CN115054690A - Spreadable hydrogel patch and preparation method and application thereof - Google Patents
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Abstract
The invention discloses a spreadable hydrogel patch and a preparation method and application thereof. The spreadable hydrogel patch is coated with nano-Fe 3 O 4 The composite chitosan-acrylamide/acrylic acid/propenyl dopamine copolymer double-network system is used as a template for preparation. On one hand, the hydrogel patch provided by the invention can be easily smeared on a wound bed to realize full coverage and complete attachment of skin defect, so that bacterial invasion is prevented and wound healing is promoted; on the other hand, the hydrogel patch has characteristics or properties such as magnetocaloric effect, adhesiveness and the like, and can realize comprehensive treatment of infected chronic wounds from both the directions of stimulating wound healing and resisting infection under the combined action of magnetic thermotherapy.
Description
Technical Field
The invention belongs to the technical field of biomedical materials, and particularly relates to a spreadable hydrogel patch and a preparation method and application thereof.
Background
The skin is an important organ which covers the surface of the human body and is in direct contact with the external environment, and is one of the most fragile tissues of the human body. Generally, after skin injury, normal tissue healing undergoes four stages of hemostasis, inflammation, hyperplasia, and tissue remodeling. However, the healing process becomes slow, delayed, interrupted or even arrested due to interference from many factors such as bacterial infection, inflammation, diabetes, etc., and such wounds are collectively referred to as chronic wounds.
Bacterial biofilm colonization is considered to be an important cause of chronic wound healing. Wolcott proposes topical application of antimicrobial dressings after surgical debridement in a manner that is most effective in disrupting and even removing the biofilm that has formed, which in turn stimulates wound healing.
Traditional wound dressings such as gauze, cotton pad and the like can only play a passive role in protecting a wound surface, and cannot solve the problems of chronic wound dehydration, biofilm infection and poor healing. Therefore, various new dressings such as hydrogel and silver ion dressing have been produced. Among them, the hydrogel having a specific function shows unique advantages in wound treatment due to its excellent biochemical and mechanical properties.
To date, hydrogels of various strategies (e.g., drug loaded, encapsulated metal preparations, etc.) have been produced to address wound infection and difficult healing issues. Among them, chemical drugs remain the first choice strategy for clinical treatment of infected wounds. Antibiotics, antibacterial drugs or angiogenesis drugs are loaded into the hydrogel, and the in-situ treatment of the infected wound is realized in a slow release or controlled release mode. In addition, inorganic metal particles are one of the most loaded antibacterial agents in hydrogels in addition to antibiotics due to their broad spectrum antibacterial and anti-inflammatory activities. Both strategies employ supported hydrogels, primarily by means of active ingredient release, to combat infection or promote wound repair. However, such hydrogels are prone to problems such as increased bacterial resistance, accumulation of drug toxicity, and implant failure. These problems have prompted researchers to develop safer and more effective multifunctional hydrogel systems to achieve comprehensive treatment of chronic wounds.
Disclosure of Invention
The invention aims to provide a spreadable hydrogel patch based on chronic wound complex therapy, which can realize complex therapy on infectious chronic wounds from two functions of destroying biological membranes and promoting wound healing by means of characteristics or properties of the spreadable hydrogel patch.
In order to achieve the purpose, the invention adopts the technical scheme that: a spreadable hydrogel patch with nano Fe structure 3 O 4 A composite chitosan-acrylamide/acrylic acid/propenyl dopamine copolymer double-network system.
The preparation method of the spreadable hydrogel patch comprises the following specific steps:
(1) improved solvothermal method for synthesizing magnetic nano Fe 3 O 4 Particles;
(2) the magnetic nano Fe is added 3 O 4 Adding the particles, chitosan, acrylic acid, allyl dopamine and acrylamide into a solvent, and uniformly stirring to obtain a mixture;
(3) adding ammonium persulfate into the mixture in the step (2), stirring uniformly, and then quickly transferring to a target mold to form hydrogel with a specific shape.
Specifically, the improved solvothermal method in the step (1) comprises the following steps: FeCl is added 3 ·12H 2 O, NaOH, mixing dodecylamine in glycol/diethylene glycol double solvent system, and reacting with polytetrafluoroethylene at high pressure to obtain magnetic nano Fe 3 O 4 And (3) granules. Wherein, the FeCl is calculated by mass ratio 3 ·12H 2 O, NaOH, the ratio of dodecylamine is 108:32: 75; the glycol/diethylene glycol double-solvent system comprises glycol and diethylene glycol, and the proportion of the glycol to the diethylene glycol is 1:4 in terms of volume ratio; the high-pressure reaction adopts a high-pressure reaction kettle,the temperature of the high-pressure reaction kettle is 200 ℃, and the reaction time is 12 h.
Specifically, in the step (2), 1 part by mass of the magnetic nano Fe is added 3 O 4 The particles are matched with 6 parts of chitosan, 11 parts of acrylic acid, 1 part of propenyl dopamine and 11 parts of acrylamide to react, the reaction method is a one-pot method, and the solvent is deionized water. In the step (3), the mass fraction of the ammonium persulfate is 0.6%.
The invention further claims application of the hydrogel patch in preparing a medicament for treating wounds. The hydrogel patch is in a structure of nano Fe 3 O 4 A composite chitosan-acrylamide/acrylic acid/propenyl dopamine copolymer double-network system.
In particular, the spreadable hydrogel patch can be used for preparing medicaments for repairing infected chronic wounds in cooperation with magnetothermal mediation, and the medicaments for treating the wounds comprise medicaments for destroying bacterial biofilms and medicaments for promoting wound healing.
By implementing the technical scheme of the invention, the following beneficial effects can be achieved:
(1) the hydrogel patch has good mechanical properties (the tensile strength is more than 50kPa, and the compressive strength is more than 100kPa), good biocompatibility, excellent magnetocaloric effect (under the action of AMF, the water temperature can be continuously increased to more than 65 ℃ within 10 min), spreadability and adhesiveness.
(2) The hydrogel patch utilizes the characteristics and properties of the hydrogel patch to resist and inhibit bacteria, is not treated in a traditional mode of releasing the loaded drug, and has important significance for solving the drug resistance of bacteria and controlling wound infection.
(3) Under the combined action of magnetic heat therapy, the effect of treating the infection type chronic wound is realized by the combined action of stimulating wound healing and resisting infection.
Drawings
Fig. 1 is a schematic design diagram of a multifunctional hydrogel patch.
FIG. 2 is an internal topography of a lyophilized DN/DAM/Fe hydrogel.
FIG. 3 shows the DN/DAM/Fe hydrogel applied to the surface of a finger by means of a syringe modified easily.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
This example uses nano Fe 3 O 4 Preparing the hydrogel patch by using the composite chitosan-acrylamide/acrylic acid/propenyl dopamine copolymer double-network system.
Based on the magnetic nano iron oxide compounded chitosan-polyolefin double-network hydrogel system shown in figure 1, the improved solvothermal method is adopted to synthesize the magnetic nano Fe 3 O 4 Particles of FeCl 3 ·12H 2 O is an iron source (AR, 2.7g), NaOH (AR, 0.8g) and dodecylamine (AR, 1.875g) are added and mixed in an ethylene glycol/diethylene glycol double solvent system (V) Ethylene glycol ＝30mL,V Diethylene glycol 120mL), put into a polytetrafluoroethylene high-pressure reaction kettle to react for 12 hours at 200 ℃ to obtain magnetic nano Fe with the diameter of about 50nm 3 O 4 And (3) granules. Then, Fe 3 O 4 (1 wt.%), CS (6 wt.%), acrylic acid (AA, 11 wt.%), propenyl dopamine (DAM, 1 wt.%), and acrylamide (AM, 11 wt.%) were added to deionized water in a one-pot process, stirred until homogeneous, then ammonium persulfate (APS, 2.8 wt.% APS/olefin monomer) was added, and after stirring, the mixture was rapidly transferred to a target mold to form a hydrogel having a specific shape.
Example 2
This example measured the mechanical properties of the hydrogel patch, and the preparation of the hydrogel patch used was described in example 1.
The compression performance (r) of cylindrical hydrogel samples (10 mm in height and 10mm in diameter) was respectively tested by an electronic universal tester Compression 2mm/min), and the tensile properties (r) of an elongated hydrogel sample (length 40mm, width 9mm, thickness 3mm) Stretching 50 mm/min). The results are shown in Table 1.
TABLE 1 composition and mechanical Properties of different hydrogels
As can be seen from Table 1, all the hydrogels exhibited suitable mechanical properties, with tensile strengths greater than 50kPa and compressive strengths greater than 100 kPa.
Example 3
This example observes the internal morphology of a lyophilized DN/DAM/Fe hydrogel, which was prepared as described in example 1.
And observing the internal appearance of the freeze-dried DN/DAM/Fe hydrogel by a high-resolution field emission scanning electron microscope. The preparation process of the freeze-dried hydrogel is as follows: and immersing the hydrogel into liquid nitrogen for quick freezing, taking out, and drying in a freeze dryer for 24 hours. The resulting internal topography is shown in fig. 2.
As can be seen from FIG. 2, the DN/DAM/Fe hydrogel shows a uniform porous structure, which is beneficial to the exchange of substances by cells and promotes the healing of wounds.
Example 4
This example tests the magnetocaloric properties of the hydrogels, and the preparation of the hydrogels used is described in example 1.
The closed vessel containing hydrogel (0.25g) and ultrapure water (0.5mL) was placed in an alternating magnetic field (AMF, magnetic field strength 200Oe), and the magnetocaloric properties of the hydrogel were measured by inserting a temperature probe below the liquid surface. The results are shown in Table 2.
TABLE 2 magnetocaloric Properties of different hydrogels
As can be seen from Table 2, the system contains magnetic Fe 3 O 4 Can be used in AMFAt the lower part, the water temperature is continuously increased to more than 65 ℃ within 10min, which shows that the magnetic thermal performance is excellent.
Example 5
This example tests the spreadability of the hydrogels, and the preparation of the hydrogels used is described in example 1.
Adding all hydrogel components (except APS) into a simple modified syringe by one-pot method, adding APS, stirring, and pushing the syringe to apply the hydrogel onto the surface of a finger. The results are shown in FIG. 3.
As can be seen from FIG. 3, the hydrogel can be easily pushed out by a syringe and applied on the finger surface, and even when the finger is moved, the hydrogel still adheres to the finger and does not deform or fall off, indicating that the prepared hydrogel has good spreadability and adhesiveness.
Example 6
This example tests the antimicrobial capacity and wound healing of hydrogel patches, and the preparation of the hydrogel patches used is described in example 1.
Female Kunming mice (weight 35g) were selected and randomly divided into 6 groups: blank untreated group, DN hydrogel group, DN/DAM hydrogel group, DN/Fe hydrogel group, and DN/DAM/Fe hydrogel group. After anesthesia skin preparation, a skin defect of 7mm in diameter was created and then 50. mu.L of Staphylococcus aureus (10. mu.L) was injected, respectively 8 CFU/mL) to establish an infection model. Then, different groups of pre-gels were applied to the wound bed by a custom syringe and the Control (CK) wounds were covered with a transparent wound dressing. After the hydrogel patch was implanted, each mouse was treated with magnetic heat for 10min at 0h and 48h, respectively. The average size of the wounds was observed periodically in each group of mice to assess the regeneration process of the wounds. The results are shown in Table 3.
TABLE 3 diameter of skin lesions in mice treated with different hydrogels
As can be seen from table 3, the healing speed of the wound of the mouse under different hydrogel treatment effects is as follows: DN/DAM/Fe hydrogel group > DN/DAM hydrogel group > DN hydrogel group.
Collecting skin tissue samples of each group of mice 7 days and 14 days after operation, soaking the skin samples in sterile PBS for homogenization to obtain bacterial suspension, diluting the bacterial suspension, further culturing the bacterial suspension in beef extract peptone culture medium, and counting the number of bacterial colonies of staphylococcus aureus to obtain the in vivo antibacterial activity of the hydrogel patch under the magnetocaloric effect. The results are shown in Table 4.
TABLE 4 colony counts of Staphylococcus aureus in mice treated with different hydrogels
As can be seen from table 4, the magnitude of the in vivo antibacterial activity of the mice under the different hydrogel treatment effects was: DN/DAM/Fe hydrogel group > DN/DAM hydrogel group > DN hydrogel group.
The present invention has been described in detail above. It will be apparent to those skilled in the art that the invention can be practiced in a wide range of equivalent parameters, concentrations, and conditions without departing from the spirit and scope of the invention and without undue experimentation. While the invention has been described with reference to specific embodiments, it will be understood that the invention may be further modified. In general, this application is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. The use of some of the essential features is possible within the scope of the claims attached below.
Claims (10)
1. The spreadable hydrogel patch is characterized in that the hydrogel patch is in a structure of nano Fe 3 O 4 A composite chitosan-acrylamide/acrylic acid/propenyl dopamine copolymer double-network system.
2. The method of making a spreadable hydrogel patch according to claim 1, comprising:
(1) improved solvothermal method for synthesizing magnetic nano Fe 3 O 4 Particles;
(2) the magnetic nano Fe is added 3 O 4 Adding the particles, chitosan, acrylic acid, allyl dopamine and acrylamide into a solvent, and uniformly stirring to obtain a mixture;
(3) adding ammonium persulfate into the mixture obtained in the step (2), stirring uniformly, and then quickly transferring to a target mould to form hydrogel with a specific shape.
3. The method of claim 2, wherein the modified solvothermal process of step (1) comprises: FeCl is added 3 ·12H 2 O, NaOH, mixing dodecylamine in glycol/diethylene glycol double solvent system, and reacting with polytetrafluoroethylene at high pressure to obtain magnetic nano Fe 3 O 4 And (3) granules.
4. The method of claim 3, wherein the FeCl is present in a mass ratio 3 ·12H 2 O, NaOH, the ratio of dodecylamine is 108:32: 75;
the glycol/diethylene glycol double-solvent system comprises glycol and diethylene glycol, and the proportion of the glycol to the diethylene glycol is 1:4 in terms of volume ratio;
the high-pressure reaction adopts a high-pressure reaction kettle, the temperature of the high-pressure reaction kettle is 200 ℃, and the reaction time is 12 hours.
5. The production method according to claim 2, wherein in the step (2), the magnetic nano-Fe is added in an amount of 1 part by mass 3 O 4 The particles are matched with 6 parts of chitosan, 11 parts of acrylic acid, 1 part of propenyl dopamine and 11 parts of acrylamide to react, the reaction method is a one-pot method, and the solvent is deionized water.
6. The production method according to claim 2, wherein the mass fraction of ammonium persulfate in the step (3) is 0.6%.
7. Use of the spreadable hydrogel patch according to claim 1 for the manufacture of a medicament for the treatment of wounds.
8. Use according to claim 7, wherein the spreadable hydrogel patch is for the manufacture of a medicament for repairing an infected chronic wound.
9. Use according to claim 7, wherein the spreadable hydrogel patch is used for the manufacture of a medicament for magneto-caloric mediated wound treatment.
10. The use of claim 7, wherein the wound treatment agent comprises a bacterial biofilm disruption agent, a wound healing promoting agent.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3305334A1 (en) * | 2016-10-06 | 2018-04-11 | Universitätsklinikum Jena | Magnetic composition and medical material for stimulating vascularisation in internal or external wound of the body |
| CN113599579A (en) * | 2021-07-26 | 2021-11-05 | 山东贝科德糖生物科技有限公司 | Double-network hydrogel and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3305334A1 (en) * | 2016-10-06 | 2018-04-11 | Universitätsklinikum Jena | Magnetic composition and medical material for stimulating vascularisation in internal or external wound of the body |
| CN113599579A (en) * | 2021-07-26 | 2021-11-05 | 山东贝科德糖生物科技有限公司 | Double-network hydrogel and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 刚芳莉: "高强度多功能磁性水凝胶的合成及其在修复类风湿性关节炎型软骨缺损中的应用", 《中国博士学位论文全文数据库 医药卫生科技辑》 * |
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