CN113040982B - Bionic fiber ring stent and preparation method thereof - Google Patents
Bionic fiber ring stent and preparation method thereof Download PDFInfo
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- CN113040982B CN113040982B CN202110237417.XA CN202110237417A CN113040982B CN 113040982 B CN113040982 B CN 113040982B CN 202110237417 A CN202110237417 A CN 202110237417A CN 113040982 B CN113040982 B CN 113040982B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F2/00—Filters implantable into blood vessels; Prostheses, i.e. artificial substitutes or replacements for parts of the body; Appliances for connecting them with the body; Devices providing patency to, or preventing collapsing of, tubular structures of the body, e.g. stents
- A61F2/02—Prostheses implantable into the body
- A61F2/30—Joints
- A61F2/44—Joints for the spine, e.g. vertebrae, spinal discs
- A61F2/442—Intervertebral or spinal discs, e.g. resilient
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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Abstract
The invention discloses a bionic fiber ring scaffold and a preparation method thereof, belonging to the field of biomedical materials. According to the preparation method of the bionic fiber ring bracket, the micro-nano fiber membrane with a three-dimensional structure is obtained by an electrostatic spinning method, then the fiber is induced by a solvent with specific parameters to generate bending deformation with good orientation degree, and finally the fiber membrane is cut and wound according to a specific mode, so that the prepared bionic fiber ring bracket product has an excellent multilayer alternative structure and tensile strain performance, the mechanical property gradient of a human fiber ring is simulated, the defects that the existing simulated fiber ring has poor tensile strain performance and lacks the mechanical gradient change of a natural fiber ring are overcome, and the biocompatibility of the product is improved by the extracellular matrix coated between layers; the preparation method has simple operation steps and lower requirements on equipment, and can realize industrial mass production. The invention also discloses the bionic fiber ring scaffold prepared by the preparation method.
Description
Technical Field
The invention relates to the field of biomedical materials, in particular to a bionic fiber ring scaffold and a preparation method thereof.
Background
Intervertebral disc degeneration is a disease which afflicts most of the elderly and even young people, and the symptom often causes pain in the waist and the back, and seriously affects normal life. The intervertebral disc is located between two vertebral bodies of human spine and mainly consists of central nucleus pulposus, annulus fibrosus and upper and lower cartilage end plates. When the annulus fibrosus is damaged, the outflow of the inner nucleus pulposus compresses the nerves causing pain and the disc highly collapses causing further tissue degeneration. Thus, the key to the treatment of degenerative disc disease is the repair of the annulus fibrosus. Structurally, the fiber loops are of a multi-layer (N ═ 15 to 25) concentric ring structure, the collagen fibers in each layer are aligned at an angle of about 30 degrees along the circumferential direction, and the fiber alignment directions of adjacent layers are alternately opposite. From the aspect of mechanical property, the fibers in the single-sheet layer are in a curled shape on the basis of orientation arrangement, and can absorb more strain on the basis of high mechanical modulus, so that mechanical load is better buffered; additionally, the concentric ring lamellae have a gradient of mechanical properties from the inner (proximal to the nucleus pulposus) to the outer (distal to the nucleus pulposus), with the outer annulus fibrosus being stronger than the inner annulus fibrosus.
At present, the treatment of intervertebral disc degeneration from conservative treatment to surgical treatment can only relieve pain of patients, cannot fundamentally recover the biomechanical function of intervertebral discs, and even can possibly cause further tissue degeneration. In recent years, with the development of medicine, tissue engineering is expected to become a favorable means for intervertebral disc repair. The biomechanical function of the intervertebral disc is closely related to the structure of the intervertebral disc, and the structure of the fibrous ring is fine and is the key point of the construction of a scaffold on tissue engineering.
In the existing published research reports, the materials used for constructing the fibrous ring scaffold for tissue engineering mainly include natural biological materials (such as collagen and silk fibroin) and polymer synthetic materials (such as polylactic acid and polycaprolactone), and the preparation methods of the materials include freeze drying technology, 3D printing technology or electrostatic spinning technology and the like. For example, the Yang et al research group freezes, dries and cross-links PLA electrospun short fibers to obtain a three-dimensional porous scaffold, and the scaffold has the characteristic of high porosity; researchers of the subject groups such as Costa use a 3D printing technology to compositely deposit silk fibroin/elastin in a shape of a fiber ring to obtain a porous fiber ring scaffold. However, monolithic artificial discs like this do not reproduce the precise hierarchical structure of the annulus fibrosus and to some extent lack anisotropic mechanical properties.
The electrostatic spinning technology is a simple and feasible technology for preparing micro-nano fibers, and the materials can be prepared into fibers matched with natural collagen fiber sizes. At present, many scholars select the technology to prepare the bionic scaffold. Researchers in the group of subjects such as Yang electro-spin a mixed material of PCL/PLGA and collagen into a fibrous membrane, and simulate a composite structure of fibrous rings by winding the fibrous membrane layer by layer due to the easy processability of the fibrous membrane. Meanwhile, cells can be planted between layers by utilizing the mode that the electrospun fiber membrane is wound layer by layer, so that the problem of cell growth is solved.
However, despite the many reports on the use of electrospinning to produce artificial annuluses, these scaffolds still do not mimic the structure and properties of natural annuluses well, mainly in terms of: (1) even if the oriented electrospun fiber has high modulus, the oriented electrospun fiber still has a straight fiber form and cannot provide excellent toughness; (2) the annular scaffold has no mechanical gradient change and fails to simulate the mechanical transition of the natural annulus from the softer nucleus to the harder peripheral annulus.
Disclosure of Invention
Based on the defects in the prior art, the invention aims to provide a preparation method of a bionic fiber ring scaffold. The method uses an electrostatic spinning method and subsequent induction to obtain a nanofiber membrane precursor with bending orientation, and the finally prepared bionic fiber ring can effectively simulate the multilevel structure and mechanical gradient performance of the in-vivo fiber ring.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a bionic fiber ring scaffold comprises the following steps:
(1) preparing an electrostatic spinning membrane from the degradable high-molecular base material by an electrostatic spinning method;
(2) fixing and immersing the electrostatic spinning membrane into an organic solution, inducing for 0.1-24 h at 20-60 ℃, taking out, freezing and drying to obtain a bent and oriented electrostatic spinning fiber membrane;
(3) cutting the electrostatic spinning fiber membrane with the bending orientation into electrostatic spinning fiber strips, wherein the long axes of the strips and the fiber orientation in the fiber membrane form a +/-25-35 degree angle during cutting;
(4) winding each electrostatic spinning fiber strip into a composite layer of concentric annular supports, and coating extracellular matrix between layers to obtain the bionic fiber ring support; the orientation direction of the electrostatic spinning fiber strips of the adjacent layers in the bionic fiber ring support is +/-25-35 degrees.
According to the preparation method of the bionic fiber ring support, the micro-nano fiber membrane with a three-dimensional structure is obtained by an electrostatic spinning method, then the fiber is induced by a solvent with specific parameters to generate bending deformation with good orientation degree, and finally the fiber membrane is cut and wound according to a specific mode, so that the prepared bionic fiber ring support product has an excellent multilayer alternative structure and tensile strain performance, the mechanical property gradient of a human fiber ring is simulated, and the extracellular matrix coated between layers also improves good biocompatibility for the product; the preparation method has simple operation steps and lower requirements on equipment, and can realize industrial mass production.
Preferably, the degradable polymer substrate in step (1) comprises at least one of PLLA (levorotatory polylactic acid), PCL (polycaprolactone), PLCL (poly L-lactide-caprolactone) or derivatives thereof.
The polymer base material has good biodegradability and biocompatibility, has no toxicity, and can be well applied to tissue engineering.
Preferably, the speed of the injection pump is 2-3 mL/h when the electrostatic spinning membrane is prepared by the electrostatic spinning method in the step (1), the spinning needle is a 9G stainless steel needle, the positive voltage applied to the needle is 12-18 kV, the negative voltage corresponding to the receiver is 0.5-1 kV, and the distance between the needle and the receiver is 8-10 cm.
Preferably, the temperature of the electrostatic spinning membrane prepared by the electrostatic spinning method in the step (1) is 20-25 ℃, the relative humidity is 60-70%, the time is 1-2 h, and the electrostatic spinning membrane is dried in a vacuum environment for more than 12h after being prepared.
The fiber prepared by the electrostatic spinning method under the condition has uniform size, is in a micro-nano structure, has no adhesion phenomenon, has moderate thickness and excellent three-dimensional structure, and is favorable for inducing a bending orientation fiber film with good orientation degree by a subsequent solvent.
Preferably, the organic solvent in the organic solution in step (2) includes at least one of ethanol, DMF (N, N-dimethylformamide), DCM (dichloromethane), TFEA (2,2, 2-trifluoroethanol), and HFIP (hexafluoroisopropanol), and the volume concentration of the organic solvent in the solution is 10-100%.
The organic solution under the concentration can effectively induce the fibers in the electrostatic spinning fiber membrane to generate uniform bending deformation, and simultaneously, the fibers are prevented from agglomerating, winding and adhering.
Preferably, the temperature for induction in the step (2) is 25-60 ℃, and the time is 20-120 min;
more preferably, the temperature for the induction in the step (2) is 40-60 ℃ and the time is 20-60 min.
Through a plurality of experiments, the inventor finds that the good and uniform bending orientation of each electrostatic spinning after solvent induction can be ensured only under the optimal conditions. If the temperature is too low or the induction time is too short, the bending deformation of the fibers is small and different in degree; however, if the temperature is too high or the induction time is too long, the deformation of the fibers is too large, the deformation of the whole fiber film is too large, the subsequent cutting and winding are not facilitated, and even the tensile strain capacity of the prepared product is weakened finally. In the optimal range, different mechanical properties can be controlled by controlling the induction time and temperature, and the mechanical property gradient design is realized.
Under the preferable condition of solvent induction, the fiber membranes with natural bending orientation with different curling degrees can be prepared according to actual needs and used for preparing three-dimensional bionic scaffolds corresponding to the actual needs.
Preferably, the long axis of the strip is within +/-30 degrees of the fiber orientation in the fiber membrane in the cutting in the step (3); and (4) the orientation direction of the electrostatic spinning fiber strips of the adjacent layers in the bionic fiber ring support is +/-30 degrees.
The fibrous ring bracket prepared by cutting and winding according to the angle can effectively simulate the mechanical property gradient of the native fibrous ring of a human body from the inner layer to the outside, so that the fibrous ring bracket is better used for supporting the intervertebral disc with serious stress on the human body.
The invention also aims to provide the bionic fiber ring scaffold prepared by the preparation method of the bionic fiber ring scaffold.
The bionic fiber ring bracket provided by the invention overcomes the defects that the simulated fiber ring in the existing report can not provide good tensile strain performance and lacks the mechanical gradient change of the natural fiber ring, can well simulate the structure and performance characteristics of the natural fiber ring, has excellent biodegradability and compatibility, and is applied to non-toxicity or rejection reaction in a human body.
The invention has the beneficial effects that the invention provides a preparation method of the bionic fiber ring bracket, the method obtains a micro-nano fiber membrane with a three-dimensional structure by an electrostatic spinning method, then the fiber can be subjected to bending deformation with good orientation degree by solvent induction of specific parameters, and finally the fiber membrane is cut and wound according to a specific mode, so that the prepared bionic fiber ring bracket product has excellent multilayer alternate structure and tensile strain performance, the mechanical property gradient of a human fiber ring is simulated, and the extracellular matrix coated between layers also improves good biocompatibility for the product; the preparation method has simple operation steps and lower requirements on equipment, and can realize industrial mass production. The invention also provides a bionic fiber ring scaffold prepared by the preparation method of the bionic fiber ring scaffold. The product overcomes the defects that the simulated fiber ring can not provide good tensile strain performance and lacks the mechanical gradient change of the natural fiber ring in the existing report, can well simulate the structure and performance characteristics of the natural fiber ring, and has excellent biodegradability and compatibility.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing a bionic fibrous ring scaffold according to the present invention;
FIG. 2 is a schematic view of a fixed mold used in the method for preparing the bionic fiber ring scaffold;
FIG. 3 is a schematic diagram of the fixing process of the electrospun fiber membrane induced by solvent in the preparation method of the bionic fiber ring scaffold;
FIG. 4 is a scanning electron microscope (left) and an enlarged (right) view of the bionic fiber ring stent of the invention;
FIG. 5 is a scanning electron microscope comparison graph (A) and a fiber diameter distribution statistical graph (B) of a bend-oriented electrospun fiber membrane obtained in example 1 and an electrospun fiber membrane obtained in comparative example 1 according to an embodiment of the present invention;
FIG. 6 is a scanning electron microscope comparison graph of electrospun fiber membranes obtained in effect example 2 of the present invention at different solvent induction times (A: no-induced sample in comparative example 1, B: 20min, C: 60min, D: 120 min);
FIG. 7 is a graph of stress-strain curve (left) and tensile strain trend (right) of electrospun fiber membranes obtained at different solvent induction times in Effect example 2 according to the embodiment of the present invention;
fig. 8 is a graph of stress-strain curve (left) and tensile strain trend (right) of the electrospun fiber membrane obtained at different solvent induction temperatures in effect example 2 according to the embodiment of the present invention.
Detailed Description
In order to better illustrate the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to specific examples and comparative examples, which are intended to be understood in detail, but not intended to limit the invention. All other embodiments obtained by a person skilled in the art without making any inventive step are within the scope of protection of the present invention. The experimental reagents and instruments designed for implementing the invention are common reagents and instruments unless otherwise specified.
Example 1
The preparation method of the bionic fibrous ring scaffold comprises the following steps, and the preparation process is shown in fig. 1:
(1) dissolving 0.8g of PLLA in 10mL of trifluoroethanol to prepare 8% polymer spinning precursor solution, and preparing an electrostatic spinning membrane by an electrostatic spinning method; when the electrostatic spinning method is used for preparing an electrostatic spinning film, the speed of an injection pump is 3mL/h, a spinning needle head is a 9G stainless steel needle head, the positive voltage applied to the needle head is 12kV, the negative voltage of a corresponding disc receiver is-1 kV, the rotating speed of the disc receiver is 3000r/min, and the distance between the needle head and the receiver is 10 cm; the temperature is 25 ℃, the relative humidity is 65%, the time is 1.5h, and the electrostatic spinning film is dried for 12h in a vacuum environment after being prepared;
(2) cutting the electrospun film to 1 × 5cm2Is fixed to a jig with both ends of 0.5cm each (actual induction area of the fiber film is 1X 4cm)2Initial length ofL04cm), fixing a clamp on a mold, loosening the fiber membrane until the length of two ends is half of the initial length, soaking the fiber membrane in absolute ethyl alcohol, inducing at 25 ℃ for 20min, taking out the fiber membrane, putting the fiber membrane into a freeze dryer, and fixing and drying the fiber membrane to obtain the electrostatic spinning fiber membrane with bending orientation; the die and the fiber membrane are fixed schematically and are shown in figures 2 and 3;
(3) cutting the electrostatic spinning fiber membrane with the bending orientation into electrostatic spinning fiber strips, wherein the long axes of the strips and the fiber orientation in the fiber membrane form +/-30 degrees during cutting;
(4) winding each electrostatic spinning fiber strip into a composite layer of concentric annular supports, and coating extracellular matrix between layers to obtain the bionic fiber ring support; the orientation direction of the electrostatic spinning fiber strips of the adjacent layers in the bionic fiber ring support is +/-30 degrees.
The bionic fiber ring scaffold obtained in the embodiment was observed under a scanning electron microscope, and the obtained result is shown in fig. 4. As can be clearly seen from the figure, the fiber membranes of the layers in the product are well wound, the distance between the layers is uniform, and the extracellular matrix coating between the layers is good.
Example 2
The preparation method of the bionic fibrous ring scaffold comprises the following steps:
(1) dissolving 0.8g of PCL in 10mL of trifluoroethanol to prepare 8% polymer spinning precursor solution, and preparing an electrostatic spinning film by an electrostatic spinning method; when the electrostatic spinning method is used for preparing an electrostatic spinning film, the speed of an injection pump is 2mL/h, a spinning needle head is a 9G stainless steel needle head, the positive voltage applied to the needle head is 15kV, the negative voltage of a corresponding disc receiver is-1 kV, the rotating speed of the disc receiver is 3000r/min, and the distance between the needle head and the receiver is 8 cm; the temperature is 20 ℃, the relative humidity is 60%, the time is 1h, and the electrostatic spinning membrane is dried for 12h in a vacuum environment after being prepared;
(2) cutting the electrospun film to 1 × 5cm2Is fixed to a jig with both ends of 0.5cm each (actual induction area of the fiber film is 1X 4cm)2Initial length L04cm), the fixture is fixed on the die, and the fiber membrane is loosened to the length of the two ends as the initial lengthImmersing half of the length of the fiber into DMF, inducing at 50 ℃ for 30min, taking out, placing into a freeze dryer, fixing and drying to obtain the electrostatic spinning fiber membrane with bending orientation;
(3) cutting the electrostatic spinning fiber membrane with the bending orientation into electrostatic spinning fiber strips, wherein the long axes of the strips and the fiber orientation in the fiber membrane form +/-30 degrees during cutting;
(4) winding each electrostatic spinning fiber strip into a composite layer of concentric annular supports, and coating extracellular matrix between layers to obtain the bionic fiber ring support; the orientation direction of the electrostatic spinning fiber strips of the adjacent layers in the bionic fiber ring support is +/-30 degrees.
Example 3
The preparation method of the bionic fibrous ring scaffold comprises the following steps:
(1) dissolving 0.8g of PLCL in 10mL of trifluoroethanol to prepare 8% polymer spinning precursor solution, and preparing an electrostatic spinning film by an electrostatic spinning method; when the electrostatic spinning method is used for preparing the electrostatic spinning film, the speed of an injection pump is 2.5mL/h, a 9G stainless steel needle is used as a spinning needle, the positive voltage applied to the needle is 18kV, the negative voltage of a corresponding disc receiver is-1 kV, the rotating speed of the disc receiver is 3000r/min, and the distance between the needle and the receiver is 9 cm; the temperature is 20 ℃, the relative humidity is 70%, the time is 1h, and the electrostatic spinning membrane is dried for 12h in a vacuum environment after being prepared;
(2) cutting the electrospun film to 1 × 5cm2Is fixed to a jig with both ends of 0.5cm each (actual induction area of the fiber film is 1X 4cm)2Initial length L04cm), fixing the fixture on a mold, loosening the fiber membrane until the length of both ends is half of the initial length, immersing in DCM, inducing at 30 ℃ for 100min, taking out, and fixing and drying in a freeze dryer to obtain the electrostatic spinning fiber membrane with bending orientation;
(3) cutting the electrostatic spinning fiber membrane with the bending orientation into electrostatic spinning fiber strips, wherein the long axes of the strips and the fiber orientation in the fiber membrane form +/-30 degrees during cutting;
(4) winding each electrostatic spinning fiber strip into a composite layer of concentric annular supports, and coating extracellular matrix between layers to obtain the bionic fiber ring support; the orientation direction of the electrostatic spinning fiber strips of the adjacent layers in the bionic fiber ring support is +/-30 degrees.
Example 4
The only difference between this example and example 1 is that the induction time in step (2) is 60 min.
Example 5
The difference between this example and example 1 is only that the induction time in step (2) is 120 min.
Example 6
This example differs from example 1 only in that the temperature at the time of induction in step (2) was 30 ℃.
Example 7
This example differs from example 1 only in that the temperature at the time of induction in step (2) was 40 ℃.
Example 8
This example differs from example 1 only in that the temperature at the time of induction in step (2) is 60 ℃.
Comparative example 1
The preparation method of the bionic fibrous ring scaffold comprises the following steps:
(1) dissolving 0.8g of PLLA in 10mL of trifluoroethanol to prepare 8% polymer spinning precursor solution, and preparing an electrostatic spinning membrane by an electrostatic spinning method; when the electrostatic spinning method is used for preparing an electrostatic spinning film, the speed of an injection pump is 3mL/h, a spinning needle head is a 9G stainless steel needle head, the positive voltage applied to the needle head is 12kV, the negative voltage of a corresponding disc receiver is-1 kV, the rotating speed of the disc receiver is 3000r/min, and the distance between the needle head and the receiver is 10 cm; the temperature is 25 ℃, the relative humidity is 65%, the time is 1.5h, and the electrostatic spinning film is dried for 12h in a vacuum environment after being prepared;
(2) cutting the electrostatic spinning fiber membrane into electrostatic spinning fiber strips, wherein the long axis of each strip and the fiber orientation in the fiber membrane form +/-30 degrees during cutting;
(3) winding each electrostatic spinning fiber strip into a composite layer of concentric annular supports, and coating extracellular matrix between layers to obtain the bionic fiber ring support; the orientation direction of the electrostatic spinning fiber strips of the adjacent layers in the bionic fiber ring support is +/-30 degrees.
Effect example 1
To verify the effect of solvent induction on the bending deformation of electrospun fibers, the bending-oriented electrospun fiber film obtained in example 1 and the electrospun fiber film obtained in comparative example 1 were observed under a scanning electron microscope, and the fiber diameters were counted, and the results are shown in fig. 5.
It can be clearly seen from the figure that the electrostatic spinning fiber after being induced by the organic solvent is subjected to regular bending deformation, and although the diameter distribution of the fiber is changed to a certain extent, no obvious uneven size or fiber adhesion occurs, which indicates that the fiber bending induction is successful under the conditions.
Effect example 2
In order to verify the influence of the solvent induction time on the appearance and tensile strain performance of the prepared bionic fiber ring scaffold, the bending-oriented electrospun fiber membranes obtained in examples 1, 4 and 5 and the electrospun fiber membrane obtained in comparative example 1 are observed under a scanning electron microscope, meanwhile, each fiber membrane is prepared into small strips with the same size, is subjected to tensile mechanical property test through a dynamic thermomechanical analyzer (DMA) and is drawn with a stress-strain curve and a tensile strain trend graph, the result is shown in FIGS. 6 and 7, wherein the sample in comparative example 1 is named as Control group.
As is apparent from fig. 6, each electrospun fiber remained uniformly dispersed, and as the induction time became longer, the degree of bending deformation of each sample fiber gradually increased, but the bending orientation thereof also began to become uneven, as compared with the non-induced sample of comparative example 1; as can be seen from fig. 7, compared with the sample of comparative example 1, the elastic phase of the samples obtained in examples 1, 4 and 5 is significantly extended, and no significant yield phenomenon occurs after 15% of pressure is reached, which indicates that the toughness of the fiber membrane product induced by the solvent is significantly improved, and by controlling the induction time, the control of different mechanical properties can be realized, and the mechanical property gradient design can be realized.
Effect example 3
In order to verify the influence of the solvent induction temperature on the appearance and tensile strain performance of the prepared bionic fiber ring scaffold, the bending-oriented electrostatic spinning fiber membranes obtained in examples 1 and 6-8 and the electrostatic spinning fiber membranes obtained in comparative example 1 are prepared into small strips with the same size, and a tensile mechanical property test is carried out by a dynamic thermomechanical analyzer (DMA) to draw a stress-strain curve and a tensile strain trend graph, wherein the result is shown in FIG. 8, and the sample in comparative example 1 is named as a Control group.
As can be seen from fig. 8, compared with the sample of comparative example 1, the elastic phase of the samples obtained in examples 1, 5 to 8 is significantly extended, and no significant yield phenomenon occurs after the pressure reaches 15%, which indicates that the toughness of the fiber membrane product induced by the solvent is significantly improved, and the control of different mechanical properties can be realized by controlling the induction temperature, thereby realizing the gradient design of the mechanical properties.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. A preparation method of a bionic fiber ring scaffold is characterized by comprising the following steps:
(1) preparing an electrostatic spinning membrane from the degradable high-molecular base material by an electrostatic spinning method;
(2) fixing and immersing the electrostatic spinning membrane into an organic solution, inducing at 25-60 ℃ for 20-120 min, taking out, freezing and drying to obtain a bent oriented electrostatic spinning fiber membrane; the organic solvent in the organic solution comprises at least one of ethanol, DMF, DCM, TFEA and HFIP;
(3) cutting the electrostatic spinning fiber membrane with the bending orientation into electrostatic spinning fiber strips, wherein the long axes of the strips and the fiber orientation in the fiber membrane form a +/-25-35 degree angle during cutting;
(4) winding each electrostatic spinning fiber strip into a composite layer of concentric annular supports, and coating extracellular matrix between layers to obtain the bionic fiber ring support; the orientation direction of the electrostatic spinning fiber strips of the adjacent layers in the bionic fiber ring support is +/-25-35 degrees; and the electrostatic spinning fiber strips with the orientation directions of plus or minus 25-35 degrees and the electrostatic spinning fiber strips with the orientation directions of minus 25-35 degrees are alternately and adjacently wound.
2. The method for preparing a biomimetic fiber ring scaffold according to claim 1, wherein the degradable polymer substrate in step (1) comprises at least one of PLLA, PCL, PLCL or derivatives thereof.
3. The method for preparing a biomimetic fiber ring scaffold according to claim 1, wherein the speed of the injection pump is 2-3 mL/h when the electrospun membrane is prepared by the electrospinning method in step (1), the spinning needle is a 9G stainless steel needle, the positive voltage applied to the needle is 12-18 kV, the negative voltage corresponding to the receiver is 0.5-1 kV, and the distance between the needle and the receiver is 8-10 cm.
4. The preparation method of the bionic fiber ring scaffold as claimed in claim 1, wherein the temperature of the electrostatic spinning membrane prepared by the electrostatic spinning method in step (1) is 20-25 ℃, the relative humidity is 60-70%, the time is 1-2 h, and the electrostatic spinning membrane is dried in a vacuum environment for more than 12h after being prepared.
5. The method for preparing a biomimetic fiber ring scaffold according to claim 1, wherein the volume concentration of the organic solvent in the solution in the step (2) is 10-100%.
6. The preparation method of the bionic fiber ring scaffold as claimed in claim 1, wherein the temperature for induction in the step (2) is 40-60 ℃ and the time is 20-60 min.
7. The method for preparing a bionic fiber ring scaffold as claimed in claim 1, wherein the long axis of the strip is within ± 30 degrees of the fiber orientation in the fiber membrane during cutting in the step (3).
8. The method for preparing the bionic fiber ring scaffold of claim 1, wherein the orientation direction of the electrospun fiber strips of the adjacent layers in the bionic fiber ring scaffold in the step (4) is ± 30 degrees; and the electrostatic spinning fiber rods with the orientation directions of plus or minus 30 degrees are alternately and adjacently wound with the electrostatic spinning fiber rods with the orientation directions of minus 30 degrees.
9. The bionic fiber ring scaffold prepared by the preparation method of any one of claims 1 to 8.
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| CN113882139B (en) * | 2021-10-20 | 2023-07-21 | 浙江理工大学 | Preparation method of anisotropic silk fibroin-based nano calcium phosphate composite material |
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