CN108786491B - Polydopamine/triclosan/titanium dioxide composite film and preparation method thereof - Google Patents
Polydopamine/triclosan/titanium dioxide composite film and preparation method thereof Download PDFInfo
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- CN108786491B CN108786491B CN201810558397.4A CN201810558397A CN108786491B CN 108786491 B CN108786491 B CN 108786491B CN 201810558397 A CN201810558397 A CN 201810558397A CN 108786491 B CN108786491 B CN 108786491B
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/58—Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
- B01D71/60—Polyamines
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2325/48—Antimicrobial properties
Abstract
The invention discloses a polydopamine/triclosan/titanium dioxide composite film and a preparation method thereof, belonging to the technical field of material surface modification. The preparation method is based on a mixed solvent method and an in-situ codeposition method, and comprises the steps of preparing dopamine-Tris buffer solution, triclosan-ethanol solution and titanium dioxide precursor sol, mixing the dopamine-Tris buffer solution with the triclosan-ethanol solution, adding the titanium dioxide precursor sol to form mixed solution, then putting a substrate into the mixed solution, soaking, taking out and drying to obtain the poly-dopamine/triclosan/titanium dioxide composite film. The film of the invention has simple preparation method and mild preparation environment, and the obtained film has good hydrophilicity, excellent biocompatibility, certain antibacterial property and certain improvement on the surface of the substrate, and can be applied to the biomedical engineering fields of in vitro cell culture, tissue engineering and the like.
Description
Technical Field
The invention belongs to the field of biomedical films, and particularly relates to a polydopamine/triclosan/titanium dioxide composite film and a preparation method thereof.
Background
The dopamine monomer isAn adhesion functional unit derived from mussel adhesion protein can be self-polymerized to form a film, has good adhesion, and a poly-dopamine (PDA) structure contains a large amount of phenolic hydroxyl and amino groups which can be used as a secondary reaction platform, so that the hydrophilicity and biocompatibility of the surface of an adhesion material can be greatly improved [ Crisp D J, Walker G, Young G A, et al].Journal of Colloid&Interface Science,1985,104(1):40-50.](ii) a Titanium dioxide is a nontoxic material with good biocompatibility and chemical stability, is widely used in the medical field and develops rapidly. The cell culture experiment result shows that the TiO2The coating has good biocompatibility [ Dieudone S C, Van den Dolder J, De Ruijter J E et al],2002,23(14):3041]And has no cytotoxicity.
In the practical application of biomedical materials, after the materials are implanted into a human body, inflammatory reaction and bacterial infection often occur, so the antibacterial property of the surface of the materials gradually becomes a research hotspot. Triclosan as one kind of efficient antiseptic disinfectant may be used in killing staphylococcus aureus, colibacillus and other bacteria and candida albicans and inhibiting virus, such as hepatitis B virus.
The solubility of the triclosan in water is extremely low (approximately equal to 4.62mg/L), and the triclosan can not adhere to the surface of the material, the binding force is extremely poor, and how to compound the triclosan on the surface of the material becomes a key point.
Disclosure of Invention
The invention aims to provide a polydopamine/triclosan/titanium dioxide composite film which has good hydrophilicity, simple preparation method and excellent biocompatibility and antibacterial property and a preparation method thereof.
The polydopamine/triclosan/titanium dioxide composite film is prepared by adopting a mixed solvent method to prepare polydopamine, triclosan and titanium dioxide on a substrate.
The substrate can be a rigid substrate such as quartz glass or a flexible substrate such as a PS substrate, and particularly, the method can also be applied to substrate materials with extremely low surface energy such as polytetrafluoroethylene.
The preparation method of the polydopamine/triclosan/titanium dioxide composite film comprises the following steps:
1) sequentially adding Tris and dopamine into deionized water to form a buffer solution, wherein the concentration of Tris is 8-12 mM, the concentration of dopamine is 1-3 g/L, and the pH value of the solution is adjusted to 8.5; preparing a triclosan-ethanol solution with the concentration of 1-3 g/L for later use;
2) mixing dopamine-Tris buffer solution and triclosan-ethanol solution, uniformly stirring by using magnetons, adding 8-12 mL of titanium dioxide sol, and continuously performing magnetic stirring to form mixed solution;
3) and (3) immersing the cleaned substrate into the mixed solution for 22-26 h, taking out the substrate, and drying to obtain the polydopamine/triclosan/titanium dioxide composite film.
The volume ratio of the added dopamine-Tris buffer solution to the triclosan-ethanol solution is 35: 2-35: 10, the prepared composite film has excellent biocompatibility and antibacterial performance, when the content of triclosan in the whole film system is low, the antibacterial performance of the film is difficult to meet the requirement, and when the content of triclosan is higher, the film has better antibacterial performance but poor biocompatibility.
The titanium dioxide sol is prepared by dispersing titanium dioxide nano particles in deionized water, wherein the concentration of the titanium dioxide nano particles is 0.5-1 mol/L.
The method adopts a mixed solvent method to mix dopamine-Tris buffer solution and triclosan-ethanol solution to form mixed solution, and adds titanium dioxide sol, wherein by utilizing the intersolubility of water and ethanol, the dopamine utilizes the self-polymerization film-forming property and the adhesiveness of polydopamine in the polymerization process to bond triclosan and titanium dioxide on the surface of a material, so that the polydopamine/triclosan/titanium dioxide composite film which is firmly combined with a substrate and has excellent biocompatibility and antibacterial property is obtained. The invention combines the adhesiveness of polydopamine, the high-efficiency antibacterial property of triclosan and the good biocompatibility and hydrophilicity of titanium dioxide, improves the hydrophilicity, cell compatibility and antibacterial property of the surface of the substrate, and ensures that cells are well adsorbed on the surface of the material. The method adopted by the invention is a mixed solvent method and an in-situ codeposition method, has low cost, mild preparation environment and simple operation, has certain modification effect on the substrate, and can be better applied to the biomedical engineering fields of in-vitro cell culture, tissue engineering and the like.
Drawings
FIG. 1 is an SEM photograph of a polydopamine/titanium dioxide composite film obtained on a polytetrafluoroethylene substrate in example 1.
FIG. 2 is an SEM photograph of the polydopamine/triclosan/titanium dioxide composite film obtained on the PTFE substrate in example 2.
FIG. 3 is a diagram showing the hydrophilicity changes of the PTFE substrate and the polydopamine/titanium dioxide film and the polydopamine/triclosan/titanium dioxide composite film prepared on the surface thereof before and after UV irradiation.
FIG. 4 shows OD values of the PTFE substrate and the fibroblasts cultured on the poly-dopamine/triclosan/titanium dioxide composite film prepared on the surface thereof after 1d and 3 d.
Detailed Description
The present invention will be described in detail with reference to the following examples and drawings, but the present invention is not limited thereto.
Example 1
1) Firstly, deionized water is used as a solvent, a certain amount of Tris with the concentration of 8mM is added into 200ml of deionized water, the pH value of the solution is adjusted to 8.5, and then 0.4g of dopamine is added into the solution to ensure that the concentration of the dopamine in the solution is 2g/L, so that dopamine-Tris buffer solution is obtained;
2) diluting titanium dioxide sol to 0.5mol/L by deionized water, adding 10ml of the diluted titanium dioxide sol into the deionized water, and stirring and mixing the solution uniformly by using magnetons;
3) and (3) immersing the cleaned polytetrafluoroethylene substrate in the solution for 22h, then taking out the polytetrafluoroethylene substrate, and placing the polytetrafluoroethylene substrate in a 60 ℃ oven for heat preservation for 1h to obtain the polydopamine/titanium dioxide composite film. The SEM image is shown in FIG. 1.
Example 2
1) Firstly, deionized water is used as a solvent, a certain amount of Tris with the concentration of 8mM is added into 200ml of deionized water, the pH value of the solution is adjusted to 8.5, and then 0.4g of dopamine is added into the solution to ensure that the concentration of the dopamine in the solution is 2g/L, so that dopamine-Tris buffer solution is obtained;
2) adding 0.2g of triclosan into 100ml of absolute ethyl alcohol to ensure that the concentration of the triclosan in the solution is 2g/L, respectively taking dopamine-Tris buffer solution and triclosan-ethyl alcohol solution, uniformly mixing the dopamine-Tris buffer solution and the triclosan-ethyl alcohol solution according to the volume ratio of 35:2 to ensure that the total volume is 100ml, then diluting titanium dioxide sol to 0.5mol/L by using deionized water, adding 10ml of titanium dioxide sol into the solution, and uniformly stirring and mixing by using magnetons;
3) and (3) immersing the cleaned polytetrafluoroethylene substrate in the solution for 22h, then taking out the polytetrafluoroethylene substrate, and placing the polytetrafluoroethylene substrate in a 60 ℃ oven for heat preservation for 1h to obtain the polydopamine/triclosan/titanium dioxide composite film. The SEM image is shown in FIG. 2.
Compared with the example 1, the surface appearance of the composite film after the trichloro is added is basically the same and the titanium dioxide nano particles are uniformly distributed in the SEM picture, and the film prepared by the method of the invention does not change the appearance basically, thereby being beneficial to the subsequent application.
Example 3
1) Firstly, deionized water is used as a solvent, a certain amount of Tris with the concentration of 8mM is added into 200ml of deionized water, the pH value of the solution is adjusted to 8.5, and then 0.4g of dopamine is added into the solution to ensure that the concentration of the dopamine in the solution is 2g/L, so that dopamine-Tris buffer solution is obtained;
2) adding 0.2g of triclosan into 100ml of absolute ethyl alcohol to ensure that the concentration of the triclosan in the solution is 2g/L, respectively taking dopamine-Tris buffer solution and triclosan-ethyl alcohol solution, uniformly mixing the dopamine-Tris buffer solution and the triclosan-ethyl alcohol solution according to the volume ratio of 35:6 to ensure that the total volume is 100ml, then diluting titanium dioxide sol to 0.5mol/L by using deionized water, adding 10ml of titanium dioxide sol into the solution, and uniformly stirring and mixing by using magnetons;
3) and (3) immersing the cleaned polytetrafluoroethylene substrate in the solution for 22h, then taking out the polytetrafluoroethylene substrate, and placing the polytetrafluoroethylene substrate in a 60 ℃ oven for heat preservation for 1h to obtain the polydopamine/triclosan/titanium dioxide composite film.
The samples obtained in this example were subjected to hydrophilicity tests before and after ultraviolet irradiation, and the results were compared with those obtained by subjecting the samples obtained in examples 1 and 2 to hydrophilicity tests before and after ultraviolet irradiation, to prepare a water contact angle change chart (see fig. 3). As can be seen from the figure, the hydrophilicity was improved to some extent by forming a film on a polytetrafluoroethylene substrate, and the resulting composite films all had the presence of titanium dioxide.
Example 4
1) Firstly, deionized water is used as a solvent, a certain amount of Tris with the concentration of 10mM is added into 200ml of deionized water, the pH value of the solution is adjusted to 8.5, and then 0.4g of dopamine is added into the solution to ensure that the concentration of the dopamine in the solution is 2g/L, so that dopamine-Tris buffer solution is obtained;
2) adding 0.2g of triclosan into 100ml of absolute ethyl alcohol to ensure that the concentration of the triclosan in the solution is 2g/L, respectively taking dopamine-Tris buffer solution and triclosan-ethyl alcohol solution, uniformly mixing the dopamine-Tris buffer solution and the triclosan-ethyl alcohol solution according to the volume ratio of 35:6 to ensure that the total volume is 100ml, then diluting titanium dioxide sol to 0.5mol/L by using deionized water, adding 10ml of titanium dioxide sol into the solution, and uniformly stirring and mixing by using magnetons;
3) and (3) immersing the cleaned polytetrafluoroethylene substrate in the solution for 24 hours, taking out the polytetrafluoroethylene substrate, and placing the polytetrafluoroethylene substrate in a 60-DEG C oven for heat preservation for 1 hour to obtain the polydopamine/triclosan/titanium dioxide composite film.
The membrane prepared in this example, the membrane prepared in example 8, and the teflon-based plate were cultured in vitro, and after culturing for 1d and 3d, the OD (optical density) was measured by CCK-8(Cell Counting Kit-8) method, and the OD of the membrane prepared in this example was significantly increased compared to the OD of the teflon-based plate (see fig. 4), indicating that the biocompatibility of the composite membrane prepared was improved to some extent compared to the substrate, and that the composite membrane has a certain modification effect on the substrate. The OD of the film obtained in example 8 was rather lower than that of the teflon-based plate, indicating that the film had poor biocompatibility although having good antibacterial properties when the triclosan content was too high.
Example 5
1) Firstly, deionized water is used as a solvent, a certain amount of Tris with the concentration of 10mM is added into 200ml of deionized water, the pH value of the solution is adjusted to 8.5, and then 0.2g of dopamine is added into the solution to ensure that the concentration of the dopamine in the solution is 1g/L, so that dopamine-Tris buffer solution is obtained;
2) adding 0.2g of triclosan into 100ml of absolute ethyl alcohol to ensure that the concentration of the triclosan in the solution is 2g/L, respectively taking dopamine-Tris buffer solution and triclosan-ethyl alcohol solution, uniformly mixing the dopamine-Tris buffer solution and the triclosan-ethyl alcohol solution according to the volume ratio of 35:8 to ensure that the total volume is 100ml, then diluting titanium dioxide sol to 0.8mol/L by using deionized water, adding 10ml of titanium dioxide sol into the solution, and uniformly stirring and mixing by using magnetons;
3) and (3) immersing the cleaned polytetrafluoroethylene substrate in the solution for 24 hours, taking out the polytetrafluoroethylene substrate, and placing the polytetrafluoroethylene substrate in a 60-DEG C oven for heat preservation for 1 hour to obtain the polydopamine/triclosan/titanium dioxide composite film.
Example 6
1) Firstly, deionized water is used as a solvent, a certain amount of Tris with the concentration of 12mM is added into 200ml of deionized water, the pH value of the solution is adjusted to 8.5, and then 0.6g of dopamine is added into the solution to ensure that the concentration of the dopamine in the solution is 3g/L, so that dopamine-Tris buffer solution is obtained;
2) adding 0.3g of triclosan into 100ml of absolute ethyl alcohol to ensure that the concentration of the triclosan in the solution is 3g/L, respectively taking dopamine-Tris buffer solution and triclosan-ethyl alcohol solution, uniformly mixing the dopamine-Tris buffer solution and the triclosan-ethyl alcohol solution according to the volume ratio of 35:10 to ensure that the total volume is 100ml, then diluting titanium dioxide sol to 1.0mol/L by using deionized water, adding 8ml of titanium dioxide sol into the solution, and uniformly stirring and mixing by using magnetons;
3) and (3) immersing the cleaned polytetrafluoroethylene substrate in the solution for 26h, then taking out the polytetrafluoroethylene substrate, and placing the polytetrafluoroethylene substrate in a 60 ℃ oven for heat preservation for 1h to obtain the polydopamine/triclosan/titanium dioxide composite film.
Example 7
1) Firstly, deionized water is used as a solvent, a certain amount of Tris with the concentration of 12mM is added into 200ml of deionized water, the pH value of the solution is adjusted to 8.5, and then 0.4g of dopamine is added into the solution to ensure that the concentration of the dopamine in the solution is 2g/L, so that dopamine-Tris buffer solution is obtained;
2) adding 0.1g of triclosan into 100ml of absolute ethyl alcohol to ensure that the concentration of the triclosan in the solution is 1g/L, respectively taking dopamine-Tris buffer solution and triclosan-ethyl alcohol solution, uniformly mixing the dopamine-Tris buffer solution and the triclosan-ethyl alcohol solution according to the volume ratio of 35:10 to ensure that the total volume is 100ml, then diluting titanium dioxide sol to 0.8mol/L by using deionized water, adding 12ml of titanium dioxide sol into the solution, and uniformly stirring and mixing by using magnetons;
3) and (3) immersing the cleaned polytetrafluoroethylene substrate in the solution for 22h, then taking out the polytetrafluoroethylene substrate, and placing the polytetrafluoroethylene substrate in a 60 ℃ oven for heat preservation for 1h to obtain the polydopamine/triclosan/titanium dioxide composite film.
Example 8
1) Firstly, deionized water is used as a solvent, a certain amount of Tris with the concentration of 12mM is added into 200ml of deionized water, the pH value of the solution is adjusted to 8.5, and then 0.4g of dopamine is added into the solution to ensure that the concentration of the dopamine in the solution is 2g/L, so that dopamine-Tris buffer solution is obtained;
2) adding 0.1g of triclosan into 100ml of absolute ethyl alcohol to ensure that the concentration of the triclosan in the solution is 1g/L, respectively taking dopamine-Tris buffer solution and triclosan-ethyl alcohol solution, uniformly mixing the dopamine-Tris buffer solution and the triclosan-ethyl alcohol solution according to the volume ratio of 35:12 to ensure that the total volume is 100ml, then diluting titanium dioxide sol to 0.8mol/L by using deionized water, adding 12ml of titanium dioxide sol, and uniformly stirring and mixing by using magnetons;
3) and (3) immersing the cleaned polytetrafluoroethylene substrate in the solution for 22h, then taking out the polytetrafluoroethylene substrate, and placing the polytetrafluoroethylene substrate in a 60 ℃ oven for heat preservation for 1h to obtain the polydopamine/triclosan/titanium dioxide composite film.
Example 9
1) Firstly, absolute ethyl alcohol is used as a solvent, a certain amount of Tris with the concentration of 12mM is added into 200ml of ethyl alcohol, the pH value of the solution is adjusted to 8.5, and then 0.4g of dopamine is added into the solution to obtain a dopamine-Tris buffer solution;
2) adding 0.1g of triclosan into 100ml of absolute ethanol to ensure that the concentration of the triclosan in the solution is 1g/L, respectively taking a dopamine-Tris ethanol solution and a triclosan-ethanol solution, uniformly mixing the dopamine-Tris ethanol solution and the triclosan-ethanol solution according to the volume ratio of 35:12 to ensure that the total volume is 100ml, then diluting titanium dioxide sol to 0.8mol/L by using deionized water, adding 12ml of the diluted titanium dioxide sol, and uniformly stirring and mixing by using magnetons;
3) the cleaned polytetrafluoroethylene substrate is immersed in the solution for 22 hours, then taken out, and placed in an oven at 60 ℃ for heat preservation for 1 hour.
In this example, it was found that dopamine cannot self-polymerize to form a film, and the desired polydopamine/triclosan/titanium dioxide composite film cannot be obtained after immersing the substrate in ethanol alone. And the water is adopted as the solvent alone, but the triclosan cannot be adhered to the surface of the material due to the extremely low solubility of the triclosan in the water, and the binding force is extremely poor. The method adopts a mixed solvent method to mix dopamine-Tris buffer solution and triclosan-ethanol solution to form mixed solution, and adds titanium dioxide sol, utilizes the intersolubility of water and ethanol to uniformly disperse triclosan, and bonds triclosan and titanium dioxide on the surface of a material through the self-polymerization film-forming property and the adhesion of polydopamine to obtain the polydopamine/triclosan/titanium dioxide composite film which is firmly combined with a substrate and has excellent biocompatibility and antibacterial property.
Claims (3)
1. A preparation method of a polydopamine/triclosan/titanium dioxide composite film is characterized in that the polydopamine, triclosan and titanium dioxide are prepared on a substrate by adopting a mixed solvent method, and the preparation method comprises the following steps:
1) sequentially adding Tris and dopamine into deionized water to form a buffer solution, wherein the concentration of Tris is 8-12 mM, the concentration of dopamine is 1-3 g/L, and the pH value of the solution is adjusted to 8.5; preparing a triclosan-ethanol solution with the concentration of 1-3 g/L for later use;
2) mixing dopamine-Tris buffer solution and triclosan-ethanol solution, uniformly stirring by using magnetons, adding 8-12 mL of titanium dioxide sol, and continuously performing magnetic stirring to form mixed solution;
3) immersing the cleaned substrate into the mixed solution for 22-26 h, taking out the substrate, and drying to obtain a polydopamine/triclosan/titanium dioxide composite film;
the titanium dioxide sol is prepared by dispersing titanium dioxide nano particles in deionized water, wherein the concentration is 0.5-1 mol/L.
2. The method for preparing polydopamine/triclosan/titanium dioxide composite film according to claim 1, wherein the substrate is polytetrafluoroethylene, a PS substrate or quartz glass.
3. The preparation method of the polydopamine/triclosan/titanium dioxide composite film according to claim 1, wherein the volume ratio of the added dopamine-Tris buffer solution to the triclosan-ethanol solution is 35: 2-35: 10.
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| CN106800375A (en) * | 2017-01-24 | 2017-06-06 | 厦门大学 | TiO2Modify the preparation method of dopamine antimicrobial coating |
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