CN102671240A - Method for preparing multifunctional antibacterial chitosan stable gel coat - Google Patents

Method for preparing multifunctional antibacterial chitosan stable gel coat Download PDF

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Publication number
CN102671240A
CN102671240A CN2012101534952A CN201210153495A CN102671240A CN 102671240 A CN102671240 A CN 102671240A CN 2012101534952 A CN2012101534952 A CN 2012101534952A CN 201210153495 A CN201210153495 A CN 201210153495A CN 102671240 A CN102671240 A CN 102671240A
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coating
mass concentration
base material
stable gel
chitosan
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计剑
王佰亮
江辉平
冯永敏
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ZHEJIANG SHUGUANG TECHNOLOGY Co Ltd
Zhejiang University ZJU
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ZHEJIANG SHUGUANG TECHNOLOGY Co Ltd
Zhejiang University ZJU
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Abstract

The invention discloses a method for preparing a multifunctional antibacterial chitosan stable gel coat. The method is characterized in that the stable gel coat which is provided with a hydrophilic surface and is stable in a water environment is obtained by using a solution of chitosan and polyvinylpyrrolidone through physical coating and base material pretreatment. The coat has good capacity of resisting gram-positive bacteria and gram-negative bacteria adhesion and killing the bacteria. The method is simple and rapid in process, mild in condition and wide in application range, can be easily and industrially implemented in the manner of spin coating, dip coating and spray coating, and can be used for effectively improving the antimicrobial property, the biocompatibility and the lubricity of the surface of a medical device.

Description

A kind of multifunctional antibiotic chitosan stable gel coating production
Technical field
The present invention relates to a kind of multifunctional antibiotic chitosan stable gel coating production.
Background technology
Along with material science, medical science, biological develop rapidly, the research of bio-medical material has been made significant headway, but still faces various challenges; The problem of some essence does not solve; Wherein, except biocompatibility issues, the major obstacle that biomaterial is used also has infection problems.In the world, it is microbial by sticking cause of disease on implant or the medical apparatus and instruments that about 64% hospital acquired infects, and only in the U.S., annual just have 100,000 people to die from relevant infection.In Europe, people will spend 5,000 ten thousand about every year and be used for the treatment that medical catheter infects, and have every year 5000 to infect death.The general process that infect to take place is: the sticking of antibacterial; Field planting and breeding form bacterium colony; The secretion extracellular matrix, bacterium colony links together through extracellular matrix, forms biomembrane (biofilm), and biomembrane discharges swim thalline and toxin, causes and infects.Biomembrane makes antibacterial develop immunity to drugs easily; Biomembrane is because its fine and close physical arrangement; Can prevent the phagocytosis of macrophage among the human immune system, experiment confirm, the antibacterial resistivity that the antibacterial in biomembrane is compared free state has increased by 1000 times.Through finishing, under the condition that keeps original performance, improve the biomedical devices biocompatibility and become the major issue in the application of modern medical service device various medical apparatus.
The surface that can anti-biotic material be divided into the adherent surface of antibacterium, the germ-resistant surface of contact and delivery of antimicrobials according to antimicrobial surface and interfacial property; The coating of anti-adhesive can play a role to the initial step of bacterial infection, but this simple type coating does not have germ-resistant function; Contact antibacterial surface comprises kinds such as grafting quaternary ammonium salt, quaternary phosphonium hydrochlorate, pyridiniujm, and the advantage of this type antimicrobial surface is that coating is firm, antibacterial ability is strong, but the problem that exists is that cytotoxicity is bigger, and biocompatibility property is relatively poor.Bactericide-release type surface can be carried out the part and discharged and administration, discharges nanometer silver, antibiotic, antibacterial peptide, lysozyme, NO molecule etc.This type coating has certain slow release and antibacterial ability, but does not have the adherent ability of antibacterium.Therefore seek the critical problem that a kind of simple finishing means in the face of device become medical apparatus infection surface design.And the polyblend technology has simply, the characteristics of easy operating, and makes rete have the complex function of its component, has solved the stability problem that swelling of paint coating brings through the pretreatment to base material, is expected to obtain having concurrently antibacterium and sticks and germ-resistant performance.
Summary of the invention
The purpose of this invention is to provide a kind of multifunctional antibiotic chitosan stable gel coating production.
The step of multifunctional antibiotic chitosan stable gel coating production is following:
1) chooses glass, quartz, Muscovitum, rustless steel, polyester film, polylactic acid membrane as base material; Base material at first, mass concentration is soaked 0.5-12h in being the PEI of 0.1-20mg/ml; Be the polyacrylic acid immersion 0.5-12h of 0.1-20mg/ml then in mass concentration; In mass concentration is the mixed liquor of N_ ethyl _ N ' _ (3_ dimethylamino) the propyl carbodiimide diimine hydrochloric acid of 1-20mg/ml and the N_ HOSu NHS that mass concentration is 2-40mg/ml, soak 2-12h again, the pH value of mixed liquor is 5.6;
2) be that the chitosan of 5-20 mg/ml and polyvinylpyrrolidonesolution solution mixed solution that mass concentration is 1-20mg/ml are coated on the substrate surface as the mode of coating liquid with spin coating, dip-coating or spraying with mass concentration; Handle 12h and vacuum drying treatment 12h through natural drying, obtain multifunctional antibiotic chitosan stable gel coating.
Described a kind of multifunctional antibiotic chitosan stable gel coating production is characterized in that the method that described mode with spin coating is coated on the substrate surface is: start the spin coating appearance; Rotating speed is 1000rad/min; Draw the 0.1ml coating liquid with dropper and drop on the base material spin coating 10s, spin coating 2min under 2500rad/min then; Drying repeats spin coating 3-5 time
Described a kind of multifunctional antibiotic chitosan stable gel coating production; It is characterized in that the method that described mode with dip-coating is coated on the substrate surface is: clamp base material with tweezers, immerse 5s in the coating liquid; Take out; The liquid on surface is evenly covered, be positioned over then on the glass plate, base material is peeled off with blade in dry back.
Described a kind of multifunctional antibiotic chitosan stable gel coating production; It is characterized in that the described method that is coated on the substrate surface with the mode of spraying is: spray coating liquor is joined in the nebulizer, be sprayed on 1s on the base material; 60 ℃ of oven drying 20min, this operation repetition 5 times.
Coating solution simple and convenient preparation of the present invention can realize pollution-free operation, but can adopt the mode of industrial realization such as spin coating, dip-coating, spraying, and is applied widely, can carry out coating modifying to the biomedical devices with complex shape structure; Coating can be improved the anti-microbial property of medical device surface, lubricity, and biocompatibility, the form with hydrogel under the human body environment exists, and this character makes biomaterial surface lubricated, reduces rubbing between material surface and the mucosal tissue and connects resistance; The coating material steady chemical structure, endurance, shearing can adapt to the interior environment of human body; Coating can realize the ability of broad-spectrum multifunctional antibiotic.
The specific embodiment
The step of multifunctional antibiotic chitosan stable gel coating production is following:
1) chooses glass, quartz, Muscovitum, rustless steel, polyester film, polylactic acid membrane as base material; Base material at first, mass concentration is soaked 0.5-12h in being the PEI of 0.1-20mg/ml; Be the polyacrylic acid immersion 0.5-12h of 0.1-20mg/ml then in mass concentration; In mass concentration is the mixed liquor of N_ ethyl _ N ' _ (3_ dimethylamino) the propyl carbodiimide diimine hydrochloric acid of 1-20mg/ml and the N_ HOSu NHS that mass concentration is 2-40mg/ml, soak 2-12h again, the pH value of mixed liquor is 5.6;
2) be that the chitosan of 5-20 mg/ml and polyvinylpyrrolidonesolution solution mixed solution that mass concentration is 1-20mg/ml are coated on the substrate surface as the mode of coating liquid with spin coating, dip-coating or spraying with mass concentration; Handle 12h and vacuum drying treatment 12h through natural drying, obtain multifunctional antibiotic chitosan stable gel coating.
Described a kind of multifunctional antibiotic chitosan stable gel coating production is characterized in that the method that described mode with spin coating is coated on the substrate surface is: start the spin coating appearance; Rotating speed is 1000rad/min; Draw the 0.1ml coating liquid with dropper and drop on the base material spin coating 10s, spin coating 2min under 2500rad/min then; Drying repeats spin coating 3-5 time.
Described a kind of multifunctional antibiotic chitosan stable gel coating production; It is characterized in that the method that described mode with dip-coating is coated on the substrate surface is: clamp base material with tweezers, immerse 5s in the coating liquid; Take out; The liquid on surface is evenly covered, be positioned over then on the glass plate, base material is peeled off with blade in dry back.
Described a kind of multifunctional antibiotic chitosan stable gel coating production; It is characterized in that the described method that is coated on the substrate surface with the mode of spraying is: spray coating liquor is joined in the nebulizer, be sprayed on 1s on the base material; At 60 ℃ of oven drying 20min, this operation repetition 5 times.
Embodiment 1
1) chooses glass as base material; Glass at first, mass concentration is soaked 0.5h in being the PEI of 0.1mg/ml; Be the polyacrylic acid immersion 0.5h of 0.1mg/ml then in mass concentration; In mass concentration is the mixed liquor of N_ ethyl _ N ' _ (3_ dimethylamino) the propyl carbodiimide diimine hydrochloric acid of 1mg/ml and the N_ HOSu NHS that mass concentration is 2mg/ml, soak 2h again, the pH value of mixed liquor is 5.6;
2) be that the chitosan of 5 mg/ml and polyvinylpyrrolidonesolution solution mixed solution that mass concentration is 1mg/ml are as coating liquid with mass concentration; Spray coating liquor is joined in the nebulizer; Be sprayed on 1s on the base material, at 60 ℃ of oven drying 20min, this operation repetition 5 times; Handle 12h and vacuum drying treatment 12h through natural drying, obtain multifunctional antibiotic chitosan stable gel coating.
Static contact angle discovers that the back hydrophilic of filming significantly increases, and compares with simple CHI film, reduces to 56.52 ± 1.29 ° by 79.45 ± 0.63 °, and atomic force microscope observation pattern table of discovery mask has very low roughness, and RMS is 2.57 ± 0.22 nm.Shake-flask culture and dilution are coated with the bactericidal property of flat band method test rete, and the result shows that this rete can kill 91% escherichia coli and 98% staphylococcus aureus at 24 h.
Embodiment 2
1) chooses quartz as base material; Quartz at first, mass concentration is soaked 12h in being the PEI of 20mg/ml; Be the polyacrylic acid immersion 12h of 20mg/ml then in mass concentration; In mass concentration is the mixed liquor of N_ ethyl _ N ' _ (3_ dimethylamino) the propyl carbodiimide diimine hydrochloric acid of 20mg/ml and the N_ HOSu NHS that mass concentration is 40mg/ml, soak 12h again, the pH value of mixed liquor is 5.6;
2) with mass concentration be the chitosan of 20 mg/ml and polyvinylpyrrolidonesolution solution mixed solution that mass concentration is 20mg/ml as coating liquid, clamp quartz with tweezers, immerse 5s in the coating liquid; Take out; The liquid of quartz surfaces is evenly covered, be positioned over then on the glass plate, handle 12h and vacuum drying treatment 12h through natural drying; Peel off base material with blade then, obtain multifunctional antibiotic chitosan stable gel coating.
Shake-flask culture and dilution are coated with the bactericidal property of flat band method test rete, and the result shows that this rete can kill 94% escherichia coli and 100% staphylococcus aureus at 24 h.Antibacterium stick experiment find with do not film base material compare, this blend film has reduced by 88% escherichia coli and has sticked and the sticking of 97% staphylococcus aureus.
Embodiment 3:
1) chooses polyester film as base material; Polyester film at first, mass concentration is soaked 12h in being the PEI of 0.1mg/ml; Be the polyacrylic acid immersion 12h of 0.1mg/ml then in mass concentration; In mass concentration is the mixed liquor of N_ ethyl _ N ' _ (3_ dimethylamino) the propyl carbodiimide diimine hydrochloric acid of 1mg/ml and the N_ HOSu NHS that mass concentration is 2mg/ml, soak 12h again, the pH value of mixed liquor is 5.6;
2) be that the chitosan of 10 mg/ml and polyvinylpyrrolidonesolution solution mixed solution that mass concentration is 1mg/ml are as spray coating liquor with mass concentration; Spray coating liquor is joined in the nebulizer; Be sprayed on 1s on the base material, at 60 ℃ of oven drying 20min, this operation repetition 5 times; Handle 12h and vacuum drying treatment 12h through natural drying, obtain multifunctional antibiotic chitosan stable gel coating.
Polyester film and through PEI; PAA and EDC/NHS handle the back contact angle and are respectively 70.3 ± 0.5 °, and 80.6 ± 0.4 °, 25.1 ± 0.8 ° and 37.2 ± 0.7 °; The AFM test RMS is respectively 2.992 ± 0.42; 2.732 ± 0.32,3.538 ± 0.28 and 3.446 ± 0.26nm, confirmed the carrying out of preprocessing process.The thickness of section field emission scanning electron microscope testing coating is 3.34 ± 0.48 μ m.Static contact angle discovers that the back hydrophilic of filming significantly increases, and compares with simple CHI film, reduces to 76.32 ± 1.24 ° by 79.45 ± 0.63 °, and atomic force microscope observation pattern table of discovery mask has very low roughness, and RMS is 3.27 ± 0.32 nm.Shake-flask culture and dilution are coated with the bactericidal property of flat band method test rete, and the result shows that this rete can kill 92% escherichia coli and 100% staphylococcus aureus at 24 h.
Embodiment 4:
1) chooses polylactic acid membrane as base material; Polylactic acid membrane at first, mass concentration is soaked 10h in being the PEI of 1mg/ml; Be the polyacrylic acid immersion 10h of 1mg/ml then in mass concentration; In mass concentration is the mixed liquor of N_ ethyl _ N ' _ (3_ dimethylamino) the propyl carbodiimide diimine hydrochloric acid of 3mg/ml and the N_ HOSu NHS that mass concentration is 6mg/ml, soak 10h again, the pH value of mixed liquor is 5.6;
2) be that the chitosan of 5 mg/ml and polyvinylpyrrolidonesolution solution mixed solution that mass concentration is 2mg/ml are as coating liquid with mass concentration; Clamp quartz with tweezers, immerse 5s in the coating liquid, take out; The liquid of quartz surfaces is evenly covered; Be positioned over then on the glass plate, handle 12h and vacuum drying treatment 12h, obtain multifunctional antibiotic chitosan stable gel coating through natural drying.
Static contact angle test rete demonstrates certain hydrophilic, is 70.43 ± 1.23 °, and atomic force microscope observation pattern table of discovery mask has very low roughness, and RMS is 3.52 ± 0.24 nm.Shake-flask culture and dilution are coated with the bactericidal property of flat band method test rete, and the result shows that this rete can kill 90% escherichia coli and 100% staphylococcus aureus at 24 h.Antibacterium stick experiment find with do not film base material compare, this blend film has reduced by 79% escherichia coli and has sticked and the sticking of 92% staphylococcus aureus.
Embodiment 5:
1) chooses glass as base material; Glass at first, mass concentration is soaked 7h in being the PEI of 3mg/ml; Be the polyacrylic acid immersion 7h of 3mg/ml then in mass concentration; In mass concentration is the mixed liquor of N_ ethyl _ N ' _ (3_ dimethylamino) the propyl carbodiimide diimine hydrochloric acid of 5mg/ml and the N_ HOSu NHS that mass concentration is 10mg/ml, soak 7h again, the pH value of mixed liquor is 5.6;
2) with mass concentration be the chitosan of 10 mg/ml and polyvinylpyrrolidonesolution solution mixed solution that mass concentration is 5mg/ml as spin coating liquid, start the spin coating appearance, rotating speed is 1000rad/min; Draw the 0.1ml coating liquid with dropper and drop on the base material spin coating 10s, spin coating 2min under 2500rad/min then; Dry; Repeat spin coating 3-5 time, handle 12h and vacuum drying treatment 12h, obtain multifunctional antibiotic chitosan stable gel coating through natural drying.
The thickness of section field emission scanning electron microscope test rete is 2.45 ± 0.38 μ m.Static contact angle test rete demonstrates certain hydrophilic, is 65.67 ± 1.32 °, and atomic force microscope observation pattern table of discovery mask has very low roughness, and RMS is 2.44 ± 0.26 nm.Shake-flask culture and dilution are coated with the bactericidal property of flat band method test rete, and the result shows that this rete can kill 94% escherichia coli and 100% staphylococcus aureus at 24 h.Antibacterium stick experiment find with do not film base material compare, this blend film has reduced by 82% escherichia coli and has sticked and the sticking of 97% staphylococcus aureus.
Embodiment 6:
1) chooses Muscovitum as base material; Muscovitum at first, mass concentration is soaked 5h in being the PEI of 5mg/ml; Be the polyacrylic acid immersion 5h of 5mg/ml then in mass concentration; In mass concentration is the mixed liquor of N_ ethyl _ N ' _ (3_ dimethylamino) the propyl carbodiimide diimine hydrochloric acid of 8mg/ml and the N_ HOSu NHS that mass concentration is 16mg/ml, soak 5h again, the pH value of mixed liquor is 5.6;
2) be that the chitosan of 2 mg/ml and polyvinylpyrrolidonesolution solution mixed solution that mass concentration is 10mg/ml are as spray coating liquor with mass concentration; Spray coating liquor is joined in the nebulizer; Be sprayed on 1s on the base material, at 60 ℃ of oven drying 20min, this operation repetition 5 times; Handle 12h and vacuum drying treatment 12h through natural drying, obtain multifunctional antibiotic chitosan stable gel coating.
The thickness of section field emission scanning electron microscope test rete is 4.45 ± 0.52 μ m.Static contact angle test rete demonstrates certain hydrophilic, is 57.45 ± 1.24 °, and atomic force microscope observation pattern table of discovery mask has very low roughness, and RMS is 2.45 ± 0.23 nm.Shake-flask culture and dilution are coated with the bactericidal property of flat band method test rete, and the result shows that this rete can kill 93% escherichia coli and 100% staphylococcus aureus at 24 h.Antibacterium stick experiment find with do not film base material compare, this blend film has reduced by 88% escherichia coli and has sticked and the sticking of 92% staphylococcus aureus.
Embodiment 7:
1) chooses rustless steel as base material; Rustless steel at first, mass concentration is soaked 3h in being the PEI of 10mg/ml; Be the polyacrylic acid immersion 3h of 10mg/ml then in mass concentration; In mass concentration is the mixed liquor of N_ ethyl _ N ' _ (3_ dimethylamino) the propyl carbodiimide diimine hydrochloric acid of 10mg/ml and the N_ HOSu NHS that mass concentration is 20mg/ml, soak 5h again, the pH value of mixed liquor is 5.6;
2) be that the chitosan of 5mg/ml and polyvinylpyrrolidonesolution solution mixed solution that mass concentration is 15mg/ml are as spray coating liquor with mass concentration; Spray coating liquor is joined in the nebulizer; Be sprayed on 1s on the base material, at 60 ℃ of oven drying 20min, this operation repetition 5 times; Handle 12h and vacuum drying treatment 12h through natural drying, obtain multifunctional antibiotic chitosan stable gel coating.
The thickness of section field emission scanning electron microscope test rete is 2.65 ± 0.32 μ m.Static contact angle test rete demonstrates certain hydrophilic, is 47.54 ± 1.53 °, and atomic force microscope observation pattern table of discovery mask has very low roughness, and RMS is 1.85 ± 0.33 nm.Shake-flask culture and dilution are coated with the bactericidal property of flat band method test rete, and the result shows that this rete can kill 76% escherichia coli and 98% staphylococcus aureus at 24 h.Antibacterium stick experiment find with do not film base material compare, this blend film has reduced by 94% escherichia coli and has sticked and the sticking of 97% staphylococcus aureus.
Embodiment 8:
1) chooses Muscovitum as base material; Muscovitum at first, mass concentration is soaked 1.5h in being the PEI of 15mg/ml; Be the polyacrylic acid immersion 1.5h of 15mg/ml then in mass concentration; In mass concentration is the mixed liquor of N_ ethyl _ N ' _ (3_ dimethylamino) the propyl carbodiimide diimine hydrochloric acid of 10mg/ml and the N_ HOSu NHS that mass concentration is 20mg/ml, soak 3h again, the pH value of mixed liquor is 5.6;
2) with mass concentration be the chitosan of 20 mg/ml and polyvinylpyrrolidonesolution solution mixed solution that mass concentration is 20mg/ml as spin coating liquid, start the spin coating appearance, rotating speed is 1000rad/min; Draw the 0.1ml coating liquid with dropper and drop on the base material spin coating 10s, spin coating 2min under 2500rad/min then; Dry; Repeat spin coating 3-5 time, handle 12h and vacuum drying treatment 12h, obtain multifunctional antibiotic chitosan stable gel coating through natural drying.
Static contact angle test rete demonstrates certain hydrophilic, is 65.45 ± 2.14 °, and atomic force microscope observation pattern table of discovery mask has very low roughness, and RMS is 4.23 ± 0.54 nm.Shake-flask culture and dilution are coated with the bactericidal property of flat band method test rete, and the result shows that this rete can kill 93% escherichia coli and 100% staphylococcus aureus at 24 h.Antibacterium stick experiment find with do not film base material compare, this blend film has reduced by 88% escherichia coli and has sticked and the sticking of 92% staphylococcus aureus.
Embodiment 9:
1) chooses quartz as base material; Quartz at first, mass concentration is soaked 1h in being the PEI of 17mg/ml; Be the polyacrylic acid immersion 1h of 17mg/ml then in mass concentration; In mass concentration is the mixed liquor of N_ ethyl _ N ' _ (3_ dimethylamino) the propyl carbodiimide diimine hydrochloric acid of 15mg/ml and the N_ HOSu NHS that mass concentration is 30mg/ml, soak 2h again, the pH value of mixed liquor is 5.6;
2) be that the chitosan of 12 mg/ml and polyvinylpyrrolidonesolution solution mixed solution that mass concentration is 9mg/ml are as coating liquid with mass concentration; Clamp quartz with tweezers, immerse 5s in the coating liquid, take out; The liquid of quartz surfaces is evenly covered; Be positioned over then on the glass plate, handle 12h and vacuum drying treatment 12h, obtain multifunctional antibiotic chitosan stable gel coating through natural drying.
The thickness of section field emission scanning electron microscope test rete is 4.24 ± 0.52 μ m.Static contact angle test rete demonstrates certain hydrophilic, is 57.45 ± 2.34 °, and atomic force microscope observation pattern table of discovery mask has very low roughness, and RMS is 3.53 ± 0.43 nm.It is lower to the Human umbilical vein endothelial cells cytotoxicity to adopt MTT and FDA experimental result to find, cytoactive surpasses 80% of TCPS, therefore has the good cell compatibility.
Embodiment 10:
1) chooses rustless steel as base material; Rustless steel at first, mass concentration is soaked 0.5h in being the PEI of 20mg/ml; Be the polyacrylic acid immersion 0.5h of 20mg/ml then in mass concentration; In mass concentration is the mixed liquor of N_ ethyl _ N ' _ (3_ dimethylamino) the propyl carbodiimide diimine hydrochloric acid of 20mg/ml and the N_ HOSu NHS that mass concentration is 40mg/ml, soak 2h again, the pH value of mixed liquor is 5.6;
2) be that the chitosan of 11 mg/ml and polyvinylpyrrolidonesolution solution mixed solution that mass concentration is 11mg/ml are as coating liquid with mass concentration; Clamp quartz with tweezers, immerse 5s in the coating liquid, take out; The liquid of quartz surfaces is evenly covered; Be positioned over then on the glass plate, handle 12h and vacuum drying treatment 12h, obtain multifunctional antibiotic chitosan stable gel coating through natural drying.
The thickness of section field emission scanning electron microscope test rete is 3.84 ± 0.32 μ m.Static contact angle test rete demonstrates certain hydrophilic, is 54.45 ± 2.04 °, and atomic force microscope observation pattern table of discovery mask has very low roughness, and RMS is 2.53 ± 0.23 nm.This coating is soaked 24h in PBS, use emission scan electron microscopic observation section is found this even film layer and stable existence in silicon chip surface, shows that pretreatment has improved the adhesive property of rete.It is lower to the Human umbilical vein endothelial cells cytotoxicity to adopt MTT and FDA experimental result to find, cytoactive surpasses 85% of TCPS, therefore has the good cell compatibility.

Claims (4)

1. multifunctional antibiotic chitosan stable gel coating production is characterized in that its step is following:
1) chooses glass, quartz, Muscovitum, rustless steel, polyester film, polylactic acid membrane as base material; Base material at first, mass concentration is soaked 0.5-12h in being the PEI of 0.1-20mg/ml; Be the polyacrylic acid immersion 0.5-12h of 0.1-20mg/ml then in mass concentration; In mass concentration is the mixed liquor of N_ ethyl _ N ' _ (3_ dimethylamino) the propyl carbodiimide diimine hydrochloric acid of 1-20mg/ml and the N_ HOSu NHS that mass concentration is 2-40mg/ml, soak 2-12h again, the pH value of mixed liquor is 5.6;
2) be that the chitosan of 5-20 mg/ml and polyvinylpyrrolidonesolution solution mixed solution that mass concentration is 1-20mg/ml are coated on the substrate surface as the mode of coating liquid with spin coating, dip-coating or spraying with mass concentration; Handle 12h and vacuum drying treatment 12h through natural drying, obtain multifunctional antibiotic chitosan stable gel coating.
2. a kind of multifunctional antibiotic chitosan stable gel coating production according to claim 1 is characterized in that the method that described mode with spin coating is coated on the substrate surface is: start the spin coating appearance; Rotating speed is 1000rad/min; Draw the 0.1ml coating liquid with dropper and drop on the base material spin coating 10s, spin coating 2min under 2500rad/min then; Drying repeats spin coating 3-5 time.
3. a kind of multifunctional antibiotic chitosan stable gel coating production according to claim 1; It is characterized in that the method that described mode with dip-coating is coated on the substrate surface is: clamp base material with tweezers, immerse 5s in the coating liquid; Take out; The liquid on surface is evenly covered, be positioned over then on the glass plate, base material is peeled off with blade in dry back.
4. a kind of multifunctional antibiotic chitosan stable gel coating production according to claim 1; It is characterized in that; The described method that is coated on the substrate surface with the mode of spraying is: spray coating liquor is joined in the nebulizer; Be sprayed on 1s on the base material, 60 ℃ of oven drying 20min, this operation repetition 5 times.
CN2012101534952A 2012-05-17 2012-05-17 Method for preparing multifunctional antibacterial chitosan stable gel coat Pending CN102671240A (en)

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CN105999406A (en) * 2016-06-02 2016-10-12 温州医科大学 Method for preparing high-efficiency antibacterial quaternary ammonium salt chitosan composite gel coating layer
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Application publication date: 20120919