CN108452370A - A kind of compound supramolecular hydrogel and preparation method thereof - Google Patents
A kind of compound supramolecular hydrogel and preparation method thereof Download PDFInfo
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- 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
- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
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- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
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- 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
- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
- A61L26/0009—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form containing macromolecular materials
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- A—HUMAN NECESSITIES
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- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
- A61L26/0061—Use of materials characterised by their function or physical properties
- A61L26/0066—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
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- 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
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/412—Tissue-regenerating or healing or proliferative agents
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Abstract
The invention discloses a kind of compound supramolecular hydrogels and preparation method thereof, belong to supramolecular hydrogel technical field.Using chitosan as gelator, using " freeze-thaw method ", the compound supramolecular hydrogel of milky is formd with traditional Chinese medicine monomer cordycepin in PBS buffer solutions.The hydrogel component is the good natural products of biocompatibility, and the synergistic effect of chitosan and cordycepin enhances the anti-microbial property of the present invention.The present invention has self-healing, the performances such as smearable, two components of the compound supramolecular hydrogel not only increase the anti-microbial property of composite material by synergistic effect, and can reduce skin wound scar and be formed, and have broad application prospects in the fields such as anti-biotic material and wound dressing.
Description
Technical field
The present invention relates to a kind of compound supramolecular hydrogels and preparation method thereof, belong to supramolecular hydrogel technology neck
Domain.
Background technology
Up to the present, various wound-healing materials have been commercialized；However, clinical practice shows the need for still having new
It asks, because they are intended only as the temporary barrier for preventing infection and body fluid to be lost in.Wound healing deficiency is easy to form chronic wounds
Or lead to the complication of threat to life.Wound healing is a complexity and dynamic process, is divided into the predictable stage：Blood is solidifying
(Gu hemostasis), inflammation, tissue growth (proliferation) and tissue remodeling (maturation).In each stage, the system secreted by inflammatory cell
Row cell factor and growth factor play an important roll for restoring impaired eucaryotic cell structure and organized layer.In this respect, people
It has been primarily focused on skin graft using growth factor functionalization and/or based on cell.It is cured being related to wound
In the cell of conjunction process, macrophage may infect, tissue repair and solution inflammation.As host defense person, macrophage
Identification and adventive is destroyed, remove dead and impaired structural constituent (classics activation), and generated and adjust tissue growth and again
The cell factor of modeling, growth factor and angiogenesis factor activation).Therefore, exploitation has biocompatibility good, without side-effects
Hydrogel wound dressing be that this field is in demand.
Hydrogel (Hydrogel) is the gel using water as decentralized medium.There is good biocompatibility to be dropped with biology for it
Solution ability is frequently utilized for the holder of organizational project, wound repair, the fields such as drug conveying.More and more researchers are closed at present
Note its application as wound dressing.Hydrogel has as wound dressing to be absorbed Wound exudate, sterilization, moisturizing, promotes wound
The effect of the healing of mouth.The supramolecular hydrogel composite material with ideal antibiotic property and biocompatibility is designed for exploitation
Novel wound dressing has a very important significance.
Invention content
In order to solve the above technical problems, the present invention provides a kind of compound supramolecular hydrogels with good antibiotic property
And preparation method thereof, which has self-healing, smearable performance, is applied in anti-biotic material and wound
There is good application prospect in terms of material.
In order to achieve the above objectives, technical scheme is as follows：A kind of compound supramolecular hydrogel, including cordycepin
Solution, chitosan solution and PBS buffer solutions.
As a preferred embodiment of the present invention, a concentration of 100mg/mL of the cordycepin solution.
As a preferred embodiment of the present invention, the solvent of the chitosan solution is 1%HAc, the chitosan solution
A concentration of 20~40mg/L.
As a preferred embodiment of the present invention, the solvent of the PBS buffer solutions is ultra-pure water, and the PBS bufferings are molten
The PH of liquid is 8.3~8.5, each phosphate concn used is 0.1mol/L.
As a preferred embodiment of the present invention, the compound supramolecular hydrogel is applied to antiseptic or/and wound
In dressing.
A kind of preparation method of compound supramolecular hydrogel, includes the following steps：
Step 1, the preparation of cordycepin solution；With dmso solution cordycepin solid powder, ultrasonic disperse obtains worm
Careless element solution；
Step 2, the preparation of chitosan solution；Chitosan is dissolved with 1%HAc, magnetic agitation is matched to accelerate chitosan to dissolve
At chitosan solution；
Step 3, the preparation of PBS buffer solutions；Use Na2HPO4And NaH2PO4Solution allocation is molten at the PBS bufferings of different Ph
Liquid；
Step 4, after mixing by the cordycepin solution, chitosan solution and PBS buffer solutions, it is put into -20 DEG C of ice
Case is refrigerated to after fully charge to place to thaw at room temperature, forms the compound supramolecular hydrogel.
As the prioritization scheme to above-mentioned preparation method, in step 1, the dmso solution cordycepin solid powder
Time by ultrasonic disperse is 5~10min, and gained cordycepin solution concentration is 100mg/mL, and preparing, the cordycepin is molten
It carries out being protected from light processing during liquid.
As the prioritization scheme to above-mentioned preparation method, in step 2, a concentration of 20~40mg/ of the chitosan solution
ml；In step 3, the Ph of the PBS buffer solutions is 8.3~8.5, and in the PBS buffer solutions, Na2HPO4 and NaH2PO4 are dense
Degree is 0.1mol/L.
As the prioritization scheme to above-mentioned preparation method, step 4, the cordycepin solution of 80 μ of μ L~100 L is taken to be added
It is protected from light in the screw socket bottle of processing to the 2.0mL for cleaning drying, rapidly joins the PBS buffer solutions of 400~420 μ L, rapidly
It shakes up, adds the chitosan solution of 500 μ L, be made into the mixed solution of 1.0mL, the process for preparation of the mixed solution exists
It is carried out under magnetic agitation；The mixed solution is waited for after mixing, after screw socket bottle is put into -20 DEG C of refrigerator freezings to fully charge
Placement is thawed at room temperature, forms the compound supramolecular hydrogel.
Through the above technical solutions, the advantageous effect of technical solution of the present invention is：The hydrogelator that the present invention uses is
Chitosan is obtained by non-covalent bond self assembly, and aquagel is in spongelike structure.
Cordycepin is first nucleosides antibiotics separated from fungi, molecular formula C10H13N5O3.Antibacterial exists
It is played an important role in wound healing process, cordycepin has the function of broad-spectrum antiseptic, it can inhibit some bacteriums, fungi etc.
The growth of pathogen.In addition, cordycepin also has antiviral, immunological regulation, removes free radical, antitumor, anti-inflammatory etc. very extensively
The biological activity of spectrum.
Chitosan (Chitosan) is a kind of hydrophilic natural polymer.Chitosan has good broad spectrum antibiotic activity,
It can inhibit the growth and breeding of some fungies, bacterium and virus.Meanwhile chitosan has the function of promoting blood coagulation, can be used as stopping blooding
Agent.It can be additionally used in wound healing, be reduced bacterial wound growth, absorb Wound exudate, be not easy the effects that syneresis, be excellent
Good wound care dressings ingredient.In addition, chitosan has the function of thickener, the mechanical strength of composite material can be enhanced.
Chitosan can be responsible for one of functional biological materials of wound healing.Chitosan has prodigious excellent as medicament sustained-release matrix
More property can play synergistic effect in conjunction with cordycepin antibacterial advantage in antibacterial anti-inflammatory field.
1) composite natural product supramolecular hydrogel prepared by the present invention, biocompatibility is good, degradable, acellular
Toxicity.
2) composite natural product supramolecular hydrogel prepared by the present invention has suitable hardness, elastic and sticky, and ten
Divide suitable dermal application, is self-healing gel.
3) environmentally protective without adding any reducing agent and dispersant in preparation process of the present invention.
4) chitosan that the present invention is added can act synergistically with cordycepin, enhance the antibiotic property of hydrogel, it is easier to
It smears, is conducive to the absorption of skin, it is made to be more suitable for making wound dressing.
5) preparation method of the present invention is simple, of low cost, can be commercialized, and is suitable for large-scale production.
6) compound supramolecular hydrogel prepared by the present invention has good antibiotic property, can effectively facilitate wound healing, will
There can be good application prospect in fields in terms of antiseptic and wound dressing etc..
Description of the drawings
Fig. 1 is scanning electron microscope (SEM) figure of aquagel；
Fig. 2 is scanning electron microscope (SEM) figure of compound supramolecular hydrogel in the embodiment of the present invention 1；
Fig. 3 be the embodiment of the present invention 1 in compound supramolecular hydrogel at digital photograph figure before hydrogel；
Fig. 4 be the embodiment of the present invention 1 in compound supramolecular hydrogel at digital photograph figure after hydrogel
Bacterial growth situation after 12h on bacterium solution inoculation solid medium in Fig. 5 embodiments 1 in 1-3 fluid nutrient mediums
Digital photograph figure, No. 1-3 arranges from left to right；
Fig. 6, Fig. 7 are to contrast effect figure.Fig. 6 is the digital photograph figure of the similar SD rats wound of weight size.Fig. 7 is 15
The digital photograph figure of wound healing situation after it, left column is the digital photograph figure without any processing to wound in Fig. 7, in be classified as
The digital photograph figure containing only aquagel is smeared, the right side, which is classified as, smears compound supramolecular hydrogel in the embodiment of the present invention 2
Digital photograph figure.
Specific implementation mode
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained without creative efforts, all
Belong to the scope of protection of the invention.
Embodiment 1
The cordycepin solid powder for weighing 50.0mg, is dissolved in 500 μ L dimethyl sulfoxide (DMSO)s, and 5~10min of ultrasonic disperse makes it
It is completely dissolved, the cordycepin solution (being kept in dark place) of a concentration of 100mg/mL is made；The chitosan of 400mg is weighed, 10mL is added
The glacial acetic acid that volume ratio is 1% promotes the dissolving of chitosan, the chitosan for being made into 40mg/mL molten under the action of magnetic agitation
Liquid.
It takes the cordycepin solution of 100 μ L to be added to clean drying to be protected from light in the 2.0mL screw socket bottles of processing, rapidly joins 400 μ
The PBS buffer solutions of L, shake up rapidly, add the chitosan solution of 500 μ L, rapid oscillation, and magnetic agitation keeps its mixing equal
It is even.In conjunction with Fig. 3, Fig. 4, which is put into -20 DEG C of refrigerator freezings, then thaw at RT (pays attention to when summer temp is excessively high in sky
Adjust lower thaw) it can be obtained compound supramolecular hydrogel.Compound supramolecular hydrogel is scanned, is obtained shown in Fig. 2
Compound supramolecular hydrogel scanning electron microscope (SEM) figure.It can be compared with Fig. 1, compound supermolecule water
In spongelike structure smoother and with different pore size inside gel.
Antibacterial experiment step：10.0g tryptones, 5.0g yeast extracts and 10.0g sodium chloride are weighed in beaker, to
Ultrapure water dissolution is added in beaker, is stirred with glass bar and promotes dissolving, adjusts pH of mixed to 7.4 with sodium hydroxide, then uses
Ultra-pure water is settled in the conical flask of 1L and prepares fluid nutrient medium.
10.0g tryptones, 5.0g yeast extracts, 10.0g sodium chloride and 15.0g agar are weighed, is added into beaker
Ultrapure water dissolution is stirred with glass bar and promotes dissolving, is adjusted pH of mixed to 7.4 with sodium hydroxide, is then used ultra-pure water constant volume
To fluid nutrient medium is prepared in the conical flask of 1L by prepared culture medium, bottleneck is stoppered with cotton, is packed tightly with gauze, then uses tin
Foil paper encases, and cotton thread is fastened.Through 110 DEG C of high pressure sterilizations 30 minutes after being sealed.By the centrifuge tube of 3 10mL number 1-3 respectively,
Respectively represent blank group (without any processing)；Aquagel group；Chitosan/cordyceps sinensis hydrogel group；It will be in 4 DEG C of refrigerators
Escherichia coli (gramnegative bacterium) bacterium solution frozen is taken out, and in aseptic operating platform, draws 100 μ L bacterium solutions respectively, is added 3
Centrifuge tube.The fluid nutrient medium of 6mL is added in No. 1 centrifuge tube；1.0mL aquagels are added in No. 2 centrifuge tubes, add
The fluid nutrient medium of 5mL；The compound supramolecular hydrogel in the example 1 of 1.0mL is added in No. 3 centrifuge tubes, adds 5mL's
Fluid nutrient medium；It shakes up and is placed on 37 DEG C of Tempeerature-constant air concussion and cultivate case cultures 4 hours.3 Micro-Organism Culture Dish to sterilize are taken,
Number 1-3 respectively shakes up solid medium heating and melting, before cooling does not solidify, pours into 3 culture dishes respectively, each falls
20mL.10 μ L bacterium solutions are taken from centrifuge tube, are seeded to solid medium, are turned after substrate solidification, are placed in 37 DEG C
Take pictures, and obtains photo shown in Fig. 5 to form bacterium colony by observation, taking-up within 12 hours for the culture of Tempeerature-constant air concussion and cultivate case.
Embodiment 2
The 100 μ L of cordycepin solution in above-described embodiment 1 are taken, is added to clean drying and is protected from light the 2.0mL screw socket bottles of processing
In, 400 μ L PBS buffer solutions identical with 1 preparation method of embodiment are rapidly joined, are shaken up rapidly, 500 μ L is added and implements
The chitosan solution of the identical 40mg/mL of 1 preparation method of example is uniformly mixed under magnetic stirring apparatus.The screw socket bottle is put into -20
DEG C refrigerator freezing, at room temperature thaw can be obtained composite natural product supramolecular hydrogel.
Zoopery step：Select healthy male Sprague-Dawley rat (180~220g)
Manufacture rat full skin wound model is to study the composite natural product supramolecular hydrogel of the present invention to wound
The effect that mouth is cured.Entire zoopery process is completed in the Xiangya Medical College, Zhongnan Univ new camupus animal department of the Chinese Academy of Sciences.First by rat
It weighs, using pentobarbital (yellow Jackets 2%, 2ml/kg) intraperitoneal injection of anesthesia rat, is struck off with electric shaver-for women
The rat back hair anaesthetized, skin are sterilized with iodine complex solution clean before surgery.It is symmetrical in a rat back with mold
The circle of three a diameter of 1cm is drawn, then is assisted by tweezers, the circular wound of a diameter of 1cm is cut with surgical scissors, as shown in Figure 6.
Three wounds of every rat correspond to three groups：I groups are blank group (to wound without any processing), II groups are chitosan water-setting
Glue group (control group), III groups are compound supramolecular hydrogel group, every group of 5 rats.It is individually closed after processing into cage,
The food and water for providing equivalent, photograph to record, and raising 15 days is observed continuously, and replace bedding and padding, water and food daily and to mouse
Wound healing situation is photographed to record.It is observed after 15 days, obtains photo described in Fig. 7.Chitosan can be cooperateed with cordycepin to be made
With, can be applied in antiseptic and wound dressing, can achieve the purpose that enhance bactericidal property with promote wound healing.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest range caused.
Claims (9)
1. a kind of compound supramolecular hydrogel, which is characterized in that buffered including cordycepin solution, chitosan solution and PBS molten
Liquid.
2. compound supramolecular hydrogel according to claim 1, which is characterized in that the cordycepin solution it is a concentration of
100mg/mL。
3. compound supramolecular hydrogel according to claim 2, which is characterized in that the solvent of the chitosan solution is
1%HAc, a concentration of 20~40mg/L of the chitosan solution.
4. compound supramolecular hydrogel according to claim 1, which is characterized in that the solvent of the PBS buffer solutions
PH for ultra-pure water, the PBS buffer solutions is 8.3~8.5, each phosphate concn used is 0.1mol/L.
5. according to any compound supramolecular hydrogels of claim 1-4, which is characterized in that the compound supermolecule
Hydrogel is applied in antiseptic or/and wound dressing.
6. a kind of preparation method of any compound supramolecular hydrogels of claim 1-4, which is characterized in that including with
Lower step：
Step 1, the preparation of cordycepin solution；With dmso solution cordycepin solid powder, ultrasonic disperse obtains cordycepin
Solution；
Step 2, the preparation of chitosan solution；Chitosan is dissolved with 1%HAc, magnetic agitation matches shelling to accelerate chitosan to dissolve
Glycan solution；
Step 3, the preparation of PBS buffer solutions；Use Na2HPO4And NaH2PO4Solution allocation at different Ph PBS buffer solutions；
Step 4, after mixing by the cordycepin solution, chitosan solution and PBS buffer solutions, it is cold to be put into -20 DEG C of refrigerators
It places after freezing to fully charge and thaws at room temperature, form the compound supramolecular hydrogel.
7. the preparation method of compound supramolecular hydrogel according to claim 6, which is characterized in that described in step 1
Dmso solution cordycepin solid powder is 5~10min by the time of ultrasonic disperse, and gained cordycepin solution concentration is
100mg/mL carries out being protected from light processing during preparing the cordycepin solution.
8. the preparation method of compound supramolecular hydrogel according to claim 6, which is characterized in that described in step 2
A concentration of 20~40mg/ml of chitosan solution；In step 3, the Ph of the PBS buffer solutions is 8.3~8.5, and the PBS is slow
It rushes in solution, Na2HPO4 and NaH2PO4 concentration is 0.1mol/L.
9. the preparation method of compound supramolecular hydrogel according to claim 7, which is characterized in that step 4, take 80 μ L
The cordycepin solution of~100 μ L, which is added to the 2.0mL of clean drying, to be protected from light in the screw socket bottle of processing, rapidly join 400~
The PBS buffer solutions of 420 μ L, shake up rapidly, add the chitosan solution of 500 μ L, and the mixing for being made into 1.0mL is molten
The process for preparation of liquid, the mixed solution carries out under magnetic stirring；It waits for the mixed solution after mixing, screw socket bottle is put
Enter to place after -20 DEG C of refrigerator freezings to fully charge and thaw at room temperature, forms the compound supramolecular hydrogel.
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| CN112641995B (en) * | 2020-12-21 | 2021-11-23 | 上海交通大学 | Chiral hydrogel dressing with antibacterial and repair promoting functions and preparation method and application thereof |
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