CN109745581A - A kind of bioactivity glass containing multi-stage porous/poly lactide-glycolide acid compound rest and preparation method thereof - Google Patents
A kind of bioactivity glass containing multi-stage porous/poly lactide-glycolide acid compound rest and preparation method thereof Download PDFInfo
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- CN109745581A CN109745581A CN201811517034.2A CN201811517034A CN109745581A CN 109745581 A CN109745581 A CN 109745581A CN 201811517034 A CN201811517034 A CN 201811517034A CN 109745581 A CN109745581 A CN 109745581A
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Abstract
The invention discloses a kind of bioactivity glass containing multi-stage porous/poly lactide-glycolide acid compound rest and preparation method thereof.Bioactivity glass/poly lactide-glycolide acid (PLGA) compound rest containing multi-stage porous is made by following methods: bioactivity glass, amphene, poly lactide-glycolide acid (PLGA) are sequentially added by a certain percentage to organic solvent 1, in 4- dioxane, ultrasound is stirred and is uniformly dispersed, it is subsequently poured into mold, is freeze-dried after pre-freeze molding.Bracket preparation process is simple, and it is convenient to operate, and quality is stablized；Due to the addition of bioactivity glass, raising mechanical property can be supplemented, with good bioactivity and osteoinductive；In addition the addition of amphene bionical can construct the multistage intercommunicating pore structure similar with nature bone, have a good application prospect in the fields such as bone defect healing and bone tissue engineer.
Description
Technical field
The invention belongs to the preparation fields of bio-medical material, and in particular to a kind of bioactivity glass containing hierarchical porous structure
Glass/poly lactide-glycolide acid (PLGA) compound rest and preparation method thereof.
Background technique
Traditional autologous bone transplanting and allogenic bone transplantation clinically are also commonly used to the treatment of bone defect patient at present,
But since autologous bone transplanting limited source, donor are insufficient, the disadvantages of allogenic bone transplantation is infected there are immunological rejection and disease,
It is difficult to the requirement for meeting sufferer to Bone Defect Repari, therefore the clinical demand to the bone tissue engineering scaffold with repair function is more next
It is stronger, this fast development for also promoting bone repairing support to study, and grind the research and development of bone renovating material as the world
Study carefully hot spot.
The main component of bone tissue is collagen and hydroxyapatite.Based on bionics angle, using with natural bone component phase
As organic and inorganic matter prepare bone renovating material and have become current one of research hotspot.Bioactivity glass is as typical
Inorganic non-metallic biomedical material has good biocompatibility, bone guided and osteoinductive, has in Bone Defect Repari field
It is widely used.Poly lactide-glycolide acid (PLGA) is by two kinds of monomers --- and lactic acid and hydroxyacetic acid polymerize at random
Made of linear polymer, be a kind of degradable functional polymer organic compound, there is good biocompatibility, nothing
The performance of malicious, good encystation and film forming is widely used in pharmacy, medical engineering material and modernization industry field.Meanwhile
PLGA is authenticated by U.S. FDA, formally pharmaceutic adjuvant is used as to include into United States Pharmacopeia.Bioactivity glass/polylactic acid-glycolic
Acetic acid copolymer (PLGA) composite material is similar with people's bone tissue in composition, and has good biocompatibility and induction
The biological characteristics such as osteogenic action meet the requirement of bone renovating material to a certain extent.
In addition, bone has natural hierarchical porous structure, and according to bionics principle, the tissue engineered bone with hierarchical porous structure
Recovery support is more advantageous to the progress of Bone Defect Repari process.The function of bone repairing support be for cell proliferation provide three-dimensional space and
The environment of metabolism, and determine the shapes and sizes of cambium, organ.Ideal cytoskeleton should have mutually first
The three-dimensional porous structure of connection and enough specific surface areas to improve the density of cell inoculation, and are conducive to required nutritional ingredient
Supply and metabolic waste discharge, promote inoculating cell by matrix porosity to surrounding tissue spread, be convenient for blood vessels in tissue
With the generation of nerve.But the technical issues of bone repairing support still remains the building of hierarchical porous structure difficulty at present, and eventually lead to
Body fluid infiltration is ineffective, internal stent cell survival lacks enough nutriments and bone, that blood vessel grows into situation is undesirable
The problems such as.
Amphene, 2,2- dimethyl -3- methylene two ring [2,2,1] heptane, white waxy solid, a kind of effumability object
Matter can be used for the preparation of tissue engineering bracket, by removing it together with solvent, construct pore structure.Bioactivity glass/
Amphene is added in poly lactide-glycolide acid (PLGA) compound rest, forms crystallite in pre-freeze forming process, and
Distillation causes micropore when freeze-drying, and finally in conjunction with the larger pore structure that organic solvent is formed, bionical construct is similar to naturally
The hierarchical porous structure of bone, to promote cell adherence and grow into and promote Bone Defect Repari effect.
The present invention is total using bioactivity glass/poly lactic-co-glycolic acid of the freeze-drying preparation containing hierarchical porous structure
Polymers (PLGA) compound rest.The compound rest has preferable mechanical property, and Si, Ca and P of bioactivity glass release
Ion can effectively facilitate Bone Defect Repari；Meanwhile the removal of amphene and organic solvent forms a few micrometers to hundred microns of connection multistage
Pore structure is conducive to body fluid infiltration, nutriment transport and cell and grows into.The bracket preparation method is simple, and it is convenient to operate, in bone
Tissue repair field has broad application prospects.
Summary of the invention
It is an object of the invention to be directed to defect of the existing bracket in structure, a kind of biology containing hierarchical porous structure is provided
Activity glass/poly lactide-glycolide acid (PLGA) compound rest and preparation method thereof obtains a kind of with good biological
The multi-stage porous recovery support of activity and self-bone grafting ability, bionical natural bony structure and ingredient, promote the reparation and regeneration of bone tissue.
In order to achieve the above objectives, technical scheme is as follows.
A kind of preparation method of the bioactivity glass containing multi-stage porous/poly lactide-glycolide acid compound rest, packet
Include following steps:
(1) bioactive glass powder is added into organic solvent Isosorbide-5-Nitrae-dioxane, ultrasound, magnetic agitation make biological work
Property glass powder is dispersed in organic solvent, obtains suspending liquid A；
(2) amphene is added in step (1) resulting suspending liquid A, magnetic agitation obtains suspension B up to being uniformly dispersed；
(3) poly lactide-glycolide acid is added into the resulting suspension B of step (2), and magnetic agitation is until mixing
Uniformly, mixed solution C is obtained；
(4) mixed solution C obtained by step (3) is poured into Teflon mould plate, is freeze-dried, is contained after pre-freeze molding
The bioactivity glass of multi-stage porous/poly lactide-glycolide acid compound rest.
Preferably, bioactive glass powder used is using the preparation of organic formwork combination sol-gel method in step (1)
Micro-nano spherical bioactive glass powder.
Preferably, concentration of the bioactive glass powder in mixed solution C described in step (1) is 0.01-0.04 g/
mL。
Preferably, ultrasonic disperse 15-30min in step (1), magnetic agitation 15-30 min.
Preferably, the quality of amphene described in step (2) is the 50-300% of poly lactide-glycolide acid quality, excellent
It is selected as 200%.
Preferably, magnetic agitation 15-30 min described in step (2).
Preferably, magnetic agitation 6-8 h described in step (3).
Preferably, concentration of the poly lactide-glycolide acid in mixed solution C described in step (3) is 0.06-
0.10 g/mL。
Preferably, the molding temperature of pre-freeze described in step (4) is -15 ~ -25 DEG C.
Preferably, the pre-freeze molding time described in step (4) is 4-24 h.
Preferably, the temperature of freeze-drying described in step (4) is -55 ~ -75 DEG C.
Preferably, the time of freeze-drying described in step (4) is 2-4 days.
A kind of bioactivity glass/poly lactic-co-glycolic acid containing multi-stage porous as made from above-described preparation method
Copolymer compound rest.
Compared with prior art, the invention has the advantages that and effect:
(1) present invention chooses bioactivity glass and two kinds of materials progress of poly lactide-glycolide acid (PLGA) are compound, obtains
The bracket arrived has good biocompatibility and self-bone grafting ability；And raw material is easy to get, it is moderate；It is prepared by freeze-drying
Porous support, method is easy, and quality is stablized.
(2) present invention chooses specific perforating agent --- and amphene prepares hierarchical porous structure in conjunction with organic solvent, the structure
The progress with metabolic process is grown into conducive to body fluid infiltration, cell.
(3) bioactivity glass/poly lactide-glycolide acid (PLGA) of the invention containing hierarchical porous structure is compound
Bracket can be applied to the fields such as bone tissue reparation and bone tissue engineer.
Detailed description of the invention
Fig. 1 a, Fig. 1 b are respectively porous bioglass/poly lactide-glycolide acid (PLGA) that amphene is not added
500 times of the amplification of compound rest, 2000 times of tungsten filament scanning electron microscope (SEM) photograph.
Fig. 1 c, Fig. 1 d are respectively the bioactivity glass containing the hierarchical porous structure/poly- cream for adding amphene in the embodiment of the present invention 3
500 times of the amplification of acid-co-glycolic acid (PLGA) compound rest, 2000 times of tungsten filament scanning electron microscope (SEM) photograph.
Fig. 2 a, Fig. 2 b are respectively the bioactivity glass containing the hierarchical porous structure/poly- cream for adding amphene in the embodiment of the present invention 3
Acid-co-glycolic acid (PLGA) compound rest and Marrow Mesenchymal Stem Cells (mBMSCs) are co-cultured 1 day and 4 days
Dead colored graph living.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1
A kind of bioactivity glass/poly lactide-glycolide acid (PLGA) compound rest containing hierarchical porous structure, preparation
Method is as follows:
(1) preparation step of bioactive glass powder:
First 40 g lauryl amines (DDA) are added into the mixed solution of 250 mL deionized waters and 800 mL dehydrated alcohols, then are set
The magnetic agitation in 40 °C of water bath with thermostatic control, is completely dissolved to lauryl amine；Added with syringe pump with the speed of 0.5 mL/min
217.34 mL ethyl orthosilicates, in the process since Si network gradually forms, solution becomes cloudy, and becomes milky for this；Again with injection
Pump adds 22.02 mL triethyl phosphates with the speed of 0.5 mL/min；Then 137.47 g calcium nitrate tetrahydrates are dissolved in 200
It in the deionized water of mL, is slowly added in reaction solution, continues to stir 3 h, be aged 24 h at room temperature；Finally by glass colloidal sol from
Gains in depth of comprehension are placed in -20 DEG C of refrigerator and are freeze-dried after 2 h of pre-freeze to white precipitate；It is subsequently placed in 650 °C of Muffle furnace hot
3 h are handled to get the bioactive glass powder of 300-500 nm.
(2) system of bioactivity glass/poly lactide-glycolide acid (PLGA) compound rest containing hierarchical porous structure
Standby step:
0.01 g bioactive glass powder is added in 1 mL Isosorbide-5-Nitrae-dioxane organic solvent, after 15 min of ultrasonic disperse
15 min of magnetic agitation keeps bioactivity glass evenly dispersed in organic solvent, obtains suspending liquid A；0.1 g amphene is added to
In resulting suspending liquid A, 15 min of magnetic agitation is dispersed in amphene in suspension, obtains suspension B；By 0.05 g
Poly lactide-glycolide acid (PLGA) adds in resulting suspension B, and magnetic agitation makes it completely dissolved, and is mixed
Liquid C；Mixed solution C is poured into Teflon mould, is freeze-dried 2 days, obtains at -60 DEG C after -20 DEG C of pre-freeze 4h
Bioactivity glass/poly lactide-glycolide acid (PLGA) compound rest with hierarchical porous structure.
Embodiment 2
A kind of bioactivity glass/poly lactide-glycolide acid (PLGA) compound rest containing hierarchical porous structure, preparation
Method is as follows:
(1) preparation step of bioactive glass powder:
First 4 g lauryl amines (DDA) are added into the mixed solution of 25 mL deionized waters and 80 mL dehydrated alcohols, then are placed in
Magnetic agitation in 40 °C of water bath with thermostatic control, is completely dissolved to lauryl amine；Add 21.73 with syringe pump with the speed of 0.5 mL/min
ML ethyl orthosilicate, in the process since Si network gradually forms, solution becomes cloudy, and becomes milky for this；Again with syringe pump with 0.5
The speed of mL/min adds 2.2 mL triethyl phosphates；Then 13.75 g calcium nitrate tetrahydrates are dissolved in the deionization of 200 mL
It in water, is slowly added in reaction solution, continues to stir 3 h, be aged 24 h at room temperature；Finally it is centrifuged glass colloidal sol to obtain white
Precipitating is placed in -20 DEG C of refrigerator and is freeze-dried after 2 h or more of pre-freeze；It is subsequently placed in 650 °C of Muffle furnace and is heat-treated 3 h；
Up to the bioactive glass powder of 300-500 nm.
(2) system of bioactivity glass/poly lactide-glycolide acid (PLGA) compound rest containing hierarchical porous structure
Standby step:
0.04 g bioactive glass powder is added into 1 mL Isosorbide-5-Nitrae-dioxane organic solvent, 15 min of ultrasonic disperse
15 min of magnetic agitation afterwards keeps bioactivity glass evenly dispersed in organic solvent, obtains suspending liquid A；By 0.18 g amphene
It adds in resulting suspending liquid A, 15 min of magnetic agitation is dispersed in amphene in suspension, obtains suspension B；It will
0.06 g poly lactide-glycolide acid (PLGA) adds in resulting suspension B, and magnetic agitation makes it completely dissolved, and obtains
To mixed liquor C；Mixed solution C is poured into Teflon mould, -20 DEG C of pre-freezes for 24 hours after -60 DEG C be freeze-dried 4
It, obtains bioactivity glass/poly lactide-glycolide acid (PLGA) compound rest with hierarchical porous structure.
Embodiment 3
A kind of bioactivity glass/poly lactide-glycolide acid (PLGA) compound rest containing hierarchical porous structure, preparation
Method is as follows:
(1) preparation step of bioactive glass powder:
First 8 g lauryl amines (DDA) are added into the mixed solution of 50 mL deionized waters and 160 mL dehydrated alcohols, then are placed in
Magnetic agitation in 40 °C of water bath with thermostatic control, is completely dissolved to lauryl amine；Add 43.46 with syringe pump with the speed of 0.5 mL/min
ML ethyl orthosilicate, in the process since Si network gradually forms, solution becomes cloudy, and becomes milky for this；Again with syringe pump with 0.5
The speed of mL/min adds 4.4 mL triethyl phosphates；Then 27.48 g calcium nitrate tetrahydrates are dissolved in the deionization of 200 mL
It in water, is slowly added in reaction solution, continues to stir 3 h, be aged 24 h at room temperature；Finally it is centrifuged glass colloidal sol to obtain white
Precipitating is placed in -20 DEG C of refrigerator and is freeze-dried after 2 h or more of pre-freeze；It is subsequently placed in 650 °C of Muffle furnace and is heat-treated 3
h；Up to the bioactive glass powder of 300-500 nm.
(2) system of bioactivity glass/poly lactide-glycolide acid (PLGA) compound rest containing hierarchical porous structure
Standby step:
0.2 g bioactive glass powder is added into 10 mL Isosorbide-5-Nitraes-dioxane organic solvent, 15 min of ultrasonic disperse
15 min of magnetic agitation afterwards keeps bioactivity glass evenly dispersed in organic solvent, obtains suspending liquid A；0.8 g amphene is added
To in resulting suspending liquid A, 15 min of magnetic agitation is dispersed in amphene in suspension, obtains suspension B；By 0.8 g
Poly lactide-glycolide acid (PLGA) is added into resulting suspension B, and magnetic agitation makes it completely dissolved, and is mixed
Close liquid C；Mixed solution C is poured into Teflon mould, is freeze-dried 3 days, obtains at -60 DEG C after -20 DEG C of pre-freeze 12h
To bioactivity glass/poly lactide-glycolide acid (PLGA) compound rest with hierarchical porous structure.
Bioactivity glass/poly lactide-glycolide acid containing hierarchical porous structure resulting to embodiment 1,2,3
(PLGA) compound rest is characterized, and since the effect picture of embodiment 1,2,3 is similar, it is resulting to only provide embodiment 3
Bioactivity glass/poly lactide-glycolide acid surface sweeping electron microscope (see Fig. 1 c, Fig. 1 d) and work containing hierarchical porous structure
Dead colored graph (see Fig. 2 a and Fig. 2 b).By Fig. 1 a, Fig. 1 b it is found that the bracket that amphene is not added only has porous structure, hole wall is closely knit；
By Fig. 1 c, Fig. 1 d it is found that the resulting bioactivity glass/poly lactide-glycolide acid for adding amphene of embodiment 1,2,3
(PLGA) compound rest not only has good porous connectivity structure, and has the alternatively distributed feature of big aperture, 100 μm of left sides
It is dispersed with 10 μm or so of aperture and 10-100 μm of hole on right macropore hole wall and surrounding, constituting has multi-stage porous
Three-dimensional structure.Cell dead colored graph (Fig. 2 a and Fig. 2 b) living shows that multi-stage porous bracket prepared by embodiment 3 and mBMSCs co-culture 1
It and after 4 days, bracket has good biocompatibility, can promote sticking and being proliferated for cell.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made by without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of the bioactivity glass containing multi-stage porous/poly lactide-glycolide acid compound rest, special
Sign is, includes the following steps:
(1) bioactive glass powder is added into organic solvent Isosorbide-5-Nitrae-dioxane, ultrasound, magnetic agitation make biological work
Property glass powder is dispersed in organic solvent, obtains suspending liquid A；
(2) amphene is added in step (1) resulting suspending liquid A, magnetic agitation obtains suspension B up to being uniformly dispersed；
(3) poly lactide-glycolide acid is added into the resulting suspension B of step (2), and magnetic agitation is until mixing
Uniformly, mixed solution C is obtained；
(4) mixed solution C obtained by step (3) is poured into Teflon mould plate, is freeze-dried, is contained after pre-freeze molding
The bioactivity glass of multi-stage porous/poly lactide-glycolide acid compound rest.
2. preparation method according to claim 1, which is characterized in that bioactive glass powder used is in step (1)
Using the micro-nano spherical bioactive glass powder of organic formwork combination sol-gel method preparation.
3. preparation method according to claim 1, which is characterized in that bioactive glass powder described in step (1) exists
Concentration in mixed solution C is 0.01-0.04 g/mL.
4. preparation method according to claim 1, which is characterized in that the quality of amphene described in step (2) is polylactic acid-
The 50-300% of co-glycolic acid quality.
5. preparation method according to claim 1, which is characterized in that the copolymerization of poly lactic-co-glycolic acid described in step (3)
Concentration of the object in mixed solution C is 0.06-0.10 g/mL.
6. preparation method according to claim 1, which is characterized in that the molding temperature of pre-freeze described in step (4) is -15
~-25℃。
7. preparation method according to claim 1, which is characterized in that the pre-freeze molding time described in step (4) is 4-
24 h。
8. preparation method according to claim 1, which is characterized in that the temperature of freeze-drying described in step (4) is -55
~-75℃。
9. preparation method according to claim 1, which is characterized in that the time of freeze-drying described in step (4) is 2-4
It.
10. a kind of bioactivity glass containing multi-stage porous/poly- cream as made from the described in any item preparation methods of claim 1 ~ 9
Acid-co-glycolic acid compound rest.
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| CN113082297A (en) * | 2021-04-15 | 2021-07-09 | 漯河医学高等专科学校 | Preparation method of superparamagnetic bone repair material |
| CN115006602A (en) * | 2022-06-10 | 2022-09-06 | 杭州昊莱生物科技有限公司 | Bone repair material with high calcium and phosphorus content and application thereof |
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| CN113082297B (en) * | 2021-04-15 | 2022-02-25 | 漯河医学高等专科学校 | Preparation method of superparamagnetic bone repair material |
| CN115006602A (en) * | 2022-06-10 | 2022-09-06 | 杭州昊莱生物科技有限公司 | Bone repair material with high calcium and phosphorus content and application thereof |
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Application publication date: 20190514 |