CN116078175A - Carbon nitride-polydopamine-nano silver antibacterial composite membrane based on chitosan - Google Patents

Carbon nitride-polydopamine-nano silver antibacterial composite membrane based on chitosan Download PDF

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CN116078175A
CN116078175A CN202210774233.1A CN202210774233A CN116078175A CN 116078175 A CN116078175 A CN 116078175A CN 202210774233 A CN202210774233 A CN 202210774233A CN 116078175 A CN116078175 A CN 116078175A
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chitosan
polydopamine
carbon nitride
nano silver
composite membrane
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叶文鹏
欧阳小琨
王南
刘陈楠
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Zhejiang Ocean University ZJOU
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Zhejiang Ocean University ZJOU
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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
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    • A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
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    • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/42—Use of materials characterised by their function or physical properties
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    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
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Abstract

The invention relates to the technical field of medical materials, in particular to a chitosan-based carbon nitride-polydopamine-nano silver antibacterial composite membrane. The invention leads C to 3 N 4 Incorporation of the PDA-Ag complex into CS-based films to giveThe carbon nitride-polydopamine-nano silver antibacterial composite membrane based on chitosan has the dual functions of photocatalysis antibacterial and nano silver coordinated antibacterial, and compared with a simple CS film, the mechanical property and antibacterial property of the film are enhanced by adding the composite, and meanwhile, the composite membrane has good biocompatibility.

Description

Carbon nitride-polydopamine-nano silver antibacterial composite membrane based on chitosan
Technical Field
The invention relates to the technical field of medical materials, in particular to a chitosan-based carbon nitride-polydopamine-nano silver antibacterial composite membrane.
Background
Wound infections caused by pathogens are a challenge in the current treatment of wounds and promotion of their healing. Therefore, development of multifunctional materials having antibacterial activity is still required. At present, some membranes made of natural high molecular polysaccharides such as chitosan, sodium alginate and the like have low mechanical strength, poor oxygen permeability and water vapor permeability, and limited antibacterial performance.
Disclosure of Invention
In order to solve the problems in the prior art, on the one hand, the invention provides a preparation method of a chitosan-based carbon nitride-polydopamine-nano silver antibacterial composite film, which comprises the following steps:
(1)C 3 N 4 PDA complex preparation: will g-C 3 N 4 Adding with Dopamine (DA) into 10mM Tris solution (pH=8.5), reacting for 24 hr, centrifuging, and lyophilizing to obtain C 3 N 4 -PDA complex;
(2)C 3 N 4 preparation of the PDA-Ag complex: preparing a silver nitrate solution with a concentration of 50mM, adding ammonia water to the silver nitrate solution to obtain a silver ammonia solution, and carrying out C in the step (1) 3 N 4 Adding the PDA compound into the silver-ammonia solution, reacting for 3 hours at room temperature, centrifuging, and freeze-drying to obtain C 3 N 4 -a PDA-Ag complex;
(3) Preparation of a chitosan-based carbon nitride-polydopamine-nano silver antibacterial composite membrane: preparing 2% chitosan acetic acid-water solution (acetic acid concentration is 0.5M), adding C in step (2) 3 N 4 And (3) adding the PDA-Ag compound into 2% chitosan acetic acid-water solution, adding glycerol into the solution, stirring and reacting for 2 hours, pouring the mixture into a mould, and drying the mixture at 40 ℃ for 24 hours to obtain the chitosan-based carbon nitride-polydopamine-nano silver antibacterial composite film.
In some embodiments, g-C in step (1) 3 N 4 The weight ratio of the compound to Dopamine (DA) is 1:1.
in some embodiments, g-C in step (1) 3 N 4 The weight volume ratio of the solution to the Tris solution is 10 mg/ml: 5.
in some embodiments, the volume ratio of silver nitrate solution to ammonia water in step (2) is 100:1.
in some embodiments, C in step (3) 3 N 4 The weight ratio of the PDA-Ag compound to the chitosan in the 2% chitosan acetic acid-water solution is 0.5% -2.5%.
In some embodiments, the weight ratio of glycerol to 2% chitosan acetic acid-water solution in step (3) is 25%.
In some embodiments, the preparation step of the 2% chitosan acetic acid-water solution in the step (3) comprises preparing 0.5mol/L acetic acid solution, and adding chitosan to prepare the chitosan acetic acid-water solution with the mass concentration of 2%.
On the other hand, the invention provides the chitosan-based carbon nitride-polydopamine-nano silver antibacterial composite membrane prepared by the preparation method.
In still another aspect, the invention provides application of the chitosan-based carbon nitride-polydopamine-nano silver antibacterial composite film in a multifunctional material for wound healing.
Compared with the prior art, the invention leads to C 3 N 4 The PDA-Ag compound is introduced into the CS-based film to obtain the chitosan-based carbon nitride-polydopamine-nano silver antibacterial composite film, and the composite film has the dual functions of photocatalysis antibacterial and nano silver coordinated antibacterial, and compared with a pure CS film, the mechanical property and antibacterial property of the film are enhanced by adding the compound, and meanwhile, the composite film has good biocompatibility.
Drawings
FIG. 1 is DA, C 3 N 4 、C 3 N 4 -infrared spectrogram of PDA.
FIG. 2 is SEM (a) C 3 N 4 (b)C 3 N 4 -PDA(c)C 3 N 4 -PDA-Ag
FIG. 3 is a graph of the solubility and swelling of different membranes.
FIG. 4 (a) C in dark conditions 0 、C 1 、C 2 、C 3 Bacteriostatic action on Staphylococcus aureus (b) C under light conditions 0 、C 1 、C 2 、C 3 Antibacterial effect on Staphylococcus aureus.
FIG. 5 is a graph showing the effect of different membranes on the cytotoxic effect of L929.
FIG. 6 is a process for preparing a composite membrane of the present invention.
Detailed Description
The following examples serve to further illustrate the invention, but they do not constitute a limitation or limitation of the scope of the invention.
Example 1 different masses C 3 N 4 Preparation of CS film of PDA-Ag Complex
1)C 3 N 4 PDA complex preparation: will g-C 3 N 4 Adding the mixture with Dopamine (DA) according to the weight ratio of 100mg to 100mg into 50ml of 10mM Tris solution (pH=8.5), reacting for 24 hours, centrifuging, and freeze-drying to obtain C 3 N 4 -PDA complex;
2)C 3 N 4 preparation of the PDA-Ag complex: preparing a silver nitrate solution with a concentration of 50mM, taking 50ml of the silver nitrate solution, adding 500ul of ammonia water to the silver nitrate solution to obtain a silver ammonia solution, and adding 0.1. 0.1g C 3 N 4 Adding the PDA compound into the silver-ammonia solution, reacting for 3 hours at room temperature, centrifuging, and freeze-drying to obtain C 3 N 4 -a PDA-Ag complex;
3) Different mass C 3 N 4 CS membrane of PDA-Ag complex: preparing 2% chitosan acetic acid-water solution (acetic acid concentration of 0.5M), and collecting 0mg, 0.5mg, 1.5mg, and 2.5mg C 3 N 4 The PDA-Ag complex was added to 50mL of a 2% chitosan acetic acid-water solution, such that C 3 N 4 The mass ratio of the PDA-Ag compound to the chitosan is respectively 0 percent, 0.5 percent and 1.5 percentRespectively adding 25g of glycerol into the above solutions, stirring for 2h, pouring into a mold, drying at 40deg.C for 24h, soaking in 5% sodium hydroxide solution for 30min, washing with pure water, and standing at room temperature to form film to obtain CS group C with different mass fractions 3 N 4 Films of PDA-Ag, designated C 0 、C 1 、C 2 、C 3 。
Specific methods of fourier transform infrared analysis (FT-IR) characterization:
sample C was subjected to FT-IR (Tensor II, bruker, germany) 3 N 4 DA and C after lyophilization 3 N 4 PDA tabletting and sample preparation, recording 4000cm according to potassium bromide tabletting method -1 -400cm -1 Spectrum in the range, results are shown in fig. 1.
Specific methods of Scanning Electron Microscope (SEM) characterization:
c was observed with Zeiss Sigma500 type SEM (Merck, germany) at an accelerating voltage of 3kV 3 N 4 、C 3 N 4 -PDA、C 3 N 4 The surface morphology of PDA-Ag is shown in FIG. 2.
Characterization by FI-IR (FIG. 1), SEM (FIG. 2), etc., demonstrates C 3 N 4 The PDA-Ag complex has been synthesized. The results in fig. 1 show that: at C 3 N 4 In the infrared spectrum of the PDA, both C can be observed 3 N 4 (809.4cm -1 ) Is also observed for the characteristic peak of DA (3430.4 cm) -1 ) The results indicate C 3 N 4 PDA is synthesized. FIG. 2 (a) is C 3 N 4 In FIG. 2 (b), it can be observed that PDA particles are attached to C 3 N 4 The surface of FIG. 2 (c) has a portion of the PDA sphere attached to it, which has a more pronounced coating than in FIG. 2 (a). These results all indicate that: has successfully prepared C 3 N 4 -a PDA-Ag complex.
Example 2 swelling Property (W ws ) And solubility (W) sb ) Is (are) determined by
Will be of different mass C 3 N 4 CS film of PDA-Ag complex is dried to constantWeigh, weigh and record the initial dry weight (M 0 ). Soaking the film in deionized water at 25deg.C for 24 hr, taking out the film, wiping off the surface water with filter paper, and weighing (M 1 ). After drying at 40℃for 24h, the film was weighed and the final dry weight (M 2 ). Each sample was repeated three times. The result is calculated according to the following formula:
Figure BDA0003725976300000031
Figure BDA0003725976300000032
the results are shown in FIG. 3, and FIG. 3 is a graph showing the swelling and solubility of different membranes, which shows that: addition of C 3 N 4 After the PDA-Ag complex, the dissolution performance of the CS film is obviously reduced, and the swelling performance is slightly reduced due to C 3 N 4 The addition of the PDA-Ag complex makes the composite membrane more dense and sealed.
Example 3 different masses C 3 N 4 Antibacterial Property study of CS film of PDA-Ag Complex
Determination of CS-based C Using Staphylococcus aureus as model 3 N 4 Antibacterial Activity of the PDA-Ag composite film. The specific method comprises the following steps: the laboratory self-preserved staphylococcus aureus is revived and cultured until the bacterial growth phase. The bacterial liquid is diluted by turbidimetry. Diluted to a bacterial concentration of 1.0X10 6 CUF/mL, with C 0 、C 1 、C 2 、C 3 Mixing, and incubating in the dark for 1 hr or light for 15min, or incubating in the dark for 45min. After the incubation, 10. Mu.L of the bacterial liquid was plated and cultured in a constant temperature incubator for 24 hours. Each group was run 3 times in parallel, and the antibacterial ratio was calculated according to the following formula.
Figure BDA0003725976300000033
CFU 0 Represents the colony count of the control group, and CFU represents the colony count after incubation with different composite membranes.
The results are shown in fig. 4, and the study results indicate that: c (C) 1 、C 2 、C 3 The antibacterial rate to staphylococcus aureus is more than 80% under dark condition, the antibacterial rate to staphylococcus aureus can reach more than 90% under illumination condition, and the antibacterial activity is more than C 0 And (3) a film.
Example 4 different Mass C 3 N 4 CS Membrane in vitro biocompatibility study of PDA-Ag Complex
The toxic effect of the composite membrane on mouse fibroblasts (L929) was evaluated by MTT (tetramethylazo salt) method. L929 cells were grown at 2X 10 4 The cells/well were seeded in 96-well plates and incubated in a 37℃cell incubator for 24h. At the same time, C 0 、C 1 、C 2 、C 3 Incubating with cell culture medium for 24h to obtain sample leaching solution. After the cell culture was completed, the sample extract was diluted to a concentration of 200. Mu.g/mL, 20. Mu.L was added to a 96-well plate, and 20. Mu.L of medium was added to a control group, and the culture was again continued for 24 hours. After the completion of the incubation, the 96-well plate was removed, 20. Mu.L of MTT was added, the incubation was continued for 4 hours, and after removing the supernatant, 150. Mu.L of dimethyl sulfoxide (DMSO) was added, and the mixture was placed in an microplate reader to measure the OD at 490 nm. Cell viability was calculated by the following formula:
Figure BDA0003725976300000041
OD 1 represents the OD value at the point of addition to the leaching solution, OD 2 OD values representing the blank.
The results are shown in fig. 5, and the results indicate that: CS group C 3 N 4 C with different masses when the addition concentration of the PDA-Ag composite membrane is 200 mug/mL 3 N 4 The viability of CS membrane treated cells of the PDA-Ag complex was above 90%.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should be covered by the protection scope of the present invention by making equivalents and modifications to the technical solution and the inventive concept thereof.

Claims (9)

1. The preparation method of the chitosan-based carbon nitride-polydopamine-nano silver antibacterial composite membrane is characterized by comprising the following steps of:
(1)C 3 N 4 PDA complex preparation: will g-C 3 N 4 Adding with Dopamine (DA) into 10mM Tris solution (pH=8.5), reacting for 24 hr, centrifuging, and lyophilizing to obtain C 3 N 4 -PDA complex;
(2)C 3 N 4 preparation of the PDA-Ag complex: preparing a silver nitrate solution with a concentration of 50mM, adding ammonia water to the silver nitrate solution to obtain a silver ammonia solution, and carrying out C in the step (1) 3 N 4 Adding the PDA compound into the silver-ammonia solution, reacting for 3 hours at room temperature, centrifuging, and freeze-drying to obtain C 3 N 4 -a PDA-Ag complex;
(3) Preparation of a chitosan-based carbon nitride-polydopamine-nano silver antibacterial composite membrane: preparing 2% chitosan acetic acid-water solution (acetic acid concentration is 0.5M), adding C in step (2) 3 N 4 And (3) adding the PDA-Ag compound into 2% chitosan acetic acid-water solution, adding glycerol into the solution, stirring and reacting for 2 hours, pouring the mixture into a mould, and drying the mixture at 40 ℃ for 24 hours to obtain the chitosan-based carbon nitride-polydopamine-nano silver antibacterial composite film.
2. The method for preparing the chitosan-based carbon nitride-polydopamine-nano silver antibacterial composite membrane according to claim 1, wherein the step (1) is characterized in that the step (1) comprises the following steps of 3 N 4 The weight ratio of the compound to Dopamine (DA) is 1:1.
3. the method for preparing the chitosan-based carbon nitride-polydopamine-nano silver antibacterial composite membrane according to claim 1, wherein the step (1) is characterized in that the step (1) comprises the following steps of 3 N 4 Weight to volume ratio with Tris solutionThe ratio of mg/ml is 10:5.
4. the method for preparing the chitosan-based carbon nitride-polydopamine-nano silver antibacterial composite membrane according to claim 1, wherein the volume ratio of the silver nitrate solution to the ammonia water in the step (2) is 100:1.
5. the method for preparing a chitosan-based carbon nitride-polydopamine-nano silver antibacterial composite membrane according to claim 1, wherein in the step (3), C is as follows 3 N 4 The weight ratio of the PDA-Ag compound to the chitosan in the 2% chitosan acetic acid-water solution is 0.5% -2.5%.
6. The method for preparing the chitosan-based carbon nitride-polydopamine-nano silver antibacterial composite membrane according to claim 1, wherein the weight ratio of glycerin to 2% chitosan acetic acid-water solution in the step (3) is 25%.
7. The method for preparing the chitosan-based carbon nitride-polydopamine-nano silver antibacterial composite membrane according to claim 1, wherein the step (3) is characterized by comprising the following steps of: the preparation method comprises the steps of preparing 0.5mol/L acetic acid solution, and then adding chitosan to prepare the chitosan acetic acid-water solution with the mass concentration of 2%.
8. The chitosan-based carbon nitride-polydopamine-nano silver antibacterial composite membrane prepared by the preparation method according to any one of claims 1 to 7.
9. The use of the chitosan-based carbon nitride-polydopamine-nano silver antibacterial composite membrane according to claim 9 in multifunctional materials for wound healing.
CN202210774233.1A 2022-07-01 2022-07-01 Carbon nitride-polydopamine-nano silver antibacterial composite membrane based on chitosan Pending CN116078175A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115198393A (en) * 2022-07-19 2022-10-18 苏州大学 Preparation method and application of metal ion detection coaxial nanofiber
CN116510696A (en) * 2023-05-11 2023-08-01 新乡医学院 Hydrogel for adsorbing hemoglobin and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115198393A (en) * 2022-07-19 2022-10-18 苏州大学 Preparation method and application of metal ion detection coaxial nanofiber
CN115198393B (en) * 2022-07-19 2023-09-29 苏州大学 Preparation method and application of coaxial nanofiber for metal ion detection
CN116510696A (en) * 2023-05-11 2023-08-01 新乡医学院 Hydrogel for adsorbing hemoglobin and preparation method thereof

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