CN111012950A - Composite repair patch and preparation method thereof - Google Patents
Composite repair patch and preparation method thereof Download PDFInfo
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- CN111012950A CN111012950A CN201911334408.1A CN201911334408A CN111012950A CN 111012950 A CN111012950 A CN 111012950A CN 201911334408 A CN201911334408 A CN 201911334408A CN 111012950 A CN111012950 A CN 111012950A
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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
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- 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
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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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- 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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/412—Tissue-regenerating or healing or proliferative agents
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Abstract
The invention relates to a composite repair patch and a preparation method thereof, and the preparation method comprises the following steps of dissolving polycaprolactone in dichloromethane to obtain a solution A, adding graphene oxide into dimethylformamide to obtain a solution B, and mixing the solution B with the solution A to obtain a solution C; mixing hexafluoroisopropanol and trifluoroethanol to form a mixed solution, adding chitosan into the mixed solution, carrying out homogenization treatment to obtain a homogenized mixed solution, and adding polycaprolactone powder to obtain a solution D; spinning the solution C to form an outer layer film, and attaching the solution D outside the outer layer film to form an inner layer film; obtaining a composite substrate; dissolving 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide in an alcohol solution, adding acetylcysteine to obtain a solution E, placing the composite substrate material in the crosslinking solution E, and taking out. The beneficial effects are that: the mechanical strength is better; has good anti-adhesion effect; has better tissue repair capability.
Description
Technical Field
The invention belongs to the technical field of medical repair patches, and particularly relates to a tissue defect repair patch and a preparation method thereof.
Background
At present, patches for repairing abdominal wall defects are various in types, but all the patches have defects in clinical application. Synthetic patches such as polypropylene, polytetrafluoroethylene are the most widely used materials in clinical practice. However, these materials are not degradable, and thus, complications such as abdominal organ adhesion, intestinal obstruction, intestinal fistula, chronic pain, etc. are likely to occur.
Although the biological patches such as small intestinal submucosa and dermal acellular matrix have good biocompatibility, the mechanical strength is insufficient, and the recurrence rate of the long-term hernia is high. The repair by using the autologous tissue skin flap is realized by 'removing the east wall and supplementing the west wall', so that the possibility of skin flap necrosis exists, and irreversible damage can be caused to a skin flap supply area. Therefore, it is necessary to design a patch which has good biocompatibility and mechanical strength to achieve the purpose of repairing and reconstructing the abdominal wall defect.
In 2018, degradable polycaprolactone-uracil ketone (PCL-UPy) electrostatic spinning patches are used for rat and rabbit abdominal wall defect repair research, but the results show that the composite scaffold is still poor in mechanical strength, high in hernia recurrence rate and high in failure rate up to 50%. Moreover, polycaprolactone can be degraded, but the degradation time is long, and the single application of polycaprolactone to abdominal wall defect repair still causes series of complications such as abdominal organ adhesion and the like.
Disclosure of Invention
Aiming at the problems, the invention provides a composite repair patch and a preparation method thereof, and mainly solves the problems that the existing synthetic patch in the prior art is easy to cause abdominal viscera adhesion, the biological patch is low in mechanical strength, high in hernia recurrence rate and the like.
In order to solve the problems, the invention adopts the following technical scheme:
a preparation method of a composite repair patch comprises the following steps,
dissolving polycaprolactone in dichloromethane to obtain solution A,
adding graphene oxide into dimethylformamide to obtain a solution B,
mixing the solution B with the solution A to obtain a solution C;
mixing hexafluoroisopropanol and trifluoroethanol to form a mixed solution, adding chitosan into the mixed solution, homogenizing to obtain a homogenized mixed solution,
adding polycaprolactone powder to obtain a solution D;
spinning the solution C to form an outer layer film, and spinning and attaching the solution D to the outside of the outer layer film to form an inner layer film;
obtaining a composite substrate material;
dissolving 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide in an alcohol solution, adding N-acetylcysteine to obtain a solution E,
and (4) placing the composite substrate material in the solution E, and taking out.
In one mode, the solution C is subjected to electrostatic spinning for 10-12h to form an outer layer film, and the solution D is subjected to electrostatic spinning for 6-8h to form an inner layer film.
One way, vacuum freezing to obtain composite substrate material; and soaking the composite substrate material in the crosslinking liquid for 20-24 h.
In one mode, the electrostatic spinning voltage is 15-18kv, the distance from the needle point to the collection panel is 8-10cm, and the flow rate is 1-1.5 ml/h.
One way, the mass ratio of the chitosan dissolved in the homogeneous mixed solution to the added polycaprolactone is 1: (8-10).
One way, in the crosslinking solution, the content of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is 50-55mmol/L, and the content of N-hydroxysuccinimide is 12.5-13 mmol/L;
the concentration of N-acetylcysteine is 0.5-0.6 mg/mL.
One way, the mass volume ratio of polycaprolactone in the solution A is 16-18%; the mass volume ratio of the graphene oxide of the solution C is 0.1-0.2%; the mass volume ratio of the chitosan in the solution D is 0.5-0.6%;
the volume ratio of the hexafluoroisopropanol to the trifluoroethanol is 3: (2-2.5).
A composite repair patch comprises a substrate,
the substrate includes:
a graphene oxide spinning film, which is a film,
and the outer side surface of the graphene oxide spinning membrane is adhered with a chitosan spinning membrane.
In one mode, the graphene oxide spinning film is a graphene oxide-polycaprolactone spinning film,
the chitosan spinning film is a chitosan-polycaprolactone spinning film.
In one form, the substrate is cross-linked with N-acetylcysteine.
The invention has the beneficial effects that:
1. the mechanical strength is better;
2. has effects in preventing abdominal viscera adhesion;
3. has better tissue repair capacity;
4. has better effect of promoting vascularization.
Drawings
FIG. 1 is a schematic flow chart of the preparation process of the composite double-layer abdominal wall defect repair patch;
FIG. 2 is a pictorial view and a scanning electron microscope image of embodiment 1 of the present invention;
FIG. 3 is a comparison graph of the tensile and tensile tests of 4 patches;
FIG. 4 is a comparison of the effectiveness of a patch of the present invention in a practical application;
FIG. 5 is a histological stain map;
FIG. 6 is a graph showing the results of a cell proliferation potency test;
FIG. 7 is a structural display diagram according to the present invention.
Detailed Description
The invention is further illustrated below:
example 1
A preparation method of a composite repair patch comprises the following steps,
dissolving polycaprolactone (molecular weight: 80000) in dichloromethane to obtain solution A with mass-volume ratio of 18%,
adding graphene oxide into dimethylformamide, stirring in ice bath to obtain solution B,
mixing the solution B with the solution A to obtain a solution C with the mass volume ratio of graphene oxide being 0.1%;
mixing hexafluoroisopropanol and trifluoroethanol according to a volume ratio of 3: 2 mixing to form a mixed solution, adding chitosan into the mixed solution, wherein the mass ratio of the dissolved chitosan to the added polycaprolactone is 1: 8, homogenizing to obtain a homogenized mixed solution,
adding polycaprolactone powder to obtain a solution D with a solute mass-volume ratio of 5%, wherein the chitosan mass-volume ratio is 0.5%;
carrying out electrostatic spinning on the solution C for 12h to form an outer layer film, and carrying out electrostatic spinning on the solution D for 6h to attach to the outside of the outer layer film to form an inner layer film; electrostatic spinning voltage is 18kv, the distance from the needle point to the collecting panel is 10cm, and the flow speed is 1 ml/h;
obtaining a composite substrate material;
dissolving 50 mmol/L1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 12.5mmol/L N-hydroxysuccinimide in alcohol solution, adding N-acetylcysteine to obtain solution E,
and (3) placing the composite substrate material in the crosslinking liquid E for 24 hours, taking out, and drying to obtain a finished product.
The structure of the finished product is as follows:
the display surface 1 is provided with an oxidized graphene spinning film 2, wherein the display surface 1 is used for making the structure of the invention clearer; has no structural significance;
a chitosan spinning film 3 is attached to the outer side surface of the graphene oxide-polycaprolactone film 2;
the graphene oxide spinning film 2 is a graphene oxide-polycaprolactone spinning film,
the chitosan spinning film 3 is a chitosan-polycaprolactone spinning film;
the substrate is provided with N-acetylcysteine in a cross-linking mode.
FIG. 1 is a flow chart of a composite bi-layer patch preparation;
FIG. 2 is a pictorial view of a composite double-layer patch and a scanning electron microscope;
fig. 3 is a mechanical strength test chart of the composite double-layer patch.
selecting a full-thickness abdominal wall defect model of an SD rat: a 2.0 multiplied by 1.5cm rectangular full-layer abdominal wall defect model is made in the middle abdomen of an SD rat (with the weight of 220-;
as shown in figure 4, no hernia formation and abdominal viscera adhesion are seen, and the composite double-layer patch can effectively avoid the hernia formation and the abdominal viscera adhesion when used for repairing abdominal wall defects.
Fig. 5 shows that the repair of abdominal wall defects by using the composite double-layer patch of the present invention can promote the formation of new collagen and the ingrowth of new blood vessels, and in fig. 5, arrows in Masson staining indicate that new collagen is formed in both the central region and the peripheral region of the material; the arrows in the CD31 staining indicate that new blood vessels are growing in both the central and peripheral regions of the material.
FIG. 6 is an in vitro CCK-8 experiment for verifying the proliferation potency of cells on a material, and is shown by graph A, the greater the amount of graphene oxide, the slower the proliferation rate of cells; as shown in the figure B, the composite double-layer patch (NAC-0.1% GO-PCL/CS-PCL) in the invention has good cell compatibility and good cell proliferation.
Example 2
A preparation method of a composite repair patch comprises the following steps,
dissolving polycaprolactone in dichloromethane to obtain a solution A with the mass volume ratio of 16 percent,
adding graphene oxide into dimethylformamide to obtain a solution B,
mixing the solution B with the solution A to obtain a solution C with the mass volume ratio of graphene oxide being 0.1%;
mixing hexafluoroisopropanol and trifluoroethanol according to a volume ratio of 3: 2 mixing to form a mixed solution, adding chitosan into the mixed solution, wherein the mass ratio of the dissolved chitosan to the added polycaprolactone is 1: 8, homogenizing to obtain a homogenized mixed solution,
adding polycaprolactone powder to obtain a solution D, wherein the mass volume ratio of the chitosan is 0.5%;
carrying out electrostatic spinning on the solution C for 10h to form an outer layer film, and carrying out electrostatic spinning on the solution D for 6h to attach to the outside of the outer layer film to form an inner layer film; electrostatic spinning voltage is 15kv, the distance from the needle point to the collecting panel is 8cm, and the flow speed is 1 ml/h;
obtaining a composite substrate material;
dissolving 50 mmol/L1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 12.5mmol/L N-hydroxysuccinimide in alcohol solution, adding N-acetylcysteine to obtain solution E,
and (3) placing the composite substrate material in the crosslinking liquid E for 20h, taking out, and drying to obtain a finished product.
Example 3
A preparation method of a composite repair patch comprises the following steps,
dissolving polycaprolactone in dichloromethane to obtain solution A with mass volume ratio of 18%,
adding graphene oxide into dimethylformamide to obtain a solution B,
mixing the solution B with the solution A to obtain a solution C with the mass volume ratio of the graphene oxide being 0.2%;
mixing hexafluoroisopropanol and trifluoroethanol according to a volume ratio of 3: 2.5 mixing to form a mixed solution, adding chitosan into the mixed solution, wherein the mass ratio of the dissolved chitosan to the added polycaprolactone is 1: 10, homogenizing to obtain a homogenized mixed solution,
adding polycaprolactone powder to obtain a solution D, wherein the mass volume ratio of the chitosan is 0.6%;
carrying out electrostatic spinning on the solution C for 12h to form an outer layer film, and carrying out electrostatic spinning on the solution D for 8h to attach to the outside of the outer layer film to form an inner layer film; electrostatic spinning voltage is 18kv, the distance from the needle point to the collecting panel is 10cm, and the flow speed is 1.5 ml/h;
obtaining a composite substrate material;
dissolving 55 mmol/L1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 13mmol/L N-hydroxysuccinimide in alcohol solution, adding N-acetylcysteine to obtain solution E,
and (3) placing the composite substrate material in the crosslinking liquid E for 24 hours, taking out, and drying to obtain a finished product.
Example 4
A preparation method of a composite repair patch comprises the following steps,
dissolving polycaprolactone in dichloromethane to obtain a solution A with the mass volume ratio of 17 percent,
adding graphene oxide into dimethylformamide to obtain a solution B,
mixing the solution B with the solution A to obtain a solution C with the mass volume ratio of the graphene oxide being 0.15%;
mixing hexafluoroisopropanol and trifluoroethanol according to a volume ratio of 3: 2.6 mixing to form a mixed solution, adding chitosan into the mixed solution, wherein the mass ratio of the dissolved chitosan to the added polycaprolactone is 1: 9, homogenizing to obtain a homogenized mixed solution,
adding polycaprolactone powder to obtain a solution D, wherein the mass volume ratio of the chitosan to the solution is 0.56%;
carrying out electrostatic spinning on the solution C for 11h to form an outer layer film, and carrying out electrostatic spinning on the solution D for 7h to attach to the outside of the outer layer film to form an inner layer film; electrostatic spinning voltage is 17kv, the distance from the needle point to the collecting panel is 9cm, and the flow speed is 1.2 ml/h;
obtaining a composite substrate material;
dissolving 52 mmol/L1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 12.6mmol/L N-hydroxysuccinimide in alcohol solution, adding N-acetylcysteine to obtain solution E,
and (3) placing the composite substrate material in the crosslinking liquid E for 22h, taking out, and drying to obtain a finished product.
It will be apparent to those skilled in the art that various modifications may be made to the above embodiments without departing from the general spirit and concept of the invention. All falling within the scope of protection of the present invention. The protection scheme of the invention is subject to the appended claims.
Claims (10)
1. A preparation method of the composite repairing patch is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
dissolving polycaprolactone in dichloromethane to obtain solution A,
adding graphene oxide into dimethylformamide to obtain a solution B,
mixing the solution B with the solution A to obtain a solution C;
mixing hexafluoroisopropanol and trifluoroethanol to form a mixed solution, adding chitosan into the mixed solution, homogenizing to obtain a homogenized mixed solution,
adding polycaprolactone powder to obtain a solution D;
spinning the solution C to form an outer layer film, and spinning and attaching the solution D to the outside of the outer layer film to form an inner layer film;
obtaining a composite substrate material;
dissolving 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide in an alcohol solution, adding N-acetylcysteine to obtain a solution E,
and (4) placing the composite substrate material in the solution E, and taking out.
2. The method for preparing a composite repair patch according to claim 1, characterized in that: and (3) carrying out electrostatic spinning on the solution C for 10-12h to form an outer layer film, and carrying out electrostatic spinning on the solution D for 6-8h to form an inner layer film.
3. The method for preparing a composite repair patch according to claim 2, characterized in that: vacuum freezing to obtain a composite substrate material; and soaking the composite substrate material in the solution E for 20-24 h.
4. The method for preparing a composite repair patch according to claim 2, characterized in that: electrostatic spinning voltage is 15-18kv, the distance from the needle point to the collecting panel is 8-10cm, and the flow rate is 1-1.5 ml/h.
5. The method for preparing a composite repair patch according to claim 1, characterized in that: the mass ratio of the chitosan dissolved in the homogeneous mixed solution to the added polycaprolactone is 1: (8-10).
6. The method for preparing a composite repair patch according to claim 1, characterized in that: in the crosslinking solution, the content of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is 50-55mmol/L, and the content of N-hydroxysuccinimide is 12.5-13 mmol/L;
the concentration of N-acetylcysteine is 0.5-0.6 mg/mL.
7. The method for preparing a composite repair patch according to claim 1, characterized in that: the mass volume ratio of the polycaprolactone in the solution A is 16-18%; the mass volume ratio of the graphene oxide of the solution C is 0.1-0.2%; the mass volume ratio of the chitosan in the solution D is 0.5-0.6%;
the volume ratio of the hexafluoroisopropanol to the trifluoroethanol is 3: (2-2.5).
8. A composite repair patch according to any of claims 1 to 7, wherein: comprises a substrate and a plurality of metal layers,
the substrate includes:
a graphene oxide spinning film (2),
and a chitosan spinning film (3) attached to the outer side surface of the graphene oxide spinning film (2).
9. A composite repair patch according to claim 8, wherein:
the graphene oxide spinning film (2) is a graphene oxide-polycaprolactone spinning film,
the chitosan spinning film (3) is a chitosan-polycaprolactone spinning film.
10. A composite repair patch according to claim 8, wherein:
the substrate is provided with N-acetylcysteine in a cross-linking mode.
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Cited By (1)
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| CN115068700A (en) * | 2022-07-12 | 2022-09-20 | 上海大学 | Multifunctional composite abdominal wall hernia repair patch and preparation method thereof |
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