CN107224606B - Preparation method of poly-sebacic acid glycerol ester PGS (PGS) -based three-dimensional macroporous scaffold - Google Patents
Preparation method of poly-sebacic acid glycerol ester PGS (PGS) -based three-dimensional macroporous scaffold Download PDFInfo
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- CN107224606B CN107224606B CN201710486636.5A CN201710486636A CN107224606B CN 107224606 B CN107224606 B CN 107224606B CN 201710486636 A CN201710486636 A CN 201710486636A CN 107224606 B CN107224606 B CN 107224606B
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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
- 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
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/12—Nanosized materials, e.g. nanofibres, nanoparticles, nanowires, nanotubes; Nanostructured surfaces
Abstract
The invention relates to a preparation method of a poly-sebacic acid glycerol ester PGS (poly-propylene glycol ether) based material three-dimensional macroporous scaffold, which comprises the following steps: dissolving a PGS (polytrimethylene sebacate) base material and polylactic acid PLLA (polylactic acid) in a solvent in a mixing manner, preparing a mixed solution at 50-60 ℃, then pouring the mixed solution into a mold, replacing the solvent after freezing, and carrying out freeze drying to obtain the nanofiber structure scaffold; and then placing the mixture in a vacuum drying oven for 24-96 hours at the temperature of 180-200 ℃ and the air pressure of 100Pa to obtain the composite material. The preparation method is simple, and the obtained PGS-based material macroporous scaffold can be prepared into various three-dimensional shapes according to requirements so as to meet various requirements.
Description
Technical Field
The invention belongs to the field of preparation of tissue engineering scaffolds, and particularly relates to a preparation method of a poly (glycerol sebacate) (PGS) -based three-dimensional macroporous scaffold.
Background
The poly-sebacic acid glycerol ester (PGS) base material is a thermosetting material, a prepolymer of the poly-sebacic acid glycerol ester (PGS) base material is viscous at room temperature, cannot be directly applied to preparation of a bracket, can be applied to tissue engineering bracket application only by performing thermosetting at high temperature under the oxygen-free low-pressure condition, and has good biocompatibility, biodegradability and elasticity. The preparation of the PGS-based material into a macroporous scaffold with a three-dimensional structure is a difficult point in the current research, because the conventional pore-forming techniques, such as a gas foaming method, a freeze-drying method, and the like, cannot be directly combined with the thermal curing process of the PGS-based material.
The method currently used to prepare PGS-based material macroporous scaffolds is a salt particle porogenic method, which generally involves two implementation techniques. One method is salt crystallization, which is to apply supersaturated salt solution on the surface of a mold and place the mold in a high temperature environment, and as water is lost, salt gradually separates out and crystals grow on the surface of the mold. The disadvantages are that:
(1) in the three-dimensional structure mold, the crystallization density is not uniform, and salt grains are difficult to be fully contacted with each other in a crystallization mode, so that a three-dimensional structure bracket with larger volume is difficult to prepare;
(2) salt crystals are prone to collapse during the process of filling a PGS-based material solution, and the preparation process is difficult to accurately control.
Another method is to fill salt into the mold and then compact the mold to make salt particles contact with each other to achieve the purpose of communicating pore diameters, and has the following disadvantages:
(1) the salt particles are ground, but the uniformity of the particle size cannot be guaranteed;
(2) in the process of filling the complex three-dimensional mold, the density of salt at each part is not uniform due to uneven stress.
In the practical application process, the tissue engineering scaffold is required to be made into various three-dimensional structures, so that the method for preparing the PGS-based material macroporous scaffold with the complex three-dimensional structure is important for exploring the method which is simple and convenient to operate, low in cost and free from negative influence on cells.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a PGS (polytrimethylene sebacate) based material three-dimensional macroporous scaffold, overcoming the defects of the existing preparation technology of the PGS based material three-dimensional macroporous scaffold, and obtaining the preparation method of the PGS based material three-dimensional macroporous scaffold, wherein polylactic acid (PLLA) is used as a pore-forming agent in the technology, so that no negative influence is caused on cells; the PLLA used as the pore-foaming agent can obtain different porosities by the modes of dissolving and dissolving with PGS base materials in different mass ratios, freeze-drying and curing; meanwhile, the technology is simple and convenient to operate.
The invention discloses a preparation method of a poly-sebacic acid glycerol ester PGS (poly-propylene glycol ether) based material three-dimensional macroporous scaffold, which comprises the following steps:
(1) dissolving a PGS (polytrimethylene sebacate) base material and polylactic acid PLLA (polylactic acid) in a solvent in a mixing manner, preparing a mixed solution at 50-60 ℃, then pouring the mixed solution into a mold, replacing the solvent after freezing, and carrying out freeze drying to obtain the nanofiber structure scaffold;
(2) and (3) placing the nano-fiber structure support in a vacuum drying oven with the temperature of 180-200 ℃ and the air pressure of 100Pa for 24-96 h, and melting PLLA while solidifying the PGS-based material to obtain the poly-glycerol sebacate PGS-based material three-dimensional macroporous support.
The PGS-based material of the polytrimethylene sebacate in the step (1) is polytrimethylene sebacate PGS and poly (sebacic acid-
Glycerol-lactic acid-polyethylene glycol-glycerol) ester PGSLP.
The mass ratio of the poly (glycerol sebacate) PGS-based material to the polylactic acid PLLA in the step (1) is 3: 7-7: 3.
The concentration of the mixed solution in the step (1) is 0.1 g/mL.
In the step (1), the solvent is one or two of tetrahydrofuran and 1, 4-dioxane.
The die in the step (1) is a three-dimensional die.
The solvent replacement after freezing in the step (1) is specifically as follows: freezing at the temperature of-20 to-80 ℃ for 4 to 24 hours, and replacing the material with an ice-water mixture
The solvent of (1).
The freeze-drying time in the step (1) is 0.5-2 d.
Advantageous effects
(1) The invention provides a novel preparation strategy of a thermosetting PGS-based material macroporous scaffold, and the method has simple operation steps;
(2) the invention is used for making PGS base material form the polylactic acid (PLLA) of the macroporous structure and does not produce the cytotoxicity, and can strengthen the mechanical strength of the material, have application prospects in the field of tissue engineering;
(3) the PGS-based material macroporous scaffold prepared by the invention can be made into various three-dimensional shapes according to the requirements, thereby being suitable for various requirements.
Drawings
A, B, C in FIG. 1 are SEM pictures of the PGS based material macroporous scaffolds prepared in examples 1, 2 and 3, respectively;
FIG. 2 is the appearance of the PGS-based material and PLLA composite material before curing in step (1) of example 2;
FIG. 3 is a graph of the compressive stress strain of the macroporous scaffolds prepared in example 1, example 2 and example 3;
FIG. 4 is the Young's modulus of the macroporous scaffolds prepared in example 1, example 2 and example 3.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
A preparation method of a three-dimensional macroporous scaffold based on poly-sebacic acid glycerol ester (PGS) comprises the following main steps:
(1) dissolving polytrimethylene sebacate (PGS) and polylactic acid (PLLA) in tetrahydrofuran at a ratio of 3:7(w/w), preparing a solution with a concentration of 10% (w/v) at 60 ℃, pouring the solution into a cylindrical three-dimensional mold with a diameter of 2cm, placing the mold into a three-dimensional mold, freezing the mold at-80 ℃ for 4 hours, replacing the solvent in the material with an ice-water mixture, and then freezing and drying the mold for 2 days to obtain the nanofiber structure scaffold;
(2) and (2) placing the nanofiber structure scaffold prepared in the step (1) in a vacuum drying oven at the temperature of 180 ℃ and the air pressure of 100Pa for 96h, solidifying the PGS-based material and simultaneously melting the PLLA to obtain the PGS macroporous scaffold with a three-dimensional structure, the Young modulus of 7.04 +/-1.37 MPa and the pore diameter of 639.188 +/-196.029 microns.
Example 2
A preparation method of a three-dimensional macroporous scaffold based on poly-sebacic acid glycerol ester (PGS) comprises the following main steps:
(1) dissolving poly (sebacic acid-glycerol-lactic acid-polyethylene glycol-glycerol) ester (PGSLP) and polylactic acid (PLLA) in tetrahydrofuran in a ratio of 5:5(w/w), preparing a solution with the concentration of 10% (w/v) at 60 ℃, pouring the solution into a cylindrical three-dimensional mold with the diameter of 3cm, placing the mold into a three-dimensional mold, freezing the mold at-20 ℃ for 24 hours, replacing the solvent in the material with an ice water mixture, and then freezing and drying the mold for 2 days to obtain the nanofiber structure scaffold;
(2) and (2) placing the nanofiber structure scaffold prepared in the step (1) in a vacuum drying oven at 190 ℃ and 100Pa for 48h, solidifying the PGS-based material and simultaneously melting the PLLA to obtain the PGSLP macroporous scaffold with a three-dimensional structure, the Young modulus of 4.48 +/-1.01 MPa and the pore diameter of 282.529 +/-86.927 microns.
Example 3
A preparation method of a three-dimensional macroporous scaffold based on poly-sebacic acid glycerol ester (PGS) comprises the following main steps:
(1) dissolving poly (sebacic acid-glycerol-lactic acid-polyethylene glycol-glycerol) ester (PGSLP) and polylactic acid (PLLA) in tetrahydrofuran in a ratio of 7:3(w/w), preparing a solution with a concentration of 10% (w/v) at 60 ℃, pouring the solution into a cylindrical three-dimensional mold with a diameter of 4cm, placing the mold into a three-dimensional mold, freezing the mold at-50 ℃ for 12 hours, replacing the solvent in the material with an ice water mixture, and then freezing and drying the mold for 2 days to obtain a nanofiber structure scaffold;
(2) and (2) placing the nanofiber structure scaffold prepared in the step (1) in a vacuum drying oven at the temperature of 200 ℃ and the air pressure of 100Pa for 24h, solidifying the PGS-based material and simultaneously melting the PLLA to obtain the PGSLP macroporous scaffold with a three-dimensional structure, the Young modulus of 2.29 +/-0.26 MPa and the pore diameter of 151.610 +/-52.762 microns.
Claims (7)
1. A preparation method of a three-dimensional macroporous scaffold based on poly (glycerol sebacate) PGS (PGS-PGS) materials comprises the following steps:
(1) dissolving a PGS (polytrimethylene sebacate) base material and polylactic acid PLLA (polylactic acid) in a solvent in a mixing manner, preparing a mixed solution at 50-60 ℃, then pouring the mixed solution into a mold, replacing the solvent after freezing, and carrying out freeze drying to obtain the nanofiber structure scaffold; wherein the base material of the PGS is the PGS;
(2) and (3) placing the nano-fiber structure support in a vacuum drying oven with the temperature of 180-200 ℃ and the air pressure of 100Pa for 24-96 h to obtain the poly-sebacic acid glycerol ester PGS-based material three-dimensional macroporous support.
2. The method for preparing the three-dimensional macroporous scaffold based on the polytrimethylene sebacate PGS (poly propylene glycol sebacate) as claimed in claim 1, wherein the method comprises the following steps: the mass ratio of the poly (glycerol sebacate) PGS-based material to the polylactic acid PLLA in the step (1) is 3: 7-7: 3.
3. The method for preparing the three-dimensional macroporous scaffold based on the polytrimethylene sebacate PGS (poly propylene glycol sebacate) as claimed in claim 1, wherein the method comprises the following steps: the concentration of the mixed solution in the step (1) is 10% (w/v).
4. The method for preparing the three-dimensional macroporous scaffold based on the polytrimethylene sebacate PGS (poly propylene glycol sebacate) as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the solvent is one or two of tetrahydrofuran and 1, 4-dioxane.
5. The method for preparing the three-dimensional macroporous scaffold based on the polytrimethylene sebacate PGS (poly propylene glycol sebacate) as claimed in claim 1, wherein the method comprises the following steps: the die in the step (1) is a three-dimensional die.
6. The method for preparing the three-dimensional macroporous scaffold based on the polytrimethylene sebacate PGS (poly propylene glycol sebacate) as claimed in claim 1, wherein the method comprises the following steps: the solvent replacement after freezing in the step (1) is specifically as follows: and (3) freezing at the temperature of-20 to-80 ℃ for 4 to 24 hours, and replacing the solvent in the material with an ice-water mixture.
7. The method for preparing the three-dimensional macroporous scaffold based on the polytrimethylene sebacate PGS (poly propylene glycol sebacate) as claimed in claim 1, wherein the method comprises the following steps: the freeze-drying time in the step (1) is 0.5-2 d.
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Citations (3)
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|---|---|---|---|---|
| CN102971018A (en) * | 2010-05-11 | 2013-03-13 | 阿勒根公司 | Porogen compositions, methods of making and uses |
| CN103201324A (en) * | 2010-05-10 | 2013-07-10 | 阿勒根公司 | Porous materials, methods of making and uses |
| WO2014100718A1 (en) * | 2012-12-21 | 2014-06-26 | University Of Pittsburgh - Of The Commonwealth System Of Higher Education | Methods of electrospinning and compositions made therefrom |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103201324A (en) * | 2010-05-10 | 2013-07-10 | 阿勒根公司 | Porous materials, methods of making and uses |
| CN102971018A (en) * | 2010-05-11 | 2013-03-13 | 阿勒根公司 | Porogen compositions, methods of making and uses |
| WO2014100718A1 (en) * | 2012-12-21 | 2014-06-26 | University Of Pittsburgh - Of The Commonwealth System Of Higher Education | Methods of electrospinning and compositions made therefrom |
Non-Patent Citations (1)
| Title |
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| 一种生物降解弹性体的合成、表征及其在血管支架上的应用;贾亚听;《中国优秀硕士学位论文全文数据库 医药卫生科技辑》;20170215(第2期);第35页4.2.2,第36页-第37页4.3.1,第42页-43页5.2 * |
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