CN117159813A - Medical catheter with hydrophilic coating and preparation method thereof - Google Patents
Medical catheter with hydrophilic coating and preparation method thereof Download PDFInfo
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- CN117159813A CN117159813A CN202311154527.5A CN202311154527A CN117159813A CN 117159813 A CN117159813 A CN 117159813A CN 202311154527 A CN202311154527 A CN 202311154527A CN 117159813 A CN117159813 A CN 117159813A
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- 239000011248 coating agent Substances 0.000 title claims abstract description 21
- 238000000576 coating method Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims description 20
- 229920002635 polyurethane Polymers 0.000 claims abstract description 45
- 239000004814 polyurethane Substances 0.000 claims abstract description 45
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 22
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 108010020346 Polyglutamic Acid Proteins 0.000 claims abstract description 12
- 229920002643 polyglutamic acid Polymers 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 34
- 238000002156 mixing Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 12
- 229920000570 polyether Polymers 0.000 claims description 12
- 229920002545 silicone oil Polymers 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 9
- 230000010355 oscillation Effects 0.000 claims description 9
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 9
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 9
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 9
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002861 polymer material Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 2
- 230000002526 effect on cardiovascular system Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910014033 C-OH Inorganic materials 0.000 description 1
- 208000032840 Catheter-Related Infections Diseases 0.000 description 1
- 239000004970 Chain extender Substances 0.000 description 1
- 229910014570 C—OH Inorganic materials 0.000 description 1
- 206010064687 Device related infection Diseases 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 206010066901 Treatment failure Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 230000002924 anti-infective effect Effects 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 125000005442 diisocyanate group Chemical group 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000399 orthopedic effect Effects 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 229920001610 polycaprolactone Polymers 0.000 description 1
- 239000004632 polycaprolactone Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
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- Materials For Medical Uses (AREA)
Abstract
A process for preparing the hydrophilic coated polyurethane catheter includes immersing the polyurethane catheter in the hydrophilic treating liquid of polyglutamic acid, polyvinyl alcohol and deionized water, and extracting at a certain speed; and (5) drying in vacuum to obtain the polyurethane catheter with the hydrophilic coating. Compared with the prior art, the polyurethane medical catheter has better firmness.
Description
Technical Field
The invention belongs to the technical field of medical instruments, and particularly relates to a medical catheter with a hydrophilic coating and a preparation method thereof.
Background
At present, the medical apparatus has almost millions of medical instruments on the global market, and has extremely remarkable significance for modern medicine in the fields of ophthalmology, orthopedics, cardiovascular treatment and the like. The medical catheter can be used as a passage for connecting the inside and the outside of a human body, so that the medical catheter is widely applied to aspects of drug delivery, drainage, blood conveying, auxiliary medical instrument introduction and the like. In 2007 alone, global medical device usage amounts to approximately 10 billion per year, while medical catheters occupy about four times the total number of medical device uses, and this number is also increasing.
The medical catheter tube is generally made of high polymer materials, and has the advantages of softness, durability, low cost, easy availability and the like, such as silicon rubber, polyurethane, polyvinyl chloride and the like. Common medical catheters are: venous indwelling needle cannula, ventilator cannula, central venous catheter, and the like. Since a polymer material used for a biomedical catheter is in close contact with human tissue, it is required to have good biocompatibility itself. However, these polymer materials are inherently more hydrophobic and thus tend to adhere to bacteria. The materials do not have the sterilization and anti-fouling functions, so that the problems of large friction coefficient of the surface of the catheter, colonization of surface pathogenic bacteria and the like are easily caused, the tissue lubrication, anti-infection and biocompatibility of the catheter are greatly influenced, a series of problems of mucosal injury, catheter related infection and the like are caused, and even treatment failure is caused.
The polyurethane medical catheter is a thermoplastic elastomer with a block structure, and the structural main body of the polyurethane medical catheter is divided into a soft section and a hard section. Wherein the soft segment is generally a longer segment, such as polyethylene glycol, polyethylene oxide, polycaprolactone, etc. with low polymerization degree, and the segment has certain flexibility relatively; the hard segment is a relatively short diisocyanate and a chain extender, and has certain rigidity relatively. Polyurethane materials meeting different performance requirements can be obtained by selecting different hard and soft segment materials and composition ratios. Therefore, polyurethane is widely used for the aspects of medical catheters, adhesives, cardiovascular stents and the like, and the surface of the polyurethane is hydrophobic, so that larger resistance is generated when the polyurethane is inserted into human tissues, the pain of a patient is aggravated, and certain damage is caused to the tissues; and the traditional polyurethane has no antibacterial function, and the hydrophobic surface is extremely easy to adhere bacteria. In addition, the surface friction coefficient of the existing polyurethane medical catheter is large, and the coating firmness is poor.
Accordingly, there is an urgent need to provide a medical catheter with a hydrophilic coating layer having better firmness and a method for preparing the same, aiming at the above-mentioned defects of the prior art.
Disclosure of Invention
The invention aims to provide a medical catheter with a hydrophilic coating and a preparation method thereof, wherein the medical catheter has better firmness.
In order to achieve the purpose of the invention, on one hand, the invention adopts the following technical scheme: a method for preparing a polyurethane catheter with a hydrophilic coating, comprising the steps of:
uniformly mixing polyglutamic acid, polyvinyl alcohol and deionized water, stirring for reaction, and then carrying out ultrasonic oscillation to obtain a transparent uniform solution 1;
uniformly mixing polyether modified silicone oil, triethanolamine and deionized water to obtain a transparent uniform solution 2;
slowly adding the solution 1 into the solution 2, then adding sodium hexametaphosphate into the mixed solution, and carrying out ultrasonic oscillation to obtain hydrophilic treatment liquid;
immersing the polyurethane catheter in hydrophilic treatment liquid, and then pulling out at a certain speed; and (5) drying in vacuum to obtain the polyurethane catheter with the hydrophilic coating.
The preparation method of the invention comprises the steps of (0.5-2.5) g of polyglutamic acid, polyvinyl alcohol and deionized water: (7-10) g:20mL.
Advantageously, the ratio of polyglutamic acid, polyvinyl alcohol and deionized water is (1-2) g: (8-9) g:20mL.
The production method according to the present invention, wherein the average molecular weight mn=5000 to 10000 of polyglutamic acid; the polyvinyl alcohol is selected from polyvinyl alcohol PVA 1799.
The preparation method of the invention, wherein the stirring reaction conditions are as follows: the reaction temperature is 60-90 ℃; the reaction time is 2-8h.
Advantageously, the conditions of the stirring reaction are: the reaction temperature is 70-80 ℃; the reaction time is 4-6h.
The preparation method of the invention comprises the following steps of (5-8) g: (2-5) g:100mL.
Advantageously, the ratio of polyether modified silicone oil, triethanolamine and deionized water is (6-7) g: (3-4) g:100mL.
The preparation method of the invention comprises the following steps of: 2.
advantageously, the volume ratio of solution 1 to solution 2 is (3-5): 2.
the preparation method according to the invention, wherein the amount of sodium hexametaphosphate is 0.1-0.4wt% based on the weight of the mixed solution.
Advantageously, sodium hexametaphosphate is used in an amount of 0.2 to 0.3wt% based on the weight of the mixed solution.
The preparation method according to the present invention, wherein the treatment time for immersing in the hydrophilic treatment liquid is 60 to 180 seconds.
Advantageously, the treatment time for immersion in the hydrophilic treatment liquid is between 90 and 120 seconds.
The preparation method disclosed by the invention is characterized in that the pulling speed is 2-10cm/min.
Advantageously, the speed of the pulling is between 5 and 6cm/min.
On the other hand, the invention also provides a polyurethane catheter with a hydrophilic coating, which is obtained by the preparation method.
According to the invention, the polyurethane medical catheter is modified by a specific preparation method to obtain the polyurethane catheter with the hydrophilic coating. Compared with the prior art, the polyurethane medical catheter has better firmness.
Detailed Description
The invention is further described below in conjunction with the detailed description.
It should be understood that the description of the specific embodiments is merely illustrative of the principles and spirit of the invention, and not in limitation thereof. Further, it should be understood that various changes, substitutions, omissions, modifications, or adaptations to the present invention may be made by those skilled in the art after having read the present disclosure, and such equivalent embodiments are within the scope of the present invention as defined in the appended claims.
In the present invention, all parts are parts by weight unless otherwise specified; all percentages are by weight.
Example 1
According to 1g:9g: uniformly mixing polyglutamic acid (Mn=5000-10000), polyvinyl alcohol PVA 1799 and deionized water according to the proportion of 20mL, stirring at 80 ℃ for reaction for 4h, and then carrying out ultrasonic vibration for 20min to obtain transparent uniform solution 1.
According to 6g:3g: and uniformly mixing polyether modified silicone oil H-204, triethanolamine and deionized water according to the proportion of 100mL to obtain transparent uniform solution 2.
Slowly adding 2 times of the volume of the solution 1 into 1 time of the volume of the solution 2 at 45 ℃, then adding sodium hexametaphosphate accounting for 0.2 percent of the weight of the mixed solution, and carrying out ultrasonic oscillation for 20 minutes to obtain the hydrophilic treatment liquid.
The polyurethane catheter was immersed in the hydrophilic treatment liquid for 90s and then pulled out at a speed of 5 cm/min. And after the polyurethane catheter is dried at room temperature, further vacuum drying is carried out, and the polyurethane catheter with the hydrophilic coating is obtained.
As can be seen from the infrared spectrum of a small amount of samples, the stretching vibration peak of the polyurethane catheter O-H with the hydrophilic coating is 3262cm -1 Move up to 3405cm -1 The position shows that the grafted polyether siloxane breaks partial hydrogen bond action in polyurethane molecules, so that the O-H stretching vibration frequency moves to a high wave number; at 1095cm -1 Symmetrical expansion joints of C-OH exist at the position; at 1038cm -1 The characteristic absorption peak of the ether in the water-soluble silicone oil is detected, which shows that polyether siloxane is grafted on the polyurethane catheter, a strong hydrophilic end is provided, oxygen atoms in the polyether chain segment easily form hydrogen bond with water, and the hydrophilicity of the coating is enhanced.
Example 2
According to 2g:8g: uniformly mixing polyglutamic acid (Mn=5000-10000), polyvinyl alcohol PVA 1799 and deionized water according to the proportion of 20mL, stirring at 70 ℃ for reaction for 6h, and then carrying out ultrasonic vibration for 30min to obtain transparent uniform solution 1.
According to 7g:4g: and uniformly mixing polyether modified silicone oil H-204, triethanolamine and deionized water according to the proportion of 100mL to obtain transparent uniform solution 2.
Slowly adding 2 times of the volume of the solution 1 into 1 time of the volume of the solution 2 at 55 ℃, then adding sodium hexametaphosphate accounting for 0.3 percent of the weight of the mixed solution, and carrying out ultrasonic oscillation for 30 minutes to obtain the hydrophilic treatment liquid.
The polyurethane catheter was immersed in the hydrophilic treatment solution for 120s and then pulled out at a speed of 6cm/min. And after the polyurethane catheter is dried at room temperature, further vacuum drying is carried out, and the polyurethane catheter with the hydrophilic coating is obtained.
Comparative example 1
According to 10g: uniformly mixing polyvinyl alcohol PVA 1799 and deionized water according to the proportion of 20mL, stirring at 80 ℃ for reaction for 4h, and then ultrasonically oscillating for 20min to obtain transparent uniform solution 1.
According to 6g:3g: and uniformly mixing polyether modified silicone oil H-204, triethanolamine and deionized water according to the proportion of 100mL to obtain transparent uniform solution 2.
Slowly adding 2 times of the volume of the solution 1 into 1 time of the volume of the solution 2 at 45 ℃, then adding sodium hexametaphosphate accounting for 0.2 percent of the weight of the mixed solution, and carrying out ultrasonic oscillation for 20 minutes to obtain the hydrophilic treatment liquid.
The polyurethane catheter was immersed in the hydrophilic treatment liquid for 90s and then pulled out at a speed of 5 cm/min. And after the polyurethane catheter is dried at room temperature, further vacuum drying is carried out, and the polyurethane catheter with the hydrophilic coating is obtained.
Comparative example 2
According to 1g:9g: uniformly mixing polyglutamic acid (Mn=5000-10000), polyvinyl alcohol PVA 1799 and deionized water according to the proportion of 20mL, stirring at 80 ℃ for reaction for 4h, and then carrying out ultrasonic vibration for 20min to obtain transparent uniform solution 1.
According to 9g: and uniformly mixing polyether modified silicone oil H-204 and deionized water according to the proportion of 100mL to obtain transparent uniform solution 2.
Slowly adding 2 times of the volume of the solution 1 into 1 time of the volume of the solution 2 at 45 ℃, then adding sodium hexametaphosphate accounting for 0.2 percent of the weight of the mixed solution, and carrying out ultrasonic oscillation for 20 minutes to obtain the hydrophilic treatment liquid.
The polyurethane catheter was immersed in the hydrophilic treatment liquid for 90s and then pulled out at a speed of 5 cm/min. And after the polyurethane catheter is dried at room temperature, further vacuum drying is carried out, and the polyurethane catheter with the hydrophilic coating is obtained.
Comparative example 3
According to 1g:9g: uniformly mixing polyglutamic acid (Mn=5000-10000), polyvinyl alcohol PVA 1799 and deionized water according to the proportion of 20mL, stirring at 80 ℃ for reaction for 4h, and then carrying out ultrasonic vibration for 20min to obtain transparent uniform solution 1.
According to 6g:3g: and uniformly mixing polyether modified silicone oil H-204, triethanolamine and deionized water according to the proportion of 100mL to obtain transparent uniform solution 2.
Slowly adding 2 times of the volume of the solution 1 into 1 time of the volume of the solution 2 at 45 ℃, and carrying out ultrasonic oscillation for 20min to obtain a hydrophilic treatment solution.
The polyurethane catheter was immersed in the hydrophilic treatment liquid for 90s and then pulled out at a speed of 5 cm/min. And after the polyurethane catheter is dried at room temperature, further vacuum drying is carried out, and the polyurethane catheter with the hydrophilic coating is obtained.
Hydrophilic and fastness Property test
The contact angle of the polyurethane catheter was measured using an OCA200 contact angle meter from DataPhysics, germany, to evaluate the hydrophilic properties. The smaller the contact angle, the better the hydrophilic properties.
The coefficient of friction of the polyurethane catheter was performed with reference to YY/T1536-2017 non-intravascular catheter guidewire sliding performance test standard. The measurement conditions were: the water bath temperature is 37 ℃; the soaking time of the tube body is 60s; the clamping force is 3N; the pulling speed is 3.33mm/s; the test length is 50mm; the number of cycles was 30. The relative ratio of the average value of the last 5 times friction coefficient to the average value of the first 5 times friction coefficient was used as the evaluation of the fastness properties of the hydrophilic coating. The smaller the ratio, the better the fastness.
Both hydrophilic and firm performance tests used unmodified polyurethane catheters as control.
The results are shown in Table 1.
TABLE 1
| Contact angle | Relative ratio of | |
| Control group | 87.4 | 1.05 |
| Example 1 | 2.9 | 0.91 |
| Example 2 | 5.1 | 0.93 |
| Comparative example 1 | 12.5 | 1.02 |
| Comparative example 2 | 20.6 | 0.97 |
| Comparative example 3 | 17.8 | 1.04 |
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention are included in the protection scope of the present invention.
Claims (10)
1. A method for preparing a polyurethane catheter with a hydrophilic coating, comprising the steps of:
uniformly mixing polyglutamic acid, polyvinyl alcohol and deionized water, stirring for reaction, and then carrying out ultrasonic oscillation to obtain a transparent uniform solution 1;
uniformly mixing polyether modified silicone oil, triethanolamine and deionized water to obtain a transparent uniform solution 2;
slowly adding the solution 1 into the solution 2, then adding sodium hexametaphosphate into the mixed solution, and carrying out ultrasonic oscillation to obtain hydrophilic treatment liquid;
immersing the polyurethane catheter in hydrophilic treatment liquid, and then pulling out at a certain speed; and (5) drying in vacuum to obtain the polyurethane catheter with the hydrophilic coating.
2. The preparation method according to claim 1, wherein the ratio of polyglutamic acid, polyvinyl alcohol and deionized water is (0.5-2.5) g: (7-10) g:20mL.
3. The production method according to claim 1, wherein the average molecular weight mn=5000-10000 of polyglutamic acid; the polyvinyl alcohol is selected from polyvinyl alcohol PVA 1799.
4. The preparation method according to claim 1, wherein the conditions of the stirring reaction are: the reaction temperature is 60-90 ℃; the reaction time is 2-8h.
5. The preparation method according to claim 1, wherein the ratio of polyether modified silicone oil, triethanolamine and deionized water is (5-8) g: (2-5) g:100mL.
6. The preparation method according to claim 1, wherein the volume ratio of the solution 1 to the solution 2 is (2-6): 2.
7. the preparation method as claimed in claim 1, wherein the amount of sodium hexametaphosphate is 0.1 to 0.4wt% based on the weight of the mixed solution.
8. The production method according to claim 1, wherein the treatment time for immersing in the hydrophilic treatment liquid is 60 to 180 seconds.
9. The preparation method according to claim 1, wherein the speed of the pulling is 2-10cm/min.
10. Polyurethane catheter with hydrophilic coating, characterized in that it is obtained according to the preparation method of any one of claims 1 to 9.
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