CN113171498A - SDS-LA/PLGA/APTES antibacterial coating - Google Patents
SDS-LA/PLGA/APTES antibacterial coating Download PDFInfo
- Publication number
- CN113171498A CN113171498A CN202110502035.5A CN202110502035A CN113171498A CN 113171498 A CN113171498 A CN 113171498A CN 202110502035 A CN202110502035 A CN 202110502035A CN 113171498 A CN113171498 A CN 113171498A
- Authority
- CN
- China
- Prior art keywords
- plga
- aptes
- sds
- coating
- layer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/08—Materials for coatings
- A61L31/10—Macromolecular materials
-
- 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
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/02—Inorganic materials
- A61L31/022—Metals or alloys
-
- 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
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/08—Materials for coatings
-
- 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
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L31/148—Materials at least partially resorbable by the body
-
- 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
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L31/16—Biologically active materials, e.g. therapeutic substances
-
- 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
- A61L2300/21—Acids
-
- 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
- A61L2300/40—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
-
- 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
- A61L2300/60—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special physical form
- A61L2300/602—Type of release, e.g. controlled, sustained, slow
-
- 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
- A61L2300/60—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special physical form
- A61L2300/606—Coatings
-
- 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
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/18—Modification of implant surfaces in order to improve biocompatibility, cell growth, fixation of biomolecules, e.g. plasma treatment
-
- 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
- A61L2420/00—Materials or methods for coatings medical devices
- A61L2420/02—Methods for coating medical devices
-
- 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
- A61L2420/00—Materials or methods for coatings medical devices
- A61L2420/06—Coatings containing a mixture of two or more compounds
-
- 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
- A61L2420/00—Materials or methods for coatings medical devices
- A61L2420/08—Coatings comprising two or more layers
Abstract
The invention relates to an SDS-LA/PLGA/APTES coating with an antibacterial function. The coating consists of APTES, PLGA, SDS and LA. The SDS-LA/PLGA/APTES coating is combined with the surface of the implant through the grafting effect of the APTES, and SDS and LA are slowly released by utilizing the degradation effect of the PLGA, so that the surface of the implant is endowed with an antibacterial function. The preparation method comprises the following steps: firstly, a large number of active oxygen vacancies are obtained on the surface of a substrate by adopting a plasma activation technology; then, the APTES is polymerized and deposited on the surface of the substrate by using a dip coating method; then utilizing the condensation reaction of carboxyl in PLGA and amino in APTES to graft and fix the PLGA and the APTES on the surface of the matrix; and then loading SDS and LA in a certain proportion into the PLGA layer to obtain the SDS-LA/PLGA/APTES coating with antibacterial effect.
Description
Technical Field
The invention relates to an SDS-LA/PLGA/APTES coating with an antibacterial function. Firstly, a large number of active oxygen vacancies are obtained on the surface of a substrate by adopting a plasma activation technology; then, the APTES is polymerized and deposited on the surface of the substrate by using a dip coating method; then utilizing the condensation reaction of carboxyl in PLGA and amino in APTES to graft and fix the PLGA and the APTES on the surface of the matrix; loading SDS and LA mixed according to a certain proportion into the PLGA layer; finally obtaining the SDS-LA/PLGA/APTES coating with antibacterial function, belonging to the technical field of biomedical materials.
Background
According to the data on the handbook of the public at work for the prevention of bacterial infections promulgated by the World Health Organization (WHO), more than 1400 million people are suffering from bacterial infections every day worldwide, of which 60% are related to the medical devices used. Chinese patent CN102671239A mentions that although antibiotics have a surprising effect on bacterial infections, abuse and overuse of traditional antibiotics will lead to the development of resistant bacteria, even "superbacteria". Therefore, biomedical metal implants having broad spectrum, not causing bacterial resistance, and having biocompatible and antibacterial properties are an urgent need for clinical applications.
The surface antibacterial function of the biomedical implant can be realized by adopting a surface modification mode. The biomedical implant surface can be endowed with special functions by depositing a coating layer having functional groups on the surface thereof and loading a specific drug. It has been reported in the literature that triaminopropyltriethoxysilane (APTES) polymeric coatings exhibit good cellular and blood compatibility in physiological environments. The chemical structure of APTES has amino group, and can provide grafting functional group for loading medicine or medicine carrier with the functions of diminishing inflammation, promoting blood circulation, etc. and is used in medicine loading, cell adsorption, protein fixation, etc. Polylactic-co-glycolic acid (PLGA) is a degradable functional polymer organic compound, has good biocompatibility, nontoxicity and good performance of forming capsules and films, and is widely applied to the fields of pharmacy, medical engineering materials and modern industry. Meanwhile, PLGA has the characteristic of being degradable in vivo, can be used as a drug sustained release carrier, and has been widely applied in the field of tissue engineering.
The mixed solution of Sodium Dodecyl Sulfate (SDS) and Levulinic Acid (LA) can effectively reduce the number of bacterial food-borne pathogens. Meanwhile, the mixed solution of SDS and LA also has the function of anti-biofilm activity. Therefore, the mixed solution of SDS and LA may be applied to the surface of a material to impart antimicrobial properties thereto.
The biomedical implant is placed in oxygen plasma through a plasma activation technology to enable the surface of the biomedical implant to obtain a large number of active oxygen vacancies, APTES is polymerized and deposited on the surface of the biomedical implant through a dip coating method, then carboxyl in PLGA and amino in APTES are subjected to condensation reaction to be grafted and fixed on the surface of the biomedical implant, and SDS and LA mixed according to a certain proportion are loaded in a PLGA layer to finally obtain the SDS-LA/PLGA/APTES coating with an antibacterial function. The idea is to prepare an SDS-LA/PLGA/APTES coating on the surface of the biomedical implant to endow the surface of the biomedical implant with an antibacterial function, and meanwhile, the idea is rarely reported in the technical field of biomedical materials. In view of the above, the invention provides a SDS-LA/PLGA/APTES coating with antibacterial function constructed on the surface of a biomedical implant.
Disclosure of Invention
The invention aims to provide an antibacterial coating applied to the surface of a biomedical implant material aiming at the urgent need of the biomedical implant material, the coating can effectively resist bacteria when being implanted, the material implantation failure caused by bacterial infection is avoided, and meanwhile, the coating has small toxic damage to tissue cells and good bioactivity and tissue compatibility.
Firstly, adopting an oxygen plasma activation technology to obtain a large number of active oxygen vacancies on the surface of the biomedical implant; then, the APTES is polymerized and deposited on the surface of the biomedical implant by using a dip coating method; then utilizing the condensation reaction of carboxyl in PLGA and amino in APTES to graft and fix the PLGA and the APTES on the surface of the biomedical implant; and loading SDS and LA mixed according to a certain proportion into a PLGA layer to obtain the SDS-LA/PLGA/APTES coating. The materials used by the coating are all nontoxic degradable materials, and the finally obtained SDS-LA/PLGA/APTES coating has good biocompatibility, promotes osteogenic differentiation of preosteoblasts and simultaneously endows the surface of the biomedical implant with an excellent antibacterial function. The coating is beneficial to reducing the risk of secondary infection after being implanted, has good biocompatibility, can be degraded in vivo, and can discharge degradation products out of the body through a circulatory system.
The invention is realized by the following technical scheme:
the SDS-LA/PLGA/APTES coating with antibacterial effect is characterized in that the SDS-LA/PLGA/APTES antibacterial coating consists of a triaminopropyltriethoxysilane APTES grafting layer which is polymerized and deposited on the surface of a biomedical implant, a polylactic acid-glycolic acid copolymer PLGA layer with the function of controlling the release of antibacterial ingredients, a sodium dodecyl sulfate SDS layer with the antibacterial function and an levulinic acid LA layer; the APTES graft layer is coated on the surface of the biomedical implant, and a large number of active oxygen vacancies obtained by a plasma activation technology and polymerization reaction of a wet chemical method are utilized for polymerization and deposition; the PLGA layer with the function of controlling the release of the antibacterial component is fixed by spin coating by utilizing the dehydration condensation reaction of carboxyl in PLGA and amino in APTES; the SDS-LA layer with the antibacterial function is obtained by loading SDS and LA which are mixed according to a certain proportion on a PLGA layer through spin coating. The preparation method of the SDS-LA/PLGA/APTES coating with the antibacterial function comprises the following steps:
(1) grinding and polishing the surface of the biomedical implant, activating the surface of the biomedical implant by using oxygen plasma, and obtaining a large number of active oxygen vacancies on the surface of the material;
(2) placing the medical implant with the activated surface obtained in the step (1) in an ethanol solution containing APTES, performing polymerization deposition on an APTES layer on the surface of the medical implant for 15-40 minutes, then placing the medical implant with the APTES layer deposited on the surface in a drying oven at 100 ℃ for dehydration treatment for 3 hours, and storing the medical implant for later use after cooling;
(3) placing the implant with APTES on the surface obtained in the step (2) into a spin coater, spin-coating a dichloromethane solution containing PLGA, fixing a PLGA layer on the surface of the dichloromethane solution, and storing the PLGA layer for later use after the PLGA layer is naturally dried;
(4) and (4) placing the implant fixed with the PLGA layer obtained in the step (3) into a spin coater, spin-coating an aqueous solution containing SDS and LA mixed according to a certain proportion, loading the SDS and LA on the surface of the aqueous solution, and naturally drying the aqueous solution to finally obtain the SDS-LA/PLGA/APTES coating with the antibacterial function.
Further, the biomedical implant in the step (1) is sequentially polished and polished step by step from coarse to fine by using metallographic abrasive paper with the numbers of 600 #, 800 #, and 1000 #, and is sequentially ultrasonically cleaned for 3-5 minutes by using absolute ethyl alcohol and deionized water;
further, the surface of the oxygen plasma activated biomedical implant in the step (1) is treated in the atmosphere of the oxygen plasma for 1-5 minutes under the conditions of power of 10-30W and pressure of 2-12 Pa, so that a large number of active oxygen vacancies are obtained on the surface of the sample;
further, the APTES ethanol solution in the step (2) is an APTES ethanol solution with the volume fraction of 5-15%, and after the solution is prepared, ultrasonic oscillation is needed for 3-5 minutes, so that the APTES absolute ethanol solution is uniformly mixed;
further, in the step (2), APTES is polymerized and deposited on the surface of the biomedical implant by adopting a wet chemical method, namely, the biomedical implant is immersed into an APTES ethanol solution which is prepared, ultrasonically vibrated and uniformly mixed for 15-40 minutes to polymerize and deposit the APTES;
further, the dichloromethane solution of PLGA in (3) is prepared according to the following steps: dichloromethane = 50-150 mg:1ml of PLGA dichloromethane solution prepared according to the proportion;
further, the parameters for spin-coating the biomedical implant in the spin-coating machine in (3) are as follows: the spin coating is divided into two stages, wherein the rotating speed of the first stage is 100-400 r/s, and the first stage rotates for 3-10 s; the second stage rotates at a speed of 800-1500 r/s for 40-80 s, and 100-300 μ L of the solution is completely dropped onto the APTES layer surface before the spin coating is finished.
Further, the aqueous solution of SDS and LA mixed in a certain proportion in (4) is an aqueous solution prepared by mixing 1-10% by mass of SDS and 1-15% by mass of LA.
Further, the parameters for spin-coating the biomedical implant in the spin-coating machine in (4) are as follows: the spin coating is divided into two stages, wherein the rotating speed of the first stage is 100-400 r/s, and the first stage rotates for 3-10 s; the rotation speed of the second stage is 800-1500 r/s, the second stage rotates for 40-80 s, and 100-300 mu L of the solution is completely dripped on the surface of the PLGA layer before the spin coating is finished.
Has the advantages that:
(1) the coating has good antibacterial effect on staphylococcus aureus, can endow the surface of the biomedical implant with antibacterial property, and reduces the risk of postoperative infection of the biomedical implant.
(2) The coating has good biocompatibility while having an antibacterial effect, so that the coating does not generate toxic action on tissue cells of an implanted part after being implanted into a human body and can promote osteogenic differentiation of preosteoblasts; the APTES and PLGA layer in the coating can control the release of the antibacterial agents SDS and LA while tightly polymerizing the surface of the biomedical implant and the antibacterial agents, thereby playing a role in long-term antibiosis.
(3) The coating has the advantages of simple structure, easy preparation and good antibacterial and biocompatibility. The coating does not need a complex preparation process, has low cost and simple and convenient preparation, can realize the antibacterial property modification of the surfaces of different metal substrates, and has universal applicability.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of the surface topography of the SDS-LA/PLGA/APTES coating of example 1.
FIG. 2 is X-ray photoelectron spectroscopy (XPS) of the SDS-LA/PLGA/APTES coating of example 1.
FIGS. 3 a and b are the zone of inhibition pictures of SDS-LA/PLGA/APTES coatings in example 1 and example 2, respectively.
FIG. 4 is a graph showing the calculation results of the antibacterial ratio of SDS-LA/PLGA/APTES coating in example 1.
Detailed Description
Example 1:
(1) firstly, selecting a biomedical implant ZA6 zinc alloy;
(2) pretreatment: sequentially grinding and polishing the zinc alloy implant by metallographic abrasive paper with the numbers of 600 #, 800 #, and 1000 # from coarse sand to fine sand, then ultrasonically cleaning by absolute ethyl alcohol and deionized water, and drying for later use;
(3) placing the zinc alloy implant in the step (2) in a plasma enhanced chemical vapor deposition device, and activating the surface of the sample for 1 minute by oxygen plasma with the power of 20W and the pressure of 8 Pa;
(4) immediately putting the zinc alloy implant with the surface activated in the step (3) into APTES ethanol solution with the volume fraction of 10 percent, and dip-coating for 30 minutes by adopting a dip-coating method;
(5) placing the sample subjected to the dip coating by the medium-wet chemical method in the step (4) in a drying oven at 100 ℃, dehydrating for 3 hours, and cooling and taking out for later use;
(6) as 100 mg PLGA: dissolving PLGA in dichloromethane with the proportion of 1ml of dichloromethane, and uniformly spin-coating the PLGA solution on the surface of the zinc alloy implant prepared in the step (5) by using a spin coater, wherein the spin coating process is divided into two stages, the rotating speed of the first stage is 200 r/s, and the rotating time is 6 s; the rotation speed of the second stage is 1000 r/s, the second stage rotates for 60 s, and 200 mu L of solution is completely dripped to the surface of the APTES layer before the spin coating is finished;
(7) preparing a mixed solution of SDS with the mass fraction of 6% and LA with the mass fraction of 9%, uniformly spin-coating the mixed solution of SDS and LA on the surface of the sample prepared in the step (6) by using a spin coating machine, wherein the spin coating process is divided into two stages, the rotating speed of the first stage is 200 r/s, and the first stage rotates for 6 s; the rotation speed of the second stage is 1000 r/s, the second stage rotates for 60 s, and 200 mu L of solution is completely dripped to the surface of the PLGA layer before the spin coating is finished.
FIG. 2 is X-ray photoelectron spectroscopy (XPS) of the SDS-LA/PLGA/APTES coating of example 1, and FIG. 3 a is the experimental results of the zone of inhibition (Staphylococcus aureus) of the SDS-LA/PLGA/APTES coating of example 1. FIG. 4 is the result of calculation of the antibacterial ratio of the SDS-LA/PLGA/APTES coating bacteria adhesion in example 1.
Example 2:
(1) firstly, selecting a biomedical implant ZA6 zinc alloy;
(2) pretreatment: sequentially grinding and polishing ZA6 zinc alloy by metallographic abrasive paper with the reference numbers of 600 #, 800 #, and 1000 # from coarse sand to fine sand, then ultrasonically cleaning by absolute ethyl alcohol and deionized water, and drying for later use;
(3) placing the ZA6 zinc alloy in the step (2) in a plasma enhanced chemical vapor deposition device, and activating and treating the surface of the sample for 3 minutes by oxygen plasma with the power of 20W and the pressure of 8 Pa;
(4) immediately putting the sample with the surface activated in the step (3) into APTES ethanol solution with the volume fraction of 10 percent, and dip-coating for 30 minutes by adopting a dip-coating method;
(5) placing the sample dipped and coated by the dip coating method in the step (4) in a drying oven at 100 ℃, dehydrating for 3 hours, and cooling and taking out for later use;
(6) as 150 mg PLGA: dissolving PLGA in dichloromethane with the proportion of 1ml of dichloromethane, and uniformly spin-coating the PLGA solution on the surface of the sample prepared in the step (5) by using a spin coater, wherein the spin coating process is divided into two stages, the rotating speed of the first stage is 400 r/s, and the rotating time is 10 s; the rotation speed of the second stage is 1500r/s, the second stage rotates for 80 s, and 300 mu L of solution is completely dripped to the surface of the APTES layer before the spin coating is finished;
(7) preparing a mixed solution of SDS with the mass fraction of 10% and LA with the mass fraction of 15%, and uniformly spin-coating the mixed solution of SDS and LA on the surface of the sample prepared in the step (6) by using a spin coating machine, wherein the spin coating parameters are as follows: the spin coating is divided into two stages, the rotating speed of the first stage is 400 r/s, and the first stage rotates for 10 s; the rotation speed of the second stage is 1500r/s, the second stage rotates for 80 s, and 300 mu L of solution is completely dripped to the surface of the PLGA layer before the spin coating is finished;
FIG. 3 b shows the results of the zone of inhibition (Staphylococcus aureus) of the SDS-LA/PLGA/APTES coating in example 2.
It should be understood that the above examples 1 and 2 of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. It will be apparent to those skilled in the art that other variations and modifications may be made in the foregoing disclosure, without departing from the spirit or essential characteristics of the invention, and it is intended to cover all such modifications and variations as fall within the true spirit and scope of the invention.
Claims (5)
1. The SDS-LA/PLGA/APTES coating with antibacterial effect is characterized in that the SDS-LA/PLGA/APTES coating consists of a triaminopropyltriethoxysilane APTES grafting layer which is polymerized and deposited on the surface of an implant, a polylactic acid-glycolic acid copolymer PLGA layer with the effect of controlling the release of antibacterial ingredients and a sodium dodecyl sulfate-levulinic acid SDS-LA layer with the antibacterial function; the triaminopropyltriethoxysilane graft layer is polymerized and deposited by utilizing a large number of active oxygen vacancies obtained by a plasma activation technology and a polymerization reaction of a wet chemical method, and is coated on the surface of the implant; the polylactic acid-glycolic acid copolymer layer with the function of controlling the release of the antibacterial components is fixed by spin coating a polylactic acid-glycolic acid copolymer solution on the surface of the triaminopropyltriethoxysilane grafting layer and utilizing the dehydration condensation reaction of carboxyl in the polylactic acid-glycolic acid copolymer and amino in the triaminopropyltriethoxysilane; the sodium dodecyl sulfate-levulinic acid layer with the antibacterial function is loaded in the polylactic acid-glycolic acid copolymer layer by spin-coating a sodium dodecyl sulfate solution and a levulinic acid solution which are mixed according to a certain proportion on the surface of the polylactic acid-glycolic acid copolymer; the preparation of the SDS-LA/PLGA/APTES coating with the antibacterial function comprises the following steps:
(1) grinding and polishing the surface of the biomedical implant, activating the surface of the biomedical implant by using oxygen plasma, and obtaining a large number of active oxygen vacancies on the surface of the material;
(2) placing the medical implant with the activated surface obtained in the step (1) in an ethanol solution containing APTES, performing polymerization deposition on the surface of the medical implant for 15-40 minutes to obtain an APTES layer, then placing the medical implant with the APTES layer deposited on the surface in a drying oven at 100 ℃ for dehydration treatment for 3 hours, and storing the medical implant for later use after cooling;
(3) placing the implant with APTES on the surface obtained in the step (2) into a spin coater, spin-coating a dichloromethane solution containing PLGA, fixing a PLGA layer on the surface of the dichloromethane solution, and storing the PLGA layer for later use after the PLGA layer is naturally dried;
(4) and (4) placing the implant fixed with the PLGA layer obtained in the step (3) into a spin coater, spin-coating an aqueous solution containing SDS and LA mixed according to a certain proportion, loading the SDS and LA on the surface of the aqueous solution, and naturally drying the aqueous solution to finally obtain the SDS-LA/PLGA/APTES coating with the antibacterial function.
2. The method of claim 1, wherein the plasma activation of the step (1) comprises the steps of: and (3) placing the polished biomedical implant into plasma enhanced chemical vapor deposition equipment, and treating the surface for 1-5 minutes in an oxygen plasma atmosphere under the conditions of power of 10-30W and pressure of 2-12 Pa, so that a large number of active oxygen vacancies are obtained on the surface of the sample.
3. The method of claim 1, wherein the ethanol solution containing APTES in step (2) comprises 5-15% by volume of APTES.
4. The method for preparing SDS-LA/PLGA/APTES coating with antibacterial effect according to claim 1, wherein the PLGA-containing dichloromethane solution of step (3) is prepared according to the ratio of PLGA to dichloromethane = 50-150 mg to 1 ml; the spin coating of the step (3) comprises the following steps: the spin coating process is divided into two stages, wherein the rotating speed of the first stage is 100-400 r/s, and the rotating speed is 3-10 s; the second stage rotates at a speed of 800-1500 r/s for 40-80 s, and 100-300 μ L of the solution is completely dropped onto the APTES layer surface before the spin coating is finished.
5. The method for preparing SDS-LA/PLGA/APTES coating with antibacterial effect as claimed in claim 1, wherein the aqueous solution of SDS and LA mixed in a certain proportion in step (4) is an aqueous solution mixed by SDS containing 1-10% by mass and LA containing 1-15% by mass; the spin coating of the step (4) comprises the following steps: the spin coating process is divided into two stages, wherein the rotating speed of the first stage is 100-400 r/s, and the rotating speed is 3-6 s; the rotation speed of the second stage is 800-1500 r/s, the second stage rotates for 40-80 s, and 100-300 mu L of the solution is completely dripped on the surface of the PLGA layer before the spin coating is finished.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110502035.5A CN113171498A (en) | 2021-05-08 | 2021-05-08 | SDS-LA/PLGA/APTES antibacterial coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110502035.5A CN113171498A (en) | 2021-05-08 | 2021-05-08 | SDS-LA/PLGA/APTES antibacterial coating |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113171498A true CN113171498A (en) | 2021-07-27 |
Family
ID=76928512
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110502035.5A Pending CN113171498A (en) | 2021-05-08 | 2021-05-08 | SDS-LA/PLGA/APTES antibacterial coating |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113171498A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113755828A (en) * | 2021-09-02 | 2021-12-07 | 福建医科大学附属口腔医院 | Method for antibacterial modification and improvement of bioactivity of titanium surface, coating and implant |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110054026A1 (en) * | 2008-05-22 | 2011-03-03 | Michael Patrick Doyle | Antimicrobial composition and use |
| US20120082717A1 (en) * | 2009-06-05 | 2012-04-05 | Snu R&Db Foundation | Complex, multilayer using the same, and device coated with the multilayer |
| US20120121679A1 (en) * | 2009-07-16 | 2012-05-17 | University Of Georgia Research Foundation, Inc. | Viricidal and microbicidal compositions and uses thereof |
| CN106512083A (en) * | 2016-10-14 | 2017-03-22 | 湖北大学 | Medical titanium alloy preparation method |
| CN107072884A (en) * | 2014-09-04 | 2017-08-18 | 西亚克特有限责任公司 | The root canal disinfection of microvesicle based on photochemical activation |
| CN110180038A (en) * | 2019-06-21 | 2019-08-30 | 西南大学 | Has the kirsite vascular stent material of drug slow release function superhigh-flexibility coating |
-
2021
- 2021-05-08 CN CN202110502035.5A patent/CN113171498A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110054026A1 (en) * | 2008-05-22 | 2011-03-03 | Michael Patrick Doyle | Antimicrobial composition and use |
| US20120082717A1 (en) * | 2009-06-05 | 2012-04-05 | Snu R&Db Foundation | Complex, multilayer using the same, and device coated with the multilayer |
| US20120121679A1 (en) * | 2009-07-16 | 2012-05-17 | University Of Georgia Research Foundation, Inc. | Viricidal and microbicidal compositions and uses thereof |
| CN107072884A (en) * | 2014-09-04 | 2017-08-18 | 西亚克特有限责任公司 | The root canal disinfection of microvesicle based on photochemical activation |
| CN106512083A (en) * | 2016-10-14 | 2017-03-22 | 湖北大学 | Medical titanium alloy preparation method |
| CN110180038A (en) * | 2019-06-21 | 2019-08-30 | 西南大学 | Has the kirsite vascular stent material of drug slow release function superhigh-flexibility coating |
Non-Patent Citations (4)
| Title |
|---|
| CHEN D等: "Control of pathogens in biofilms on the surface of stainless steel by levulinic acid plus sodium dodecyl sulfate", 《INTERNATIONAL JOURNAL OF FOOD MICROBIOLOGY》 * |
| CHEN ZL等: "Plasma deposited APTES: A potential film for biomedical application", 《MATERIALS LETTERS》 * |
| SANKALP AGARWAL等: "Enhanced corrosion protection and biocompatibility of a PLGA–silane coating on AZ31 Mg alloy for orthopaedic applications", 《RSC ADV》 * |
| 吕霞丽等: "乙酰丙酸-十二烷基硫酸钠对结核分枝杆菌的杀灭作用及其安全性毒理学评价", 《首都医科大学学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113755828A (en) * | 2021-09-02 | 2021-12-07 | 福建医科大学附属口腔医院 | Method for antibacterial modification and improvement of bioactivity of titanium surface, coating and implant |
| CN113755828B (en) * | 2021-09-02 | 2023-10-24 | 福建医科大学附属口腔医院 | Method for antibacterial modification of titanium surface and improvement of biological activity of titanium surface, coating and implant |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CA2438491C (en) | Method of making lubricious anti-microbial polymeric surfaces | |
| US6541678B2 (en) | Immunostimulating coating for surgical devices | |
| CN104189963B (en) | Reduction can the preparation method of surface coating of degradable magnesium alloy blood vessel rack degradation rate | |
| Wenhao et al. | In vitro and in vivo evaluation of structurally-controlled silk fibroin coatings for orthopedic infection and in-situ osteogenesis | |
| CN108815587B (en) | Hydrogel coating with long-term antibacterial function and preparation method thereof | |
| Du et al. | Preparation of vancomycin-loaded alginate hydrogel coating on magnesium alloy with enhanced anticorrosion and antibacterial properties | |
| CN107661544B (en) | Antibacterial porous orthopedic implant with bone-promoting composite function and preparation method thereof | |
| Yin et al. | Development of mussel adhesive polypeptide mimics coating for in-situ inducing re-endothelialization of intravascular stent devices | |
| US20110212152A1 (en) | Modified anti-microbial surfaces, devices and methods | |
| AU2002235694A1 (en) | Method of making anti-microbial polymeric surfaces | |
| JP2005516736A (en) | Polymer coating for medical devices | |
| CN110064075B (en) | Self-assembled antibacterial coating based on nano silver/D-cysteine and preparation method thereof | |
| US20200000976A1 (en) | A medical implant and a method of coating a medical implant | |
| CN110885665A (en) | Preparation method of high-stability hydrophilic coating for surface of medical instrument | |
| CN107937880B (en) | Method for modifying surface of metal material, product and application thereof | |
| CN113171498A (en) | SDS-LA/PLGA/APTES antibacterial coating | |
| CN114191620A (en) | Hydrogel coating, supported antibacterial coating, and preparation method and application thereof | |
| CN107648674B (en) | Metal implant with antibacterial and osseointegration promoting functions and preparation method thereof | |
| WO2009073643A2 (en) | Nitric oxide release coatings incorporating nitric oxide synthase enzyme | |
| CN112870443B (en) | Dental implant and preparation method thereof | |
| CN114732945B (en) | Method for improving bioactivity of titanium alloy bone | |
| CN114618024B (en) | Endothelial function bionic material, preparation method and application thereof | |
| CN115591011B (en) | Degradable zinc metal surface dynamic functional coating and preparation method thereof | |
| AU2011224699A1 (en) | Coating with antimicrobial agents | |
| CN117244118A (en) | Coating preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20210727 |