CN111888518A - Preparation method of transparent silkworm cocoon-based double faced adhesive tape for non-invasive sewing - Google Patents
Preparation method of transparent silkworm cocoon-based double faced adhesive tape for non-invasive sewing Download PDFInfo
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- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/0005—Ingredients of undetermined constitution or reaction products thereof
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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
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Abstract
The invention provides a preparation method of a transparent silkworm cocoon-based double faced adhesive tape for non-invasive sewing, which comprises the steps of firstly treating silkworm cocoons by using a ternary solution to obtain a soft and transparent silkworm cocoon film, then spraying a formic acid-calcium chloride solution on the surface of the soft and transparent silkworm cocoon film to modify the surface of the silkworm cocoon film to obtain viscosity, and volatilizing formic acid to obtain the transparent silkworm cocoon-based double faced adhesive tape for non-invasive sewing. The transparent silkworm cocoon-based double-sided adhesive tape for non-invasive suturing, prepared by the invention, has good flexibility, extensibility and transparency, can be kept in a soft state without hardening when being adhered to a wound, can adapt to wet tissue adhesion, and has wide application prospect. The invention is made of natural materials, omits complex preparation process, has simple operation and is suitable for industrial production.
Description
Technical Field
The invention relates to the technical field of non-invasive suturing, in particular to a preparation method of a transparent silkworm cocoon-based double faced adhesive tape for non-invasive suturing.
Background
After human surgery or injury, wound suturing is one of the key steps of wound healing, and the quality of wound healing is directly influenced. The difficulty of wound closure is increased by the presence of uncertainty in the location, shape, etc. of the injured tissue, which requires a relatively high closure technique for the surgeon when closing such wounds. The reason is that different suturing modes are needed mainly because the growth and recovery capacities of tissues and organs at different parts are different; tissues of different layers need to be separately sutured; the location of the lesion and the arrangement of tissue fibers also affect the method of suturing.
The noninvasive suture taking the medical adhesive as the core can solve the problem of the position which is difficult to reach by the traditional suture mode, is simple and convenient to operate, has high wound closing speed, does not cause secondary damage to the wound, and has obvious advantages in clinical application compared with the traditional suture mode (suture lines, steel nails and the like). In the research of new medical adhesive materials, there are currently three main types of adhesive materials, adhesive water adhesives inspired by mussels, hydrogels crosslinked by photoinitiation of imino groups, and adhesive hydrogels prepared by glycine derivatives-vinyl monomers and hydroxyapatite. The adhesive water mucilage glue inspired by the mussel mainly takes polydopamine as a base material, and the adhesive prepared by utilizing the structure of the polydopamine similar to the mussel protein has the advantages of high adhesion to different surfaces, cell affinity and the like. The hydrogel which is subjected to the photoinitiation imino crosslinking reaction is a hydrogel which is adhered by covalently bonding the water viscose and amino groups on the surface of a human body through the photoinitiation imino crosslinking reaction. The adhesive hydrogel prepared from the glycine derivative-vinyl monomer and the hydroxyapatite is prepared by adding the glycine derivative-vinyl monomer with biocompatibility and the hydroxyapatite. Both the hydrogel which is subjected to the imino crosslinking reaction initiated by light and the adhesive hydrogel prepared from the glycine derivative-vinyl monomer and the hydroxyapatite can be used for adhering wet tissues, but the hydrogel is synthesized by a chemical reaction, the preparation process is relatively complex, and the preparation process has the problem of environmental incompatibility, so that the development of the two types of hydrogels is hindered.
Compared with synthetic materials, natural materials are more adaptable to the development of hydrogels. The silk fibroin is a reproducible protein natural material, has the advantages of wide source, good biocompatibility, good degradability, adjustable mechanical property and the like, and has wide application in the field of biomedicine. In addition, it has been shown that silk fibroin can be crosslinked by a crosslinking agent or co-assembled with other polymers to prepare adhesives. Wherein, calcium ions can change the secondary structure in the silk fibroin so as to lead the silk fibroin film to have a plurality of different performances. For example, Hyunjoo j.lee et al prepared a silk fibroin-based glue using a formic acid-calcium chloride solution. The calcium ions have the function of capturing water in the formic acid solution and are combined with random coils in the silk fibroin through the metal chelating effect, so that the glue has good reusability, tensile property, biocompatibility and adhesiveness. However, this glue is liquid and cannot be shaped, resulting in its lack of mechanical properties. In addition, it requires a substrate during use and cannot be applied to wet tissue, thereby limiting its use in medical adhesives.
Aiming at the problems of the existing adhesive, the research and development of the adhesive for suturing in the future mainly aims to enable the adhesive to have wet tissue adhesion and take natural materials, so that a complex preparation process is omitted, and the applicable range of products is expanded. Meanwhile, the physical properties of the material are comprehensively considered, so that the adhesive can adhere to tissues and simultaneously has physical and chemical properties similar to those of the tissues, such as flexibility, extensibility, transparency and the like.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of a transparent silkworm cocoon-based double-sided adhesive tape for non-invasive suturing.
In research, the calcium ions and the silk fibroin have special effects, the special effects can enable the silk fibroin to have viscosity, and the formic acid-calcium chloride solution can enable the material to have good ductility. However, the existence of formic acid completely destroys the natural structure of silk fibroin, and simultaneously, the preparation process becomes more complicated. Further research shows that the ternary solution can make the silkworm cocoon become soft and transparent on the basis of keeping the natural structure of the silkworm cocoon, and after the silkworm cocoon is made soft, the formic acid-calcium chloride solution is sprayed on the surface of the silkworm cocoon in a proper proportion to enable the silkworm cocoon to have adhesiveness on the basis of keeping the natural structure. Meanwhile, the research finds that the spraying of the formic acid-calcium chloride solution does not affect the softness and transparency of the silkworm cocoons, and more importantly, the adhesive can keep a soft state without hardening when being adhered to wounds, and the adhesive also has adhesion to wet tissues.
Except for special description, the percentages are mass percentages.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a transparent silkworm cocoon-based double-sided adhesive for non-invasive sewing comprises two steps of preparing a soft and transparent silkworm cocoon film and preparing the transparent silkworm cocoon-based double-sided adhesive, and is characterized in that: the transparent silkworm cocoon-based double-sided adhesive for non-invasive sewing is prepared by spraying a formic acid-calcium chloride solution on the surface of a soft and transparent silkworm cocoon membrane to modify the surface of the silkworm cocoon membrane to obtain viscosity and volatilizing formic acid.
In the method, the concentration of the formic acid-calcium chloride solution is 5-30% by mass percent. Preferably, the concentration of the formic acid-calcium chloride solution is 20%.
In the method, formic acid-calcium chloride solution is sprayed on the surfaces of two layers of the silkworm cocoon membranes, after the spraying is finished, the silkworm cocoon membranes are placed in an environment of 40-80 ℃, the surface modification of the silkworm cocoon membranes is accelerated, the heating is continuously carried out for 0.5-3h, after the heating is finished, the modified silkworm cocoon membranes are placed at room temperature for ventilation, the formic acid on the surfaces is completely volatilized, and the formic acid is volatilized completely, so that the soft and transparent silkworm cocoon-based double faced adhesive tape is obtained.
Further, formic acid-calcium chloride solution is sprayed on the surfaces of the two layers of the silkworm cocoon membranes, after the spraying is finished, the silkworm cocoon membranes are placed in an environment with the temperature of 65 ℃, the surface modification of the silkworm cocoon membranes is accelerated, the heating is continuously carried out for 1 hour, after the heating is finished, the modified silkworm cocoon membranes are placed at room temperature for ventilation, the formic acid on the surfaces is completely volatilized, and the formic acid is volatilized completely, so that the soft and transparent silkworm cocoon base double faced adhesive disclosed by the invention is obtained.
In the method, the ternary solution is prepared from anhydrous calcium chloride, deionized water and anhydrous alcohol according to a molar ratio of 1: 2-9: 1-3. Further, the ternary solution is prepared from anhydrous calcium chloride, deionized water and anhydrous alcohol according to a molar ratio of 1: 8: 2, and (3) preparing.
In the method, the step of preparing the soft and transparent silkworm cocoon membrane by using the ternary solution comprises the following steps: completely soaking the silkworm cocoons without silkworm pupas in the ternary solution, pouring the ternary solution after completely soaking, and filling the ternary solution into a filter flask again, wherein the amount of the ternary solution is based on the fact that the silkworm cocoons are completely submerged; then, carrying out suction filtration on the suction filtration bottle filled with the ternary solution and the silkworm cocoons on a suction filtration machine for three times, wherein the boiling of the solution is used as a standard during suction filtration; after the suction filtration is finished, the silkworm cocoon and the ternary solution are separately packaged in a wide-mouth bottle, then the wide-mouth bottle is placed in a water bath kettle for water bath until the silkworm cocoon becomes soft and transparent, the wide-mouth bottle is taken out, and the ternary solution is washed away by deionized water to obtain the soft and transparent silkworm cocoon membrane.
In the method, the temperature of the water bath is 55-60 ℃.
A preparation method of a transparent silkworm cocoon-based double faced adhesive tape for non-invasive suture adopts the following steps:
(1) preparing a soft and transparent silkworm cocoon membrane:
the method is characterized in that the molar ratio of anhydrous calcium chloride, deionized water and anhydrous alcohol is 1: 8: 2 preparing a ternary solution, completely soaking the silkworm cocoons without silkworm chrysalis in the ternary solution, pouring the ternary solution after the silkworm cocoons are completely soaked, and filling the ternary solution into a filter flask again, wherein the amount of the ternary solution is based on the fact that the silkworm cocoons are completely submerged; then, carrying out suction filtration on the suction filtration bottle filled with the ternary solution and the silkworm cocoons on a suction filtration machine for three times, wherein the boiling of the solution is used as a standard during suction filtration; after the suction filtration is finished, subpackaging the silkworm cocoon and the ternary solution in a wide-mouth bottle, then placing the wide-mouth bottle in a water bath kettle at the temperature of 58 ℃ for water bath until the silkworm cocoon becomes soft and transparent, taking out the wide-mouth bottle, and washing away the ternary solution by using deionized water to obtain a soft and transparent silkworm cocoon membrane;
(2) preparing a transparent silkworm cocoon base double faced adhesive tape:
and (2) spraying a 20 mass percent formic acid-calcium chloride solution onto the surfaces of two layers of the silkworm cocoon membranes, placing the silkworm cocoon membranes in an environment at 65 ℃ after spraying is finished, accelerating the surface modification of the silkworm cocoon membranes, continuously heating for 1h, and after heating is finished, placing the modified silkworm cocoon membranes at room temperature for ventilation to completely volatilize formic acid on the surfaces and completely volatilize formic acid, thus obtaining the soft and transparent silkworm cocoon-based double faced adhesive tape.
Has the advantages that:
the invention provides a preparation method of a transparent silkworm cocoon-based double faced adhesive tape for non-invasive sewing, which comprises the steps of firstly treating silkworm cocoons by using a ternary solution to obtain a soft and transparent silkworm cocoon film, then spraying a formic acid-calcium chloride solution on the surface of the soft and transparent silkworm cocoon film to modify the surface of the silkworm cocoon film to obtain viscosity, and volatilizing formic acid to obtain the transparent silkworm cocoon-based double faced adhesive tape for non-invasive sewing. The transparent silkworm cocoon-based double-sided adhesive tape for non-invasive suturing, prepared by the invention, has good flexibility, extensibility and transparency, can be kept in a soft state without hardening when being adhered to a wound, can adapt to wet tissue adhesion, and has wide application prospect. The invention is made of natural materials, omits complex preparation process, has simple operation and is suitable for industrial production.
Drawings
FIG. 1 is a graph showing the results of adhesion strength of cocoon-based double-sided tapes prepared with different formic acid-calcium chloride mass ratios;
FIG. 2 is a graph showing the results of the adhesion of cocoon-based double-sided adhesive tape to rabbit liver wounds at different times;
FIG. 3 is a graph showing the results of adhesion of cocoon-based double-sided adhesive tape to a wound of a pig kidney;
FIG. 4 is a schematic view of a shearing test of a silkworm cocoon-based double-sided adhesive tape on a pigskin;
FIG. 5 is a graph showing the results of a shearing test of a silkworm cocoon-based double-sided tape on a pigskin.
Detailed Description
The present invention is described in detail below with reference to specific examples, which are given for the purpose of further illustrating the invention and are not to be construed as limiting the scope of the invention, and the invention may be modified and adapted by those skilled in the art in light of the above disclosure.
Example 1
A preparation method of a transparent silkworm cocoon-based double faced adhesive tape for non-invasive suture adopts the following steps:
(1) preparing a soft and transparent silkworm cocoon membrane, namely treating the silkworm cocoon in a ternary solution (molar ratio; water: calcium chloride: alcohol: 8:1:2) in a water bath for a certain time, and washing the ternary solution to obtain the soft and transparent silkworm cocoon membrane;
firstly, 648ml of deionized water is added into 500g of calcium chloride, 525ml of alcohol is added after the calcium chloride solution is cooled and the calcium chloride is completely dissolved, and the preparation of the ternary solution is completed after the solution is cooled for the second time. And then, completely soaking the silkworm cocoons without silkworm pupas in the ternary solution, namely pouring a proper amount of the ternary solution into a filter flask filled with the silkworm cocoons, then shaking the filter flask to soak the surfaces of the silkworm cocoons, pouring the ternary solution after the silkworm cocoons are completely soaked, and refilling the ternary solution into the filter flask, wherein the amount of the ternary solution is based on the fact that the silkworm cocoons are completely submerged. And then, carrying out suction filtration on the suction filtration bottle filled with the ternary solution and the silkworm cocoons on a suction filtration machine. Carrying out suction filtration for three times, wherein the solution is boiled during suction filtration; after the suction filtration is finished, the silkworm cocoon and the ternary solution are subpackaged in a wide-mouth bottle, then the wide-mouth bottle is placed in a water bath at 58 ℃ in a water bath until the silkworm cocoon becomes soft and transparent, the silk cocoon is taken out, and the ternary solution is washed away by deionized water to obtain the soft and transparent silkworm cocoon membrane.
(2) Preparing a transparent silkworm cocoon base double faced adhesive tape, namely spraying a formic acid-calcium chloride solution on the surface of a silkworm cocoon membrane to modify the surface of the silkworm cocoon membrane to obtain viscosity, and volatilizing formic acid to obtain the transparent silkworm cocoon base double faced adhesive tape;
adding 13.11ml of formic acid solution into 4g of calcium chloride, completing the preparation of 20 mass percent formic acid-calcium chloride solution after the calcium chloride is completely dissolved, spraying the formic acid-calcium chloride solution on the two surfaces of the silkworm cocoon membrane, placing the silkworm cocoon membrane in an environment of 65 ℃ after the spraying is completed, accelerating the modification process of the surface of the silkworm cocoon membrane, and continuously heating for one hour. After heating, placing the modified silkworm cocoon membrane at room temperature (25 ℃) and ventilating to completely volatilize formic acid on the surface for six hours; after formic acid is volatilized, the soft and transparent silkworm cocoon base double faced adhesive tape is obtained.
Referring to example 1, the influence of the mass ratio of formic acid-calcium chloride on the adhesion strength and softness of the cocoon-based double-sided adhesive tape of the present invention was examined, and the results of the examination are shown in table 1 below, in which the adhesion strength of the cocoon-based double-sided adhesive tape of the present invention prepared by using the formic acid-calcium chloride in a representative mass ratio is shown in fig. 1.
TABLE 1 influence of the mass ratio of formic acid-calcium chloride on the adhesion strength and softness of silkworm cocoon-based double-sided adhesive tape
Examining the adhesion performance of the silkworm cocoon-based double-sided adhesive prepared in the embodiment 1 of the invention on wounds, the experimental process comprises the following steps: after anesthetizing the rabbit, a 3 cm opening was cut into the rabbit's chest with a scalpel, and a portion of the liver was removed. Then, a 8mm long wound was cut on the liver, and double-sided adhesive tape was attached to the wound of the liver. Finally, the liver stuck with the double-sided adhesive tape is placed back into the rabbit body, and the chest cavity is sutured. These rabbits were euthanized on days 14, 28, 42, and 56, respectively. The liver with the double-sided tape attached was then taken out and photographed, and the result is shown in fig. 2. As a result: the double-sided adhesive tape remained adhered to the liver at day 56, indicating that the double-sided adhesive tape had good permanent adhesion capability and the appearance of the double-sided adhesive tape was still relatively soft.
The adhesion performance of the silkworm cocoon-based double faced adhesive tape prepared in the embodiment 1 of the invention to the kidney is examined, and the experimental process comprises the following steps: a 1 cm long wound was cut on the pig kidney to create a kidney wound model; the cocoon-based double sided tape was then adhered directly to the kidney wound as shown in fig. 3. In the model, even when the cocoon-based double-sided tape was completely attached to the kidney, the wound of the kidney was observed through the double-sided tape.
In order to more intuitively embody the viscosity of the silkworm cocoon-based double-sided adhesive tape, the inventor performs a shearing test by replacing human tissues with pig skin, and inspects the viscosity of the silkworm cocoon-based double-sided adhesive tape prepared in example 1, wherein a schematic diagram of the shearing test is shown in fig. 4, and fig. 5 shows a result of the shearing test, and the result shows that the silkworm cocoon-based double-sided adhesive tape treated by using a formic acid-calcium chloride solution with the mass fraction of calcium chloride of 20% has excellent adhesion and the shearing strength is as high as 53.77 KPa.
Claims (10)
1. A preparation method of a transparent silkworm cocoon-based double-sided adhesive for non-invasive sewing comprises two steps of preparing a soft and transparent silkworm cocoon film and preparing the transparent silkworm cocoon-based double-sided adhesive, and is characterized in that: the transparent silkworm cocoon-based double-sided adhesive for non-invasive sewing is prepared by spraying a formic acid-calcium chloride solution on the surface of a soft and transparent silkworm cocoon membrane to modify the surface of the silkworm cocoon membrane to obtain viscosity and volatilizing formic acid.
2. The method of claim 1, wherein: the concentration of the formic acid-calcium chloride solution is 5-30% by mass percentage.
3. The method of claim 2, wherein: the concentration of the formic acid-calcium chloride solution is 20%.
4. The method of claim 1, wherein: and spraying a formic acid-calcium chloride solution on the surfaces of two layers of the silkworm cocoon membranes, placing the silkworm cocoon membranes in an environment of 40-80 ℃ after spraying is finished, accelerating the surface modification of the silkworm cocoon membranes, continuously heating for 0.5-3h, and after heating is finished, placing the modified silkworm cocoon membranes at room temperature for ventilation to completely volatilize formic acid on the surfaces and volatilize the formic acid, thus obtaining the soft and transparent silkworm cocoon-based double faced adhesive.
5. The method of claim 4, wherein: and after the heating is finished, the modified silkworm cocoon membrane is placed at room temperature for ventilation, so that the formic acid on the surface is completely volatilized, and the formic acid is volatilized completely, so that the soft and transparent silkworm cocoon-based double faced adhesive tape is obtained.
6. The method of any one of claims 1-5, wherein: the ternary solution is prepared from anhydrous calcium chloride, deionized water and anhydrous alcohol in a molar ratio of 1: 2-9: 1-3.
7. The method of claim 6, wherein: the ternary solution is prepared from anhydrous calcium chloride, deionized water and anhydrous alcohol in a molar ratio of 1: 8: 2, and (3) preparing.
8. The method of any one of claims 1-5, wherein: the preparation method of the soft and transparent silkworm cocoon membrane comprises the following steps: completely soaking the silkworm cocoons without silkworm pupas in the ternary solution, pouring the ternary solution after completely soaking, and filling the ternary solution into a filter flask again, wherein the amount of the ternary solution is based on the fact that the silkworm cocoons are completely submerged; then, carrying out suction filtration on the suction filtration bottle filled with the ternary solution and the silkworm cocoons on a suction filtration machine for three times, wherein the boiling of the solution is used as a standard during suction filtration; after the suction filtration is finished, the silkworm cocoon and the ternary solution are separately packaged in a wide-mouth bottle, then the wide-mouth bottle is placed in a water bath kettle for water bath until the silkworm cocoon becomes soft and transparent, the wide-mouth bottle is taken out, and the ternary solution is washed away by deionized water to obtain the soft and transparent silkworm cocoon membrane.
9. The method of claim 8, wherein: the temperature of the water bath kettle is 55-60 ℃.
10. A preparation method of a transparent silkworm cocoon-based double faced adhesive tape for non-invasive suture adopts the following steps:
(1) preparing a soft and transparent silkworm cocoon membrane:
the method is characterized in that the molar ratio of anhydrous calcium chloride, deionized water and anhydrous alcohol is 1: 8: 2 preparing a ternary solution, completely soaking the silkworm cocoons without silkworm chrysalis in the ternary solution, pouring the ternary solution after the silkworm cocoons are completely soaked, and filling the ternary solution into a filter flask again, wherein the amount of the ternary solution is based on the fact that the silkworm cocoons are completely submerged; then, carrying out suction filtration on the suction filtration bottle filled with the ternary solution and the silkworm cocoons on a suction filtration machine for three times, wherein the boiling of the solution is used as a standard during suction filtration; after the suction filtration is finished, subpackaging the silkworm cocoon and the ternary solution in a wide-mouth bottle, then placing the wide-mouth bottle in a water bath kettle at the temperature of 58 ℃ for water bath until the silkworm cocoon becomes soft and transparent, taking out the wide-mouth bottle, and washing away the ternary solution by using deionized water to obtain a soft and transparent silkworm cocoon membrane;
(2) preparing a transparent silkworm cocoon base double faced adhesive tape:
and (2) spraying a 20 mass percent formic acid-calcium chloride solution onto the surfaces of two layers of the silkworm cocoon membranes, placing the silkworm cocoon membranes in an environment at 65 ℃ after spraying is finished, accelerating the surface modification of the silkworm cocoon membranes, continuously heating for 1h, and after heating is finished, placing the modified silkworm cocoon membranes at room temperature for ventilation to completely volatilize formic acid on the surfaces and completely volatilize formic acid, thus obtaining the soft and transparent silkworm cocoon-based double faced adhesive tape.
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