CN111228563A - Preparation method of silk fibroin and tannic acid composite medical adhesive - Google Patents
Preparation method of silk fibroin and tannic acid composite medical adhesive Download PDFInfo
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- CN111228563A CN111228563A CN202010053074.7A CN202010053074A CN111228563A CN 111228563 A CN111228563 A CN 111228563A CN 202010053074 A CN202010053074 A CN 202010053074A CN 111228563 A CN111228563 A CN 111228563A
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- silk fibroin
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- tannic acid
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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
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/0047—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L24/0073—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material with a macromolecular matrix
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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
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/001—Use of materials characterised by their function or physical properties
- A61L24/0015—Medicaments; Biocides
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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
- A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
- A61L2300/23—Carbohydrates
- A61L2300/232—Monosaccharides, disaccharides, polysaccharides, lipopolysaccharides
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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
- A61L2300/60—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special physical form
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- Health & Medical Sciences (AREA)
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- Materials Engineering (AREA)
- Engineering & Computer Science (AREA)
- Surgery (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Composite Materials (AREA)
- Materials For Medical Uses (AREA)
Abstract
The invention discloses a preparation method of a silk fibroin and tannic acid composite medical adhesive, which comprises the following steps of taking silkworm silk fibroin and tannic acid as main raw materials, combining strong hydrogen bonds of the silk fibroin and the tannic acid to enable the silk fibroin to be rapidly separated out from a solution, thus obtaining the viscous silk fibroin and tannic acid composite adhesive, freeze-drying the prepared composite adhesive, grinding the composite adhesive into freeze-dried powder, paving the freeze-dried powder at a wound when in use, and forming adhesive to adhere to the wound and block the wound to realize wound sealing as soon as the freeze-dried powder meets water. The method for preparing the medical adhesive is simple and easy to implement, and the freeze-dried powder is convenient to store for a long time and is beneficial to sterilization before use.
Description
Technical Field
The invention relates to the technical field of medical materials, in particular to a preparation method of a silk fibroin and tannic acid composite medical adhesive.
Background
The ideal medical adhesive is safe, non-toxic, non-irritating, non-teratogenic, high in adhesive strength, good in biocompatibility and antibacterial property, capable of being used under the condition of existence of blood and tissue fluid, free of degradation product dissolution influencing healing, free of cytotoxicity, low in heat generated by curing and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a preparation method of a silk fibroin and tannin composite medical adhesive, and particularly provides a preparation method of a medical adhesive used in a freeze-dried powder form, wherein the freeze-dried powder form is not only beneficial to long-time storage, but also convenient for sterilization before use, which is a very important link before the medical adhesive is used. When in use, the freeze-dried powder is spread on a wound to absorb water (spray a small amount of water) and coagulate so as to realize wound sealing, and since silk fibroin and tannic acid are natural biological materials, the silk fibroin and tannic acid composite has good biocompatibility, no toxic or side effect and can be degraded and metabolized in tissues.
In order to achieve the purpose, the technical scheme provided by the invention is as follows: the preparation method of the silk fibroin and tannin composite medical adhesive comprises the following steps:
1) adding a lithium bromide solution into the degummed silk, heating for dissolving, and dialyzing to obtain a silk fibroin solution;
2) adding a tannic acid solution into the silk fibroin solution until the mixed solution is light yellow, stirring to uniformly mix, standing until the solution becomes clear and transparent from turbidity, and removing the supernatant to obtain a silk fibroin and tannic acid compound;
3) the silk fibroin and tannin composite is freeze-dried and ground to obtain composite freeze-dried powder, namely the silk fibroin and tannin composite medical adhesive, namely the medical adhesive is in a freeze-dried powder use form, and the freeze-dried powder is sprayed with water to be coagulated when the medical adhesive is used.
In the step 1), the degummed silk is silk fibroin obtained by degummed silkworm silk.
In the step 2), the concentration of the silk fibroin solution is 1-7 w/w%.
In the step 2), the concentration of the tannic acid solution is between 5 and 60 w/v%.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the raw materials of the composite freeze-dried powder prepared by the invention are only silk fibroin and tannic acid, and the composite freeze-dried powder is simple in raw material, wide in source and low in cost.
2. The silk fibroin and the tannin are respectively natural animal protein and natural plant polyphenol, and have the advantages of good biocompatibility and biodegradability in vivo.
3. The reaction process only needs simple mixing to form the compound through physical crosslinking reaction without complicated chemical synthesis process.
4. The adhesive is stored in a freeze-dried powder form, so that the stability of the material is improved, and sterilization before use is more convenient.
5. The prepared composite freeze-dried powder can be recovered into the adhesive to seal the wound when meeting water, and the operation is simple and easy to implement and the reaction is mild.
6. The silk fibroin has the anti-swelling property, and can avoid the excessive expansion of the adhesive in the body to cause the tissue extrusion.
7. The tannic acid has an antibacterial function and can reduce the risk of adhesive bacterial contamination.
Drawings
FIG. 1 is a photograph of an OHP film adhesion tensile test.
Fig. 2 is a photograph of a tissue adhesion tensile test.
Fig. 3 is a photograph of the adhesion of glue to the heart.
Detailed Description
The invention is further illustrated below with reference to a number of specific examples.
Example 1
Adding lithium bromide solution into degummed silk (specifically silk fibroin obtained by degummed silkworm silk), heating for dissolving, dialyzing to obtain silk fibroin solution, mixing 1 w/w% silk fibroin solution with 5 w/v% tannic acid solution, stirring, standing for several hours, removing clear solution, freeze drying the precipitate, grinding into powder, wetting and condensing 10mg of lyophilized powder, placing between two OHP films, and making contact area between viscose and OHP be 10 × 5mm2The adhesive strength of the adhesive was tested in a 180 ° tensile test mode using a texture analyzer (as shown in fig. 1), with 3 replicates.
Example 2
Adding lithium bromide solution into degummed silk (specifically silk fibroin obtained by degummed silkworm silk), heating for dissolving, dialyzing to obtain silk fibroin solution, mixing 7 w/w% silk fibroin solution with 5 w/v% tannic acid solution, stirring, standing for several hours, removing clear solution, freeze drying the precipitate, grinding into powder, wetting and condensing 10mg of lyophilized powder, placing between two OHP films, and making contact area between viscose and OHP be 10 × 5mm2The adhesive strength of the adhesive was tested in a 180 ° tensile test mode using a texture analyzer (as shown in fig. 1), with 3 replicates.
Example 3
Adding lithium bromide solution into degummed silk (specifically silk fibroin obtained by degummed silkworm silk), heating for dissolving, dialyzing to obtain silk fibroin solution, mixing 3 w/w% silk fibroin solution with 30 w/v% tannic acid solution, stirring, standing for several hours, removing clear liquid, freeze drying the precipitate, grinding into powder, and collecting lyophilized powder 10mg of the solution is wetted and coagulated and then placed between two OHP films, and the contact area between the viscose and the OHP films is 10 multiplied by 5mm2The adhesive strength of the adhesive was tested in a 180 ° tensile test mode using a texture analyzer (as shown in fig. 1), with 3 replicates.
Example 4
Adding lithium bromide solution into degummed silk (specifically silk fibroin obtained by degummed silkworm silk), heating for dissolving, dialyzing to obtain silk fibroin solution, mixing 1 w/w% silk fibroin solution with 60 w/v% tannic acid solution, stirring, standing for several hours, discarding clear solution, freeze-drying the precipitate, grinding into powder, wetting and condensing 10mg of lyophilized powder, placing between two OHP films, and making contact area between viscose and OHP be 10 × 5mm2The adhesive strength of the adhesive was tested in a 180 ° tensile test mode using a texture analyzer (as shown in fig. 1), with 3 replicates.
Example 5
Adding lithium bromide solution into degummed silk (specifically silk fibroin obtained by degummed silkworm silk), heating for dissolving, dialyzing to obtain silk fibroin solution, mixing 7 w/w% silk fibroin solution with 60 w/v% tannic acid solution, stirring, standing for several hours, discarding clear solution, freeze-drying the precipitate, grinding into powder, wetting and condensing 10mg of lyophilized powder, placing between two OHP films, and making contact area between viscose and OHP be 10 × 5mm2The adhesive strength of the adhesive was tested in a 180 ° tensile test mode using a texture analyzer (as shown in fig. 1), with 3 replicates.
The specific detection results of the above examples 1 to 5 are shown in the following table 1:
TABLE 1 adhesion Strength values of adhesives in the examples
The following experiments are carried out on the prepared silk fibroin and tannin composite medical adhesive:
example 6 (Water adhesion resistance of composite medical adhesive of Silk fibroin and tannin)
(1) Preparation of the experiment: the lyophilized powder obtained in example 3 was wetted with a small amount of water to obtain a corresponding adhesive and placed between two OHP films having a width of 10mm and a contact area of 10X 5mm2After full contact, the mixture is respectively placed in deionized water for 5h, 3h, 1h, 30min and 10 min.
(2) Adhesion testing: the adhesive strength of each set of samples was tested using a 180 ° tensile test mode of a texture analyzer at a tensile speed of 50mm/min for each set of three replicates. The test results are shown in table 2 below:
TABLE 2 adhesion properties after soaking for various periods of time
As can be seen from the results in the table, the adhesive has good adhesive performance, and the adhesive strength is not only not influenced by the soaking time, but also enhanced due to the prolonged time.
Example 7 (adhesive Property of composite medical adhesive of Silk fibroin and tannin to tissue)
(1) Preparation of the experiment: adding a small amount of water into the freeze-dried powder obtained in example 3 to wet the freeze-dried powder to obtain a corresponding adhesive, placing the adhesive at one end of two pieces of OHP films with the width of 10mm, and connecting the other side of the adhesive with the thickness of 30X 20mm2The rabbit tissue was contacted at both ends, placed at room temperature and two slides placed on top, and allowed to fully contact the OHP membrane under a certain force (as shown in figure 2).
(2) Adhesion testing: and testing the adhesive strength of the adhesive by using a 180-degree tensile test mode of a texture analyzer, wherein the tensile speed is 50mm/min, and three samples are parallel. The resulting adhesive strength was the maximum value of the tensile force measured divided by the contact area of the adhesive with the OHP film (0.01X 0.005 m)2) The adhesion values to rabbit skin, rabbit liver and rabbit heart were: 10.9 +/-3.3 kPa, 8.5 +/-3.6 kPa and 8.7 +/-3.1 kPa.
Example 8 (Heart burst pressure test)
(1) Sample preparation: the rabbit heart was sampled, the blood stasis in the heart was squeezed out, a hole with a diameter of 2mm was drilled in the right ventricle, 60mg of the lyophilized powder of example 3 was coated on and around the hole in a circular shape with a diameter of 10mm, and the lyophilized powder was then wetted with physiological saline to adhere to the heart (as shown in fig. 3).
And (3) testing the blasting pressure: burst pressure testing was performed using a home-made device with a 50ml syringe and a digital pressure display. The syringe is filled with normal saline, and is injected into the heart at the speed of 2ml/min, and the joint with the heart and the rest part of the right ventricle of the heart, which is communicated with the outside, are sealed by glue. The number of replicates was 3. The obtained burst pressure value is 31.8 + -7.4 mmHg, and when a hard OHP film is added on the surface of the adhesive as a support, the burst pressure value can be increased to 46.8 + -17.1 mmHg.
The above-mentioned embodiments are merely preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, so that the changes in the shape and principle of the present invention should be covered within the protection scope of the present invention.
Claims (4)
1. The preparation method of the silk fibroin and tannin composite medical adhesive is characterized by comprising the following steps:
1) adding a lithium bromide solution into the degummed silk, heating for dissolving, and dialyzing to obtain a silk fibroin solution;
2) adding a tannic acid solution into the silk fibroin solution until the mixed solution is light yellow, stirring to uniformly mix, standing until the solution becomes clear and transparent from turbidity, and removing the supernatant to obtain a silk fibroin and tannic acid compound;
3) the silk fibroin and tannin composite is freeze-dried and ground to obtain composite freeze-dried powder, namely the silk fibroin and tannin composite medical adhesive, namely the medical adhesive is in a freeze-dried powder use form, and the freeze-dried powder is sprayed with water to be coagulated when the medical adhesive is used.
2. The preparation method of the silk fibroin and tannin composite medical adhesive according to claim 1, which is characterized by comprising the following steps: in the step 1), the degummed silk is silk fibroin obtained by degummed silkworm silk.
3. The preparation method of the silk fibroin and tannin composite medical adhesive according to claim 1, which is characterized by comprising the following steps: in the step 2), the concentration of the silk fibroin solution is 1-7 w/w%.
4. The preparation method of the silk fibroin and tannin composite medical adhesive according to claim 1, which is characterized by comprising the following steps: in the step 2), the concentration of the tannic acid solution is between 5 and 60 w/v%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112587715A (en) * | 2021-01-08 | 2021-04-02 | 成都煌泓亢环保科技有限公司 | Preparation method of high-adhesion medical composite adhesive |
| CN113279253A (en) * | 2021-04-02 | 2021-08-20 | 百事基材料（青岛）股份有限公司 | Silk large biological fiber containing coffee active component and preparation method thereof |
| CN113398323A (en) * | 2021-06-30 | 2021-09-17 | 华中科技大学同济医学院附属协和医院 | Preparation method and application of sericin adhesive |
| CN114808454A (en) * | 2022-05-05 | 2022-07-29 | 苏州大学 | Amorphous colloid array structure yarn-dyed fabric and preparation method thereof |
| CN115779138A (en) * | 2022-11-24 | 2023-03-14 | 山东宝森新材料科技有限公司 | Silk fibroin hemostatic powder and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112587715A (en) * | 2021-01-08 | 2021-04-02 | 成都煌泓亢环保科技有限公司 | Preparation method of high-adhesion medical composite adhesive |
| CN113279253A (en) * | 2021-04-02 | 2021-08-20 | 百事基材料（青岛）股份有限公司 | Silk large biological fiber containing coffee active component and preparation method thereof |
| CN113398323A (en) * | 2021-06-30 | 2021-09-17 | 华中科技大学同济医学院附属协和医院 | Preparation method and application of sericin adhesive |
| CN114808454A (en) * | 2022-05-05 | 2022-07-29 | 苏州大学 | Amorphous colloid array structure yarn-dyed fabric and preparation method thereof |
| CN115779138A (en) * | 2022-11-24 | 2023-03-14 | 山东宝森新材料科技有限公司 | Silk fibroin hemostatic powder and preparation method and application thereof |
| CN115779138B (en) * | 2022-11-24 | 2024-05-24 | 山东宝森新材料科技有限公司 | Silk fibroin hemostatic powder and preparation method and application thereof |
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Application publication date: 20200605 |