone tissue engineering bracket material according to any one of claim 1~6, it is characterised in that described poly-
The mass ratio of lactide coglycolide and hydroxyapatite is 1：(5~15)；The polylactide-co-glycolide and hydroxyapatite
The ratio of gross mass and organic solvent volume is 1g：(1~10) mL；Polylactide-co-glycolide and the hydroxyapatite total amount with
The mass ratio (1~9) of polyglycollide fibre：(9~1).
8. the preparation method of injectable bone tissue engineering bracket material, comprises the following steps described in a kind of claim 1：
A), polylactide-co-glycolide, hydroxyapatite, polyglycollide fibre and organic solvent are mixed, and obtain injectable bone
Tissue engineering bracket material.
9. preparation method according to claim 8, it is characterised in that the step a) is specifically included：
A1 after), hydroxyapatite and organic solvent are mixed, then mix with polylactide-co-glycolide, obtain mixed liquor；
A2), the mixed liquor is mixed with polyglycollide fibre, obtains injectable bone tissue engineering bracket material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710303911.5A CN107050506A (en) | 2017-05-03 | 2017-05-03 | A kind of bone tissue engineering stent material of fibre-reinforced Injectable in-situ solidification and pore-forming and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710303911.5A CN107050506A (en) | 2017-05-03 | 2017-05-03 | A kind of bone tissue engineering stent material of fibre-reinforced Injectable in-situ solidification and pore-forming and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107050506A true CN107050506A (en) | 2017-08-18 |
Family
ID=59597700
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710303911.5A Pending CN107050506A (en) | 2017-05-03 | 2017-05-03 | A kind of bone tissue engineering stent material of fibre-reinforced Injectable in-situ solidification and pore-forming and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107050506A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1986007250A1 (en) * | 1985-06-14 | 1986-12-18 | Materials Consultants Oy | Surgical device for immobilization of bone fracture |
| CN101209355A (en) * | 2007-12-25 | 2008-07-02 | 暨南大学 | Preparation of material for bone plate, bone peg and bone block |
| CN101716372A (en) * | 2009-12-30 | 2010-06-02 | 中国科学院长春应用化学研究所 | Method for preparing tissue engineering scaffold by pore forming of directional soluble fibres |
| CN102164563A (en) * | 2008-07-25 | 2011-08-24 | 史密夫和内修有限公司 | Fracture fixation systems |
| CN103211671A (en) * | 2013-02-01 | 2013-07-24 | 东华大学 | Textile multicomponent enhancement structure-gradually degradable ureteral stent tube and preparation method thereof |
| CN104189954A (en) * | 2014-09-19 | 2014-12-10 | 中国科学院长春应用化学研究所 | In-situ tissue solidification engineering scaffold and preparation method thereof |
-
2017
- 2017-05-03 CN CN201710303911.5A patent/CN107050506A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1986007250A1 (en) * | 1985-06-14 | 1986-12-18 | Materials Consultants Oy | Surgical device for immobilization of bone fracture |
| CN101209355A (en) * | 2007-12-25 | 2008-07-02 | 暨南大学 | Preparation of material for bone plate, bone peg and bone block |
| CN102164563A (en) * | 2008-07-25 | 2011-08-24 | 史密夫和内修有限公司 | Fracture fixation systems |
| CN101716372A (en) * | 2009-12-30 | 2010-06-02 | 中国科学院长春应用化学研究所 | Method for preparing tissue engineering scaffold by pore forming of directional soluble fibres |
| CN103211671A (en) * | 2013-02-01 | 2013-07-24 | 东华大学 | Textile multicomponent enhancement structure-gradually degradable ureteral stent tube and preparation method thereof |
| CN104189954A (en) * | 2014-09-19 | 2014-12-10 | 中国科学院长春应用化学研究所 | In-situ tissue solidification engineering scaffold and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| FEVEN MATTEWS MICHAEL等: "Effect of nanofillers on the physico-mechanical properties of load bearing bone implants", 《MATERIALS SCIENCE AND ENGINEERING C》 * |
| 刘颖等: "《工程材料及成形技术基础》", 31 July 2009 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1103320C (en) | Dissolvable oxides for biological applications | |
| Wu et al. | Composite fibrous membranes of PLGA and chitosan prepared by coelectrospinning and coaxial electrospinning | |
| Ishii et al. | In vivo tissue response and degradation behavior of PLLA and stereocomplexed PLA nanofibers | |
| CN105885436B (en) | A kind of bio-ink material for 3D printing and its preparation method and application | |
| US7981945B2 (en) | Antimicrobial, radiopaque, microfiber-reinforced, polymeric methacrylate bone cement | |
| CN107303397B (en) | A kind of biologically active Injectable compound bone cement and its preparation method and application | |
| CN106456823A (en) | Medical product and method for the production thereof | |
| KR20140084042A (en) | Microneedle deposition technique | |
| CN112999426A (en) | Chitosan/polycaprolactone composite microsphere gel | |
| JP7047058B2 (en) | Method for producing biodegradable polymer fine particles and biodegradable polymer fine particles produced thereby | |
| CN103083735A (en) | Composite membrane for guiding bone tissue regeneration and preparation method thereof | |
| KR101531091B1 (en) | Injectable agent for tissue repair treatment comprising the substance polymerizing hydrophobic biocompatible polymer and hydrophilic biocompatible polymer | |
| CN106729985A (en) | A kind of long-acting promoting healing artificial skin and preparation method thereof | |
| JP2805086B2 (en) | Filler for living tissue | |
| KR20220023951A (en) | Aripiprazole sustained-release microspheres and method for preparing the same | |
| CN108273131A (en) | A kind of composite bone cement, preparation method and applications and a kind of bone renovating material | |
| CN108653794A (en) | A kind of preparation method of based composite dressing for medical use | |
| CN107050506A (en) | A kind of bone tissue engineering stent material of fibre-reinforced Injectable in-situ solidification and pore-forming and preparation method thereof | |
| CN105079885A (en) | Injectable PLGA (poly(lactic-co-glycolic acid)) porous composite microsphere preparation embedded with BMP-2 and TGF-beta1 containing microspheres as well as preparation method and application of composite microsphere preparation | |
| CN107096067A (en) | A kind of tissue engineering bracket material of fiber reinforcement in-situ solidifying pore-forming and preparation method thereof | |
| CN109010922A (en) | Bone Defect Repari nano fibrous membrane and preparation method thereof | |
| CN112169019B (en) | Direct-writing forming 3D printing biological ink and preparation method thereof | |
| CN103432570B (en) | A kind of thymalfasin sustained-release micro-spheres and preparation method thereof | |
| CN112494728A (en) | Microsphere-based stent and preparation method and application thereof | |
| CN113440650B (en) | Method for preparing injectable hydrogel through gel crumbling recombination |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170818 |