CN115160625A - Method for modifying polymer catheter on surface of polyethylene glycol hydrogel - Google Patents
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- CN115160625A CN115160625A CN202210881837.6A CN202210881837A CN115160625A CN 115160625 A CN115160625 A CN 115160625A CN 202210881837 A CN202210881837 A CN 202210881837A CN 115160625 A CN115160625 A CN 115160625A
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- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L29/00—Materials for catheters, medical tubing, cannulae, or endoscopes or for coating catheters
- A61L29/08—Materials for coatings
- A61L29/085—Macromolecular materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61L29/00—Materials for catheters, medical tubing, cannulae, or endoscopes or for coating catheters
- A61L29/14—Materials characterised by their function or physical properties, e.g. lubricating compositions
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L29/00—Materials for catheters, medical tubing, cannulae, or endoscopes or for coating catheters
- A61L29/14—Materials characterised by their function or physical properties, e.g. lubricating compositions
- A61L29/145—Hydrogels or hydrocolloids
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- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/056—Forming hydrophilic coatings
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/10—Materials for lubricating medical devices
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- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
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Abstract
The invention discloses a method for modifying a polymer catheter on the surface of polyethylene glycol hydrogel. Firstly, carrying out oxygen plasma treatment on a polymer conduit to obtain a polymer conduit with an activated surface; then placing the polymer catheter in a polyethylene glycol-acrylamide solution, and initiating polymerization through the surface active group of the polymer catheter to obtain the polyethylene glycol hydrogel surface modified polymer catheter. The PEG-PAM hydrogel with excellent hydrophilicity and lubricity is adopted for modification, so that the property of a ureter matrix is improved, the deposited adhesion is reduced, and the anti-shell capability of the ureter stent is improved.
Description
Technical Field
The invention belongs to the field of biomedical materials and urology science, and particularly relates to a method for modifying a polymer catheter on the surface of polyethylene glycol hydrogel.
Background
For patients with problems in the urinary system, ureteral stents are often placed inside the body after related operations to support, drain, improve renal function, etc. However, the introduction of foreign bodies into the urinary tract can cause stent surface encrustation and discomfort and infection of the urinary tract, especially for patients requiring long-term indwelling ureteral stents.
Encrustation refers to the deposition of mineral crystals on the surface and lumen of the ureteral stent, which, when the stent is scaled, become calcified and embrittled, losing tensile strength, increasing the risk of the stent breaking or the ureteral tearing off during removal. Crystal deposits can impede the drainage process through the stent lumen and can also interact with the urothelium of the ureter, causing damage to the ureter. In addition, long-term retention of ureteral stents has been shown to increase the risk of chronic kidney disease and increased the risk of hospitalization due to urinary tract infection or sepsis after stent retrieval.
At present, biomedical polymers with good mechanical properties and biocompatibility, such as silica gel, polyvinyl fluoride (PVC), polyurethane (PU) and the like, become widely used matrix materials at present, but the anti-crusting capability of the biomedical polymers is still insufficient, and the surfaces of the biomedical polymers need to be modified. Among them, the use of hydrogel coatings with good lubricity, such as polyethylene glycol (PEG) type hydrogels, can provide excellent hydrophilicity, lubricity to the ureter, thus helping the stent to improve the anti-crusting capability, but the preparation of hydrogel coatings has the disadvantages of insufficient stability and unsuitability for small tubular stents.
Disclosure of Invention
In order to solve the defects and shortcomings of the prior art, the invention aims to provide a method for modifying the surface of a polymer catheter by polyethylene glycol hydrogel.
The invention leads polyethylene glycol which is already a polymer to be in a hydrogel state by a simple method of initiating hydrogel polymerization by plasma, and endows the polymer catheter with hydrophilicity and lubricity.
The purpose of the invention is realized by the following technical scheme:
a method for modifying the surface of a polymer catheter by polyethylene glycol hydrogel comprises the following steps:
(1) Carrying out oxygen plasma treatment on the polymer conduit to obtain a polymer conduit with an activated surface;
(2) And (3) placing the polymer catheter with the activated surface into a polyethylene glycol-acrylamide solution, and carrying out polymerization reaction for 50-120 min at the temperature of 60-80 ℃ to obtain the polyethylene glycol hydrogel surface-modified polymer catheter.
Preferably, before the polymer conduit in the step (1) is subjected to oxygen plasma treatment, isopropanol and deionized water are sequentially used for ultrasonic cleaning for 5-10 min, and then drying treatment is carried out at 30-40 ℃ for 3-4 h.
Preferably, the polymer catheter of step (1) is one of a silicone catheter, a polyvinyl fluoride (PVC) catheter and a Polyurethane (PU) catheter.
Preferably, the vacuum degree of the oxygen plasma treatment in the step (1) is less than or equal to 0.3mbar; the oxygen plasma treatment times are 1-4 times, and each treatment time is 5-10 min.
Preferably, after the surface of the polymer conduit in the step (1) is treated by oxygen plasma, active groups such as hydroxyl, carboxyl and the like are generated, and the surface-activated polymer conduit is obtained.
Preferably, in the polyethylene glycol-acrylamide solution in the step (2), the polyethylene glycol accounts for 20-40% of the mass of the solvent, and the acrylamide accounts for 40-60% of the mass of the solvent; more preferably, the mass of the polyethylene glycol accounts for 20-30% of the mass of the solvent, and the mass of the acrylamide accounts for 40-50% of the mass of the solvent; the solvent is water.
Preferably, after the polymerization reaction in the step (2) is finished, the residual colloid on the surface of the polymer conduit is washed by water, and the polymer conduit is dried for 2 to 8 hours at the temperature of between 40 and 60 ℃ to obtain the polyethylene glycol hydrogel modified polymer conduit.
Preferably, the polymerization reaction in the step (2) is carried out at the temperature of 60-80 ℃ for 50-120 min.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the method is suitable for surface modification of various medical instruments with complicated shapes, such as ureter surface modification with the diameter of only 2-3mm, and solves the problem that the surface modification of the existing medical instruments with complicated shapes is difficult.
2. The invention adopts a plasma initiated polymerization method to concentrate the polymerization reaction on the surface of the polymer catheter, thereby ensuring the firm combination of the hydrogel obtained after polymerization and the matrix and successfully realizing the controllability of only modifying the surface of the polymer catheter.
3. The PEG-PAM hydrogel with excellent hydrophilicity and lubricity is adopted for modification, so that the property of a ureter matrix is improved, the deposited adhesion is reduced, the anti-crusting capability of the ureter stent is improved, and the problem of complications in clinical use is favorably solved.
4. The invention adopts PEG hydrogel with excellent flexibility and biocompatibility as a surface modification material, so that the clinical problems of physiological toxicity and human body injury caused by the improvement of the ureter performance are avoided.
5. The invention has simple preparation process, easily obtained raw materials, simple operation and easy popularization and application.
Drawings
FIG. 1 shows the surface condition of samples of uncoated coating (a) and coated coating (b) at 40 times magnification of example 1.
FIG. 2 is a graph showing the change in hydrophilicity of different monomer gel coats in the same process as in example 1 and comparative examples 1-2.
FIG. 3 is a graph of the surface topography of uncoated (a) and coated different hydrogel coatings (b) example 1PEG-PAAM, (c) comparative example 1PEG-PAA, (d) comparative example 2PEG-PVP polyurethane catheters after 1 month of in vitro simulation (specifically, one month of continuous flow of artificial urine through the catheter).
FIG. 4 is a graph of mass change and growth rate of uncoated and different hydrogel coatings (example 1PEG-PAAM, comparative example 1PEG-PAA, comparative example 2 PEG-PVP) polyurethane catheters after 1 month of in vitro simulation (specifically, allowing artificial urine to flow continuously through the catheter for one month).
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
Those who do not specify specific conditions in the examples of the present invention follow conventional conditions or conditions recommended by the manufacturer. The raw materials, reagents and the like used without reference to manufacturers are all conventional products which can be obtained by commercial purchase.
Example 1
The method for modifying the surface of the polymer catheter by the polyethylene glycol hydrogel comprises the following steps and process conditions of the steps:
the method comprises the following steps: taking a polyurethane catheter with the length of 1.5cm, respectively ultrasonically cleaning the polyurethane catheter with isopropanol and water for 8min, and then putting the polyurethane catheter into a 40 ℃ blast drier for drying for 3h until no moisture remains in the catheter cavity.
Step two: and (3) carrying out primary plasma treatment on the cleaned polyurethane conduit by taking oxygen as a plasma raw gas, keeping the vacuum degree at 0.29mbar, and generating active groups on the surface of the polyurethane conduit after the treatment lasts for 5 min.
Step three: 6g PEG, 15g AAM dissolved in 30mL water to get polyethylene glycol-acrylamide solution.
Step four: transferring the oxygen plasma treated polyurethane conduit and the polyethylene glycol-acrylamide aqueous solution into a small bottle with a cover, screwing down the bottle cover for sealing, immersing the oxygen plasma treated polyurethane conduit into the polyethylene glycol-acrylamide aqueous solution, and polymerizing for 1h in an oven at 80 ℃.
Step five: and taking out the polymer catheter sample, cleaning the polymer catheter sample by using deionized water of an ultrasonic cleaning machine for 8min, then drying the polymer catheter sample in a drying oven at the temperature of 40 ℃ for 2h, and leaving a layer of PEG-PAAM coating on the surface to obtain the PEG-PAAM surface modified polyurethane catheter.
Comparative example 1
The method for modifying the surface of the polymer catheter by the polyethylene glycol hydrogel comprises the following steps and process conditions of the steps:
the method comprises the following steps: taking a polyurethane catheter with the length of 1.5cm, respectively ultrasonically cleaning the polyurethane catheter with isopropanol and water for 8min, and then putting the polyurethane catheter into a 40 ℃ blast drier for drying for 3h until no moisture remains in the catheter cavity.
Step two: and (3) carrying out primary plasma treatment on the cleaned polyurethane conduit by taking oxygen as a plasma raw gas, keeping the vacuum degree at 0.29mbar, and generating active groups on the surface of the polyurethane conduit after the treatment lasts for 5 min.
Step three: 6g PEG, 15g Acrylic Acid (AA) were dissolved in 30mL water to obtain an aqueous polyethylene glycol-acrylic acid solution.
Step four: the oxygen plasma treated polyurethane catheter and the aqueous polyethylene glycol-acrylic acid solution were transferred together into a vial with a cap, the cap was tightened and sealed, the oxygen plasma treated polyurethane catheter was immersed in the aqueous polyethylene glycol-acrylic acid solution and allowed to polymerize in an oven at 80 ℃ for 1h.
Step five: and taking out the polymer catheter sample, washing the polymer catheter sample by using deionized water of an ultrasonic cleaning machine for 8min, then drying the polymer catheter sample in an oven at the temperature of 40 ℃ for 2h, and leaving a layer of PEG-PAA coating on the surface to obtain the PEG-PAA surface modified polyurethane catheter.
Comparative example 2
The method for modifying the surface of the polymer catheter by the polyethylene glycol hydrogel comprises the following steps and process conditions of the steps:
the method comprises the following steps: taking a polyurethane catheter with the length of 1.5cm, respectively ultrasonically cleaning the polyurethane catheter with isopropanol and water for 8min, and then putting the polyurethane catheter into a 40 ℃ blast drier for drying for 3h until no moisture remains in the catheter cavity.
Step two: and (3) carrying out primary plasma treatment on the cleaned polyurethane conduit by taking oxygen as a plasma raw gas, keeping the vacuum degree at 0.29mbar, and treating for 5min to generate active groups on the surface of the polyurethane conduit.
Step three: 6g PEG, 15g N-vinyl pyrrolidone (NVP) was dissolved in 30mL water to give an aqueous solution of polyethylene glycol-N-vinyl pyrrolidone.
Step four: transferring the oxygen plasma treated polyurethane conduit and the polyethylene glycol-N-vinyl pyrrolidone aqueous solution into a small bottle with a cover, screwing down the bottle cover for sealing, immersing the oxygen plasma treated polyurethane conduit into the polyethylene glycol-N-vinyl pyrrolidone aqueous solution, and polymerizing for 1h in an oven at 80 ℃.
Step five: and taking out the polymer catheter sample, washing the polymer catheter sample for 8min by using deionized water of an ultrasonic cleaning machine, then drying the polymer catheter sample in a drying oven at the temperature of 40 ℃ for 2h, and leaving a layer of PEG-PVP coating on the surface to obtain the PEG-PVP surface modified polyurethane catheter.
Example 2
A method for modifying the surface of a polymer catheter by polyethylene glycol hydrogel comprises the following steps and process conditions:
the method comprises the following steps: taking a polyurethane catheter with the length of 1.5cm, respectively ultrasonically cleaning the polyurethane catheter with isopropanol and water for 10min, and then putting the polyurethane catheter into a 50 ℃ forced air drier for drying for 3h until no moisture remains in the catheter cavity.
Step two: and (3) carrying out plasma treatment on the cleaned polyurethane conduit twice by taking oxygen as plasma raw gas, keeping the vacuum degree at 0.29mbar, and generating active groups on the surface of the polyurethane conduit after each treatment for 5 min.
Step three: 9g PEG, 12g AAM dissolved in 30mL water to get polyethylene glycol-acrylamide solution.
Step four: transferring the oxygen plasma treated polyurethane conduit and the polyethylene glycol-acrylamide aqueous solution into a small bottle with a cover, screwing down the bottle cover for sealing, immersing the oxygen plasma treated polyurethane conduit into the polyethylene glycol-acrylamide aqueous solution, and polymerizing for 2h in an oven at 60 ℃.
Step five: and taking out the polymer catheter sample, washing the polymer catheter sample for 10min by using deionized water of an ultrasonic cleaning machine, then drying the polymer catheter sample in a drying oven at 40 ℃ for 3h, and leaving a layer of PEG-PAAM coating on the surface to obtain the PEG-PAAM surface modified polyurethane catheter.
The contact angle of the PEG-PAAM surface modified polyurethane catheter obtained in this example was 40.5 °.
Example 3
The method for modifying the surface of the polymer catheter by the polyethylene glycol hydrogel comprises the following steps and process conditions of the steps:
the method comprises the following steps: taking a silica gel catheter with the length of 3cm, respectively ultrasonically cleaning the silica gel catheter with isopropanol and water for 10min, and then putting the silica gel catheter into a blast drier with the temperature of 40 ℃ for drying for 4h until no moisture remains in the catheter cavity completely.
Step two: and (3) carrying out plasma treatment on the cleaned silica gel guide tube twice by taking oxygen as plasma raw gas, keeping the vacuum degree at 0.29mbar, and generating active groups on the surface of the silica gel guide tube after each treatment for 5 min.
Step three: 10g PEG, 18gAAM dissolved in 30mL water to get polyethylene glycol-acrylamide aqueous solution.
Step four: transferring the oxygen plasma treated polyurethane conduit and the polyethylene glycol-acrylamide aqueous solution into a small bottle with a cover, screwing down the bottle cover for sealing, immersing the oxygen plasma treated polyurethane conduit into the polyethylene glycol-acrylamide aqueous solution, and polymerizing for 2h in an oven at 60 ℃.
Step five: and taking out the polymer catheter sample, cleaning the polymer catheter sample by using deionized water of an ultrasonic cleaning machine for 10min, then drying the polymer catheter sample in a drying oven at 40 ℃ for 3h, and leaving a PEG-PAAM coating on the surface to obtain the PEG-PAAM surface modified polyurethane catheter.
The contact angle of the PEG-PAAM surface modified polyurethane catheter obtained in this example was 33.4 °.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (8)
1. A method for modifying the surface of a polymer catheter by polyethylene glycol hydrogel is characterized by comprising the following steps:
(1) Carrying out oxygen plasma treatment on the polymer conduit to obtain a polymer conduit with an activated surface;
(2) And (3) placing the polymer catheter with the activated surface into a polyethylene glycol-acrylamide solution, and carrying out polymerization reaction for 50-120 min at the temperature of 60-80 ℃ to obtain the polyethylene glycol hydrogel surface-modified polymer catheter.
2. The method for modifying the polymer conduit on the surface of the polyethylene glycol hydrogel according to claim 1, wherein the vacuum degree of the oxygen plasma treatment in the step (1) is less than or equal to 0.3mbar; the oxygen plasma treatment times are 1-4 times, and each treatment time is 5-10 min.
3. The method for modifying the polymer catheter by the polyethylene glycol hydrogel surface according to claim 1, wherein in the polyethylene glycol-acrylamide solution in the step (2), the polyethylene glycol accounts for 20-40% of the solvent by mass, and the acrylamide accounts for 40-60% of the solvent by mass; the solvent is water.
4. The method for modifying the polymer catheter by the polyethylene glycol hydrogel surface according to claim 3, wherein in the polyethylene glycol-acrylamide solution in the step (2), the polyethylene glycol accounts for 20-30% of the mass of the solvent, and the acrylamide accounts for 40-50% of the mass of the solvent.
5. The method for modifying the surface of the polymer catheter by using the polyethylene glycol hydrogel according to claim 1, wherein the polymerization reaction in the step (2) is carried out at a temperature of 60-80 ℃ for 50-120 min.
6. The method of claim 1, wherein the polymer catheter of step (1) is one of a silicone catheter, a polyvinyl fluoride catheter and a polyurethane catheter.
7. The method for modifying the surface of the polymer catheter by using the polyethylene glycol hydrogel according to claim 1, wherein after the polymerization reaction in the step (2) is finished, residual colloid on the surface of the polymer catheter is washed by water and dried at 40-60 ℃ for 2-8 h to obtain the polyethylene glycol hydrogel modified polymer catheter.
8. The method for modifying the surface of the polymer catheter by using the polyethylene glycol hydrogel as claimed in claim 1, wherein the polymer catheter in the step (1) is sequentially ultrasonically cleaned by using isopropanol and deionized water for 5-10 min before being subjected to oxygen plasma treatment, and then is dried at 30-40 ℃ for 3-4 h.
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| US5290548A (en) * | 1987-04-10 | 1994-03-01 | University Of Florida | Surface modified ocular implants, surgical instruments, devices, prostheses, contact lenses and the like |
| US20170360994A1 (en) * | 2014-12-09 | 2017-12-21 | Tangible Science, Llc | Medical device coating with a biocompatible layer |
| US20180042742A1 (en) * | 2015-03-19 | 2018-02-15 | Nanyang Technological University | Stent assembly and method of preparing the stent assembly |
| US20190125934A1 (en) * | 2017-10-26 | 2019-05-02 | Massachusetts Institute Of Technology | Tough hydrogel coating and method of manufacture |
| CN111870742A (en) * | 2020-06-24 | 2020-11-03 | 东南大学 | Preparation method of hydrophilic lubricating coating on surface of PVC (polyvinyl chloride) catheter |
| CN112574460A (en) * | 2020-12-16 | 2021-03-30 | 苏州凝智新材料发展有限公司 | Polymer medical instrument with hydrophilic lubricating coating and preparation method thereof |
| US20220075098A1 (en) * | 2018-12-19 | 2022-03-10 | Tangible Science, Inc. | Systems and methods of treating a hydrogel-coated medical device |
-
2022
- 2022-07-26 CN CN202210881837.6A patent/CN115160625A/en active Pending
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|---|---|---|---|---|
| US5290548A (en) * | 1987-04-10 | 1994-03-01 | University Of Florida | Surface modified ocular implants, surgical instruments, devices, prostheses, contact lenses and the like |
| US20170360994A1 (en) * | 2014-12-09 | 2017-12-21 | Tangible Science, Llc | Medical device coating with a biocompatible layer |
| US20180042742A1 (en) * | 2015-03-19 | 2018-02-15 | Nanyang Technological University | Stent assembly and method of preparing the stent assembly |
| US20190125934A1 (en) * | 2017-10-26 | 2019-05-02 | Massachusetts Institute Of Technology | Tough hydrogel coating and method of manufacture |
| US20220075098A1 (en) * | 2018-12-19 | 2022-03-10 | Tangible Science, Inc. | Systems and methods of treating a hydrogel-coated medical device |
| CN111870742A (en) * | 2020-06-24 | 2020-11-03 | 东南大学 | Preparation method of hydrophilic lubricating coating on surface of PVC (polyvinyl chloride) catheter |
| CN112574460A (en) * | 2020-12-16 | 2021-03-30 | 苏州凝智新材料发展有限公司 | Polymer medical instrument with hydrophilic lubricating coating and preparation method thereof |
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| Title |
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| 宋心远等编著: "《新型染整技术》", 中国纺织出版社, pages: 28 - 30 * |
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