CN115624649A - Bionic antibacterial adhesion pad material with temperature responsiveness - Google Patents
Bionic antibacterial adhesion pad material with temperature responsiveness Download PDFInfo
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- CN115624649A CN115624649A CN202211347222.1A CN202211347222A CN115624649A CN 115624649 A CN115624649 A CN 115624649A CN 202211347222 A CN202211347222 A CN 202211347222A CN 115624649 A CN115624649 A CN 115624649A
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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
- A61L24/04—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials
- A61L24/046—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- 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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- 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
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/02—Surgical adhesives or cements; Adhesives for colostomy devices containing 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
- 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
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
Abstract
The invention provides a bionic antibacterial adhesion pad material with temperature responsiveness. The material contains Ga nano particles, so that the adhesiveness of the Ga nano particles has reversible temperature responsiveness; ga nano particles in the material influence the modulus and the adhesion performance of the whole material; the melting point of the Ga nano particles is 30 ℃, and when the environmental temperature reaches a high-temperature threshold, the Ga nano particles are converted from a solid state to a liquid state, so that the modulus of the adhesion pad material is obviously reduced, and the adhesion performance is obviously reduced; when the environmental temperature is lower than the low-temperature threshold, the modulus of the adhesion pad material is enhanced, and the adhesion performance is enhanced. The adhesion pad material disclosed by the invention is good in sterilization performance, obvious in anti-fouling effect and reversible in response to temperature. The method has potential application value in the fields of biomedicine, wearable flexible electronic equipment and the like.
Description
Technical Field
The invention belongs to the technical field of bionic adhesion materials, and particularly relates to a bionic antibacterial adhesion pad material with temperature responsiveness.
Background
With the development of society, materials with single and stable and invariable adhesive properties no longer meet the needs of people. It is imperative to develop materials that can be modified under certain conditions for both hardness and adhesion. Nature provides many examples of excellent adhesion materials that achieve reliable and switchable adhesion on a contact surface. For example, snails secrete small mucoids during exercise and have low adhesion and can maintain conformal contact with rock or tree surfaces. When the dope dries, its shear modulus increases greatly, forming a hard film with strong adhesion to the target material surface. The mucus secreted by the skin of long snakes is a highly hydrated biomacromolecule. When the fish skin feels stimulated by the outside, the fish skin can realize the self-adaptive modulus conversion along with the contraction and the layering of red and white muscles in the body. All of the above polymeric adhesives have excellent switchable adhesion properties and are achieved by using an external stimulus (water or heat) to transition the material between solid (high modulus) and liquid (low modulus).
In recent years, the problem of iatrogenic infection generated in the use process of biomedical materials is endless, and the iatrogenic infection poses serious threats to the health and life of people. The construction of the surface antibacterial coating is one of the most effective strategies for solving the problems of the iatrogenic infections. The construction of the surface antibacterial coating not only endows the biomedical material with antibacterial performance, but also improves the biocompatibility of the material and endows the biomedical material with the functions of adhesion resistance, oxidation resistance, biological recognition, sensing and the like.
Based on the above, the organic modified Ga nano particles with modulus responsive to temperature and antibacterial property are added into the organic silicon resin to prepare the bionic antibacterial material with adhesion property and temperature responsive property.
Disclosure of Invention
The invention aims to provide a bionic antibacterial adhesion pad material with temperature responsiveness.
In order to achieve the purpose, the invention adopts the following scheme:
the antibacterial adhesion pad material provided by the invention has the advantages of good bactericidal performance, obvious antifouling effect, good biocompatibility and reversible temperature responsiveness of adhesion.
Furthermore, the Ga nanoparticles in the material have great influence on the modulus and the adhesion performance of the whole material. The melting point of the Ga nano particles is about 30 ℃, and when the environmental temperature reaches a high temperature threshold (40 ℃), the Ga nano particles can be converted from a solid state to a liquid state, so that the modulus of the adhesion pad material is obviously reduced, and the adhesion performance is obviously reduced; when the environmental temperature is lower than the low-temperature threshold (20 ℃), the modulus of the adhesion pad material is enhanced, and the adhesion performance is enhanced.
Furthermore, the antibacterial adhesion mat material also has the following characteristics:
other metals, such as In and Sn, etc., are allowed to be mixed into the Ga nanoparticles In the material. The melting points of the mixed Ga alloy nano particles are different according to different compositions and contents. The melting point of the Ga alloy nano particles is never changed within the range of 10-72 ℃ by regulating the composition proportion of the Ga alloy nano particles.
Furthermore, the antibacterial adhesion pad material related by the invention also has the following characteristics:
ga used in the material is a good antibacterial agent, and Ga nanoparticles or Ga alloy nanoparticles release Ga 3+ Plays an important role in antibacterial activity due to Ga 3+ In vivo with Fe 3+ Having a high degree of similarity, ga 3+ Can replace Fe 3+ However, ga 3+ Single electron reduction cannot be performed, and thus iron metabolism of bacteria is destroyed, resulting in bacterial death; while Ga 3+ It results in the production of reactive oxygen species, which cause bacterial cells to mutate and die.
Furthermore, the antibacterial adhesion mat material also has the following characteristics:
the Ga nanoparticles have poor dispersibility in the medium and are easy to agglomerate and deposit in the medium. Therefore, organic (such as oleic acid, dodecanethiol, polydopamine and the like) modified Ga nanoparticles or Ga alloy nanoparticles are used, and the organically modified Ga nanoparticles or Ga alloy nanoparticles can be uniformly distributed in a medium and do not agglomerate.
Furthermore, the antibacterial adhesion mat material also has the following characteristics:
the polydopamine has antibacterial performance, so that the modified Ga nanoparticles or Ga alloy nanoparticles have super-strong antibacterial performance.
Furthermore, the antibacterial adhesion pad material related by the invention also has the following characteristics:
the main component of the adhesion pad material is organic silicon resin (one or a plurality of organic silicon, polyurethane, epoxy resin and the like are compounded), the organic silicon resin is a substance with low surface energy, the anti-fouling performance is good, and dirt on the adhesion pad is easy to clean.
Furthermore, the antibacterial adhesion pad material related by the invention also has the following characteristics:
the adhesion pad material has the self-healing property, and the Ga nanoparticles or Ga alloy nanoparticles can promote the crosslinking of unreacted vinyl in the organic silicon resin to initiate polymerization, so that the self-healing effect is generated, and the service life of the adhesion pad is longer.
Furthermore, the antibacterial adhesion mat material also has the following characteristics:
the adhesion pad of the invention has a nano-scale rough structure constructed by organically modified Ga nanoparticles or Ga alloy nanoparticles, so that the anti-fouling performance and the adhesion performance of the surface of the material are stronger.
Furthermore, the antibacterial adhesion pad material related by the invention also has the following characteristics:
ga-released Ga 3+ Can replace Fe in organism 3+ This makes it possible to kill not only bacteria but also some other microorganisms, such as microalgae, which is the caseEndows the adhesion pad material with the algae resistance.
Furthermore, the antibacterial adhesion pad material related by the invention also has the following characteristics:
the adhesion pad material has better temperature responsiveness as the content of the organically modified Ga nanoparticles or Ga alloy nanoparticles in the adhesion pad material is higher, and the maximum content of the organically modified Ga nanoparticles in the adhesion pad material is 30%. When the adhesion pad material is organic modified Ga alloy nano particles, the content of the Ga nano particles is based on the content of the Ga alloy nano particles.
The beneficial effects of the invention are realized as follows:
according to the bionic antibacterial adhesion pad material with the adhesion performance and the temperature responsiveness, ga nano particles in the material have great influence on the modulus and the adhesion performance of the whole material, the melting point of Ga is about 30 ℃, and when the environment is heated from a lower temperature to a higher temperature, ga is converted from a solid state to a liquid state, so that the modulus of the adhesion pad material is obviously reduced, and the adhesion performance is obviously reduced. However, when the temperature is decreased from a higher temperature to a lower temperature, the modulus of the adhesion pad material is increased, and the adhesion performance is enhanced. The organic modified Ga nano particles endow the adhesive pad with super-strong sterilization performance. The organic modified Ga nano particles are not only uniformly distributed in the material, but also uniformly distributed on the surface of the material, so that a nano-scale rough structure is constructed on the surface of the material, and the adhesion pad material is endowed with better anti-pollution performance and adhesion performance. The adhesion pad material has good sterilization performance (the sterilization rate to E.coli and S.aureus is more than 90%), obvious anti-fouling effect and reversible responsiveness of adhesion performance to temperature.
Drawings
Fig. 1 is a schematic structural diagram of a bionic anti-bacterial adhesion pad material with temperature responsiveness according to an embodiment of the present invention, in which Ga nanoparticles are modified by organic substances such as oleic acid, dodecanethiol, and polydopamine.
Fig. 2 is a schematic structural diagram of the bionic anti-microbial adhesion pad material with temperature responsiveness according to an embodiment of the present invention, in which Ga nanoparticles are not modified.
FIG. 3 shows the cell activity of the adhesion pad material of the present invention.
Detailed Description
The invention is further illustrated by the following examples:
example 1
The adhesion of the material disclosed by the patent is tested for temperature response. As shown in fig. 1 and 2, the antibacterial adhesion pad material 1 with temperature responsiveness provided in this embodiment 1 includes a support layer 3, and an organic layer 5 coating organic modified nanoparticles 4. The supporting layer 3 is a solid structure and made of organic resin. The organically modified nanoparticles 4 are distributed uniformly both inside and on the surface of the support layer 3. The Ga nanoparticles 6 in fig. 2 have poor dispersibility in the support layer 3 and the agglomeration phenomenon is severe.
The adhesion force of the adhesion pad material of the invention was tested at a 180 ° peel angle using an adhesion force testing device, and a friction force test was performed under a load of 5 mN.
Pure organic resin adhesive pad at room temperature: the adhesion force was 12kPa, and the friction force was 16kPa.
Biomimetic adhesive pad containing nanoparticles 6 at 20 ℃: the adhesion was 30kPa, and the friction was 31kPa. .
Biomimetic adhesive pad containing nanoparticles 6 at 40 ℃: the adhesion was 15kPa, and the friction was 17kPa.
Biomimetic adhesive pad containing organically modified nanoparticles 4 at 20 ℃: the adhesion force was 40kPa, and the friction force was 43kPa
Biomimetic adhesive pad containing organically modified nanoparticles 4 at 40 ℃: the adhesion was 20kPa, and the friction was 23kPa.
After 500 repeated tests, the organic resin adhered to the pad at normal temperature: the adhesion was 5kPa, and the friction was 10kPa.
After 500 replicates, the biomimetic adhesive pad containing nanoparticles 6 at 20 ℃ was: the adhesion was 29kPa, and the friction was 28kPa.
After 500 replicates, the biomimetic adhesive pad containing nanoparticles 6 at 40 ℃ was: the adhesion was 14kPa, and the friction was 16kPa.
After 500 replicates, the biomimetic adhesive pad containing organically modified nanoparticles 4 at 20 ℃ was: the adhesion was 38kPa, and the friction was 41kPa.
After 500 replicates, the biomimetic adhesive pad containing organically modified nanoparticles 4 at 40 ℃ was: the adhesion was 19kPa, and the friction was 22kPa.
From the above test data, we reach three conclusions.
First, when the organic modified nanoparticles 4 and 6 containing Ga are added to the organic resin adhesive, the adhesive force is enhanced, and the adhesive pad containing the uniformly distributed organic modified nanoparticles 4 has the strongest adhesive force. This shows that the Ga-containing small particles do contribute to the improved adhesion properties of the material.
Secondly, after the two kinds of Ga-containing particles are added, the adhesion performance of the adhesion pad obviously has good response to the temperature, which is mainly caused by Ga, ga is solid at 20 ℃ and liquid at 40 ℃, and the conversion between the solid state and the liquid state enables the adhesion performance of the material to be greatly changed.
Finally, it can also be observed that the durability of the adhesive pad is significantly improved after the two types of particles containing Ga are added, because Ga can promote the continued reaction of the unreacted vinyl groups in the organic resin, so that the material has self-repairing properties.
Example 2
The material of the invention is tested for biocompatibility. We first tested the cellular activity of the material of the invention. The coating is first soaked in a solution of fibronectin to promote cell adhesion. Inoculating Human Umbilical Vein Endothelial Cells (HUVECs) on the cell surface, in DMEM containing 10% fetal bovine serum, at 5% 2 And cultured at 37 ℃ for 7 days, and a live/dead kit is added for cell activity detection. Fluorescence images were taken with a confocal microscope. The fluorescent live/dead stain images showed two sets of morphologic rules with few dead cells (fig. 3), indicating that the coating was not toxic to human cells.
Example 3
The durability test of the adhesion performance of the material on human skin is divided into two tests. Firstly, the first step is toThe materials of the present invention were attached to the forearm skin and peeled away to perform the adhesion test on the skin. Before the adhesion test, the forearm skin was washed with a mixture of deionized water and ethanol. The samples were cured on a plastic film and then cut into 50mm wide, 50mm long and 300 μm thick samples for testing. The adhesion test was performed on the samples after 14 days of application to the forearm skin and the freshly cured samples. Adhesion as cured was 1.6N cm -1 The peel force of the cured product before 14 days was 1.5N cm -1 . The adhesion of the material of the invention to the skin after two weeks is still ensured to be firmly attached to the forearm skin.
A cyclic adhesion peel test on the skin was then performed. After 100 times of adherent stripping, the adhesion force is still more than 1.45N cm -1 It shows that the material can still be used as a skin adhesive after continuous stripping.
Example 4
Test against e.coli (e.coli): firstly, preparing a Luria-Bertani (LB) liquid culture medium by using NaCl, yeast extract, tryptone and sterile water, and then adding agar into the LB liquid culture medium formula to obtain an LB solid culture medium; coli was added to LB liquid medium and cultured at 37 ℃ for 12 hours. Thereafter, the inventive material and a Ga-free organic resin square piece (20 mm. Times.20 mm) were placed in E.coli (20 mL) and cultured at 37 ℃ for 12 hours. And thirdly, taking the material and the organic resin square slice out of the bacteria solution, cleaning redundant bacteria on the surface of the slice by using sterile water, and then carrying out ultrasonic treatment on the square slice in the sterile water for 5min to shake off the bacteria attached to the surface of the square slice. And (3) coating the bacterial liquid containing the shake-off bacteria diluted by 1000 times on an LB solid culture medium, culturing for 12h at 37 ℃, then taking a picture of the LB solid culture medium, and counting the number of colonies. The antibacterial activity of the material on E.coli is evaluated by a flat plate counting method by taking an organic resin square sheet as a control group.
Table 1 shows the test results of e.coli resistance, and compared with the organic resin square plate, the e.coli resistance of the material of the present invention is 95%, which indicates that the addition of the organically modified Ga provides the material of the present invention with excellent e.coli resistance.
Table 1: coli resistance test results
| Antibacterial ratio (%) of PDA-Ga-PDMS | |
| E.coli | 95 |
| S.aureus | 96 |
Example 5
Test against staphylococcus aureus (s. Aureus): aureus was added to LB liquid medium and cultured at 37 ℃ for 12 hours. Thereafter, the material of the present invention and an organic resin square piece (20 mm. Times.20 mm) were placed in E.coli (20 mL) and cultured at 37 ℃ for 12 hours. And thirdly, taking the material and the organic resin square slice out of the bacteria solution, cleaning redundant bacteria on the surface of the slice with sterile water, and then ultrasonically treating the square slice in the sterile water for 5min to shake off the bacteria attached to the surface of the square slice. And (3) coating the bacterial liquid containing the shake-off bacteria diluted by 1000 times on an LB solid culture medium, culturing for 12h at 37 ℃, then taking a picture of the LB solid culture medium, and counting the number of colonies. The killing efficiency of the material of the invention on S.aureus is evaluated by a flat plate counting method by taking an organic resin square plate as a control group, and the related results are listed in the table I.
As can be seen from table 1, compared with the organic resin square sheet, the bacteriostatic efficiency of the material of the present invention to s.aureus is 96%, which indicates that the addition of the organically modified Ga provides the material of the present invention with excellent s.aureus resistance activity.
Example 6
The adhesion pad material is prepared by mixing organic silicon resin and organically modified Ga or alloy nano particles into a film, wherein the maximum content of the organically modified Ga or alloy nano particles is 30%, and when the content of the nano particles exceeds 30%, the film cannot be formed after the organic silicon resin and the nano particles are mixed, so that the adhesion pad material cannot be prepared.
The above embodiments are merely illustrative of the technical solutions of the present invention. Any modification or supplement or equivalent replacement made by a person skilled in the art on the basis of this embodiment is within the scope of the invention as claimed in the claims.
Claims (9)
1. A bionic antibacterial adhesion pad material with temperature responsiveness is characterized in that: the material contains Ga nano particles, so that the adhesiveness of the material has reversible temperature responsiveness; ga nano particles in the material influence the modulus and the adhesion performance of the whole material; the melting point of the Ga nano particles is 30 ℃, and when the environmental temperature reaches a high-temperature threshold, the Ga nano particles are converted from a solid state to a liquid state, so that the modulus of the adhesion pad material is obviously reduced, and the adhesion performance is obviously reduced; when the environmental temperature is lower than the low-temperature threshold, the modulus of the adhesion pad material is enhanced, and the adhesion performance is enhanced.
2. The bionic antibacterial adhesion pad material with temperature responsiveness of claim 1, wherein: other metals are allowed to be mixed into the Ga nano particles, and the melting points of the mixed Ga alloy nano particles are different according to different compositions and contents; the melting point of the Ga alloy nano particles is changed within the range of 10-72 ℃ by regulating and controlling the composition proportion of the Ga alloy nano particles.
3. The bionic antibacterial adhesion pad material with temperature responsiveness of claim 2, wherein: ga nanoparticles or Ga alloy nanoparticles released Ga 3+ Plays an important role in antibacterial activity due to Ga 3+ In vivo with Fe 3+ Having a high degree of similarity, ga 3+ Can replace Fe 3+ But Ga 3+ Cannot undergo one-electron reduction, and thus the iron metabolism of the bacteria is disrupted, resulting in bacterial death; at the same time Ga 3+ It results in the generation of active oxygen.
4. The bionic antibacterial adhesion pad material with temperature responsiveness of claim 3, wherein: organically modified Ga nanoparticles or Ga alloy nanoparticles are used, which are uniformly distributed in the medium and do not agglomerate.
5. The bionic antibacterial adhesion pad material with temperature responsiveness of claim 4, wherein: the Ga nano particles or Ga alloy nano particles modified by the polydopamine have super-strong bactericidal performance.
6. The bionic antibacterial adhesion pad material with temperature responsiveness of claim 1 or 5, wherein: the main component of the adhesion pad material is organic silicon resin which comprises one or a plurality of compounds of organic silicon, polyurethane and epoxy resin.
7. The anti-microbial adhesion pad material with temperature responsiveness of claim 6, wherein: the adhesion pad material has a nano-scale rough structure constructed by organically modified Ga nanoparticles or Ga alloy nanoparticles, so that the surface of the material has stronger anti-fouling performance and adhesion performance.
8. The anti-microbial adhesion pad material with temperature responsiveness of claim 3, 4, 5, 6 or 7, wherein: the Ga nano particles and the Ga alloy nano particles can promote the crosslinking of vinyl groups which are not reacted in the organic silicon resin to initiate polymerization, so that a self-healing effect is generated, and the service life of the adhesive pad is longer.
9. The anti-microbial adhesion pad material with temperature responsiveness of claim 1 or 2, wherein: the maximum content of the organic modified Ga nano particles in the adhesion pad material is 30 percent.
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