Tracheal tube with antibacterial lubricating function and preparation method thereof
An antibacterial and lubricating endotracheal tube was prepared by combining oxygen plasma treatment with modified polyethyleneimine, tannic acid and modified fucoidan, which solved the problem of insufficient antibacterial and lubricating properties of traditional tubes and achieved long-lasting lubrication and antibacterial performance.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-04
- Publication Date
- 2026-03-31
AI Technical Summary
Existing endotracheal tubes are inadequate in terms of antibacterial properties and lubrication, resulting in high friction during intubation, which can easily cause patient discomfort and increase the risk of infection. In addition, traditional lubricants are prone to falling off and their lubrication effect is not long-lasting.
Oxygen plasma treatment is used to increase the polar groups on the material surface. Modified polyethyleneimine and tannic acid are combined to form a composite antibacterial coating. A hydrophilic lubricating coating is formed by N-vinylpyrrolidone and modified fucoidan. The coating is firmly adhered by electrostatic action.
It improves the antibacterial activity and lubrication properties of endotracheal tubes, reduces friction, enhances coating adhesion and durability, and reduces infection risk and coefficient of friction.
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Figure CN120514932B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of biomedical materials technology, specifically to a tracheal tube with antibacterial and lubricating functions and its preparation method. Background Technology
[0002] Endotracheal intubation is an important emergency and treatment procedure. By inserting a medical endotracheal tube through the mouth or nose into the airway, it ensures a clear airway and allows for mechanical ventilation. This technique is widely used in clinical treatments such as cardiopulmonary resuscitation, respiratory medicine, and anesthesiology, and can be used to manage respiratory failure, airway obstruction, and loss of consciousness. Currently, commonly used endotracheal tubes are mainly made of polymer materials such as silicone rubber, polyvinyl chloride (PVC), and polydimethylsiloxane (PDMS). These materials are widely used in the manufacture of medical consumables and medical devices due to their ease of processing, high toughness, and high stability.
[0003] Endotracheal intubation is widely used in clinical practice, but currently used endotracheal tubes still have shortcomings in terms of antibacterial properties and lubrication. The materials of traditional endotracheal tubes are not mechanically compatible with human soft tissue, resulting in high friction during intubation. This can easily cause strong discomfort to patients, such as coughing and sore throat. This friction can also cause edema or inflammation of the airway wall, further leading to problems such as difficulty speaking and swallowing. Furthermore, traditional tubes lack antibacterial properties, allowing bacteria and other organisms to easily adhere to the tube surface, forming a biofilm and causing tube contamination. This can not only lead to local infections but also cause the spread of pathogens, resulting in systemic infections and increasing the risk of ventilator-associated pneumonia (VAP).
[0004] Regarding lubrication, while the use of lubricants can reduce airway irritation from intubation to some extent, traditional lubricants such as lidocaine gel only adhere to the tube surface for a short time, resulting in limited lubrication. During intubation, the lubricant is gradually consumed due to contact and friction between the tube and surrounding tissues, leading to a weakening of the lubrication effect. Furthermore, residual lubricant may affect postoperative airway function. In recent years, the application of super-lubricating coating technology has improved the lubrication of endotracheal tubes to some extent, but the adhesion and durability of this coating still need improvement. Summary of the Invention
[0005] To address the shortcomings of existing technologies, the present invention aims to provide a tracheal tube with antibacterial and lubricating functions and its preparation method.
[0006] To achieve the above objectives, the present invention adopts the following technical solution:
[0007] In a first aspect, the present invention provides a method for preparing a tracheal tube with antibacterial and lubricating functions, comprising the following steps:
[0008] S1. Preparation of pre-treated endotracheal tubes
[0009] The tracheal tube to be processed is placed in an oxygen plasma instrument for activation treatment to obtain a pre-processed tracheal tube.
[0010] In this step, the endotracheal tube is made of polyvinyl chloride, silicone rubber, or polydimethylsiloxane.
[0011] In this step, the gas flow rate for oxygen plasma treatment is 100-150 sccm, for example, 100 sccm, 105 sccm, 110 sccm, 115 sccm, 120 sccm, 125 sccm, 130 sccm, 135 sccm, 140 sccm, 145 sccm, or 150 sccm can be selected; the treatment power is 100-300W, for example, 100W, 150W, 200W, 250W, or 300W can be selected; the treatment time is 3-10 min, for example, 3 min, 4 min, 5 min, 6 min, 7 min, 8 min, 9 min, or 10 min can be selected; the treatment pressure is 10-100 Pa, for example, 10 Pa, 20 Pa, 30 Pa, 40 Pa, 50 Pa, 60 Pa, 70 Pa, 80 Pa, 90 Pa, or 100 Pa can be selected, but it is not limited to the listed values, and other unlisted values within the range are also applicable.
[0012] In this step, the materials used for the endotracheal tube are mostly hydrophobic. This invention treats the material surface with oxygen plasma to introduce oxygen-containing groups such as hydroxyl and carboxyl groups into the material surface. The increase of these polar groups makes the material surface more hydrophilic and also enhances the bonding strength with the coating.
[0013] S2, Preparation of modified polyethyleneimine
[0014] Polyethyleneimine and 2,3-epoxypropyltrimethylammonium chloride were added to deionized water and heated and stirred to react. After the reaction was completed, the mixture was dialyzed and freeze-dried to obtain modified polyethyleneimine.
[0015] In this step, the mass ratio of polyethyleneimine to 2,3-epoxypropyltrimethylammonium chloride is 5-10:8-12. For example, 5:8, 5:10, 5:12, 6:10, 8:8, 8:10, 8:12, 10:8, 10:11, and 10:12 can be selected, but it is not limited to the listed values. Other unlisted values within the range are also applicable.
[0016] In this step, the temperature for heating and stirring the reaction is 70-85℃, for example, 70℃, 75℃, 80℃, or 85℃ can be selected; the reaction time is 8-16h, for example, 8h, 10h, 12h, 14h, 15h, or 16h can be selected, but it is not limited to the listed values. Other unlisted values within the range are also applicable.
[0017] In this step, dialysis is performed using a dialysis membrane with a molecular weight cutoff of 1000 Da to remove unreacted 2,3-epoxypropyltrimethylammonium chloride.
[0018] Polyethyleneimine has abundant amino groups (primary, secondary, and tertiary amines), which can chemically bond with polar groups (such as carboxyl and hydroxyl groups) on the surface of the substrate. For example, amino groups can form amide bonds with carboxyl groups and hydrogen bonds with hydroxyl groups, thereby enhancing the adhesion between PEI and the substrate. In this invention, 2,3-epoxypropyltrimethylammonium chloride is used to modify polyethyleneimine, thereby enhancing the antibacterial properties of polyethyleneimine.
[0019] S3. Preparation of antibacterial modified endotracheal tubes
[0020] Modified polyethyleneimine and tannic acid were added to deionized water, mixed evenly, and then immersed in the pretreated tracheal tube for soaking treatment. After removal, the tube was cured to obtain an antibacterial modified tracheal tube.
[0021] In this step, the mass ratio of modified polyethyleneimine, tannic acid, and deionized water is 1-3:0.5-1.5:100. For example, 1:0.5:100, 1:1:100, 1:1.5:100, 2:0.5:100, 2:1:100, 2:1.5:100, 3:0.5:100, 3:1:100, and 3:1.5:100 can be selected, but it is not limited to the listed values. Other unlisted values within the range are also applicable.
[0022] In this step, the curing temperature is 100-120℃, for example, 100℃, 105℃, 110℃, 115℃, or 120℃ can be selected; the curing time is 1-2h, for example, 1h, 1.5h, or 2h can be selected, but it is not limited to the listed values. Other unlisted values within the range are also applicable.
[0023] In this invention, modified polyethyleneimine and tannic acid are used as a composite antibacterial coating, which makes the endotracheal tube have good antibacterial activity against a variety of bacteria and can effectively inhibit the adhesion and growth of bacteria. At the same time, tannic acid also has good adhesion properties, which allows the composite antibacterial coating to adhere firmly to various substrates, ensuring that the coating has long-lasting antibacterial properties.
[0024] S4. Preparation of endotracheal tubes with antibacterial and lubricating functions
[0025] N-vinylpyrrolidone and modified fucoidan were added to an ethanol aqueous solution, followed by an initiator. The mixture was stirred until homogeneous to obtain a coating solution. The antibacterial modified tracheal tube was then immersed in the coating solution, removed, and subjected to ultraviolet crosslinking under nitrogen protection. After washing and drying, the tracheal tube with antibacterial and lubricating functions was obtained.
[0026] In this step, the mass ratio of N-vinylpyrrolidone, modified fucoidan, aqueous ethanol solution, and initiator is 10-15:3-6:100:0.5-1.
[0027] Specifically, the initiator is selected from benzophenone, 3-methylbenzophenone or 4-methylbenzophenone.
[0028] Specifically, the preparation method of the modified fucoidan is as follows: fucoidan is dissolved in deionized water to obtain an aqueous phase; acryloyl chloride and triethylamine are dissolved in dichloromethane to obtain an organic phase; under nitrogen protection, the organic phase is added dropwise to the aqueous phase, and the reaction is stirred. After the reaction is completed, precipitation, washing, vacuum drying, and grinding are performed to obtain the modified fucoidan.
[0029] More specifically, the mass ratio of fucoidan, acryloyl chloride and triethylamine is 5-10:4-6:2-3.
[0030] More specifically, the stirring reaction is carried out at room temperature for 4-8 hours.
[0031] In this step, the UV light intensity during UV crosslinking is 150-200 mW / cm². 2 The UV crosslinking time is 90-120s.
[0032] In this step, fucoidan is a natural water-soluble polysaccharide extracted from brown algae, mainly composed of L-fucose and sulfate groups. This invention first modifies it to introduce double bonds, then uses N-vinylpyrrolidone and modified fucoidan as functional monomers. After UV-initiated polymerization, a hydrophilic lubricating coating is obtained. The sulfate groups in the hydrophilic lubricating coating are negatively charged and can attract the quaternary ammonium cations in the antibacterial coating through electrostatic interaction, thus firmly fixing the hydrophilic lubricating coating to the surface of the tracheal tube. Compared to the easy detachment of a single polyvinylpyrrolidone (PVP) hydrophilic coating, this invention effectively solves the problem of easy detachment of the hydrophilic coating. Simultaneously, the fucoidan provided by this invention also has good anti-protein adhesion properties, and together with N-vinylpyrrolidone, it improves the anti-protein adhesion effect of the tracheal tube.
[0033] The present invention also provides a tracheal tube with antibacterial lubrication function prepared by the above preparation method.
[0034] Compared with the prior art, the present invention has the following beneficial effects:
[0035] (1) The present invention uses oxygen plasma to treat the surface of the material, and introduces oxygen-containing groups such as hydroxyl and carboxyl groups into the surface of the material. The increase of these polar groups makes the surface of the material more hydrophilic, and also enhances the bonding strength with the coating.
[0036] (2) In this invention, 2,3-epoxypropyltrimethylammonium chloride is first used to modify polyethyleneimine to enhance its antibacterial properties. Then, modified polyethyleneimine and tannic acid are used as a composite antibacterial coating, which makes the tracheal tube have good antibacterial activity against a variety of bacteria and can effectively inhibit the adhesion and growth of bacteria. At the same time, tannic acid also has good adhesion properties, which makes the composite antibacterial coating firmly adhered to various substrates, ensuring that the coating has long-lasting antibacterial properties.
[0037] (3) Fucoidan is a natural water-soluble polysaccharide extracted from brown algae, mainly composed of L-fucose and sulfate groups. In this invention, fucoidan is first modified to introduce double bonds. Then, N-vinylpyrrolidone and modified fucoidan are used as functional monomers. After UV-initiated polymerization, a hydrophilic lubricating coating is obtained. The cross-linked hydrophilic lubricating coating is a hydrogel with an interpenetrating network structure. This structure can absorb and retain moisture in a humid environment, forming a stable lubricating layer on the surface. Even after repeated friction and long-term use, it can still maintain low friction. The friction coefficient is improved, and the sulfate groups in the hydrophilic lubricating coating are negatively charged, which can attract the quaternary ammonium salt cations in the antibacterial coating through electrostatic interaction, so that the hydrophilic lubricating coating is firmly fixed on the surface of the tracheal tube. Compared with the easy detachment of the single polyvinylpyrrolidone (PVP) hydrophilic coating, the present invention effectively solves the problem of easy detachment of the traditional hydrophilic coating and has a better lubrication effect. At the same time, the fucoidan provided by the present invention also has good anti-protein adhesion properties, and works together with N-vinylpyrrolidone to improve the anti-protein adhesion effect of the tracheal tube. Attached Figure Description
[0038] Figure 1 The graph shows the antibacterial performance test results for different groups;
[0039] Figure 2 The graph shows the test results of friction performance for different groups;
[0040] Figure 3 The graph shows the test results of the anti-protein adhesion performance of different groups. Detailed Implementation
[0041] The present invention will be further described in detail below through specific preferred embodiments, but the present invention is not limited to the following embodiments.
[0042] It should be noted that, unless otherwise specified, all chemical reagents involved in this invention were purchased through commercial channels.
[0043] The endotracheal tube used in this embodiment of the invention is made of PVC; the average relative molecular mass of polyethyleneimine is 3000.
[0044] Example 1
[0045] A method for preparing an endotracheal tube with antibacterial and lubricating functions includes the following steps:
[0046] S1. Place the tracheal tube to be treated in an oxygen plasma instrument and activate it. The gas flow rate of the oxygen plasma treatment is 100 sccm, the power of the treatment is 150W, the treatment time is 5min, and the treatment pressure is 50Pa to obtain the pretreated tracheal tube.
[0047] S2. Add 5g of polyethyleneimine and 8g of 2,3-epoxypropyltrimethylammonium chloride to 100mL of deionized water, heat and stir at 85℃ for 8h. After the reaction is complete, dialyze with a dialysis membrane with a molecular weight cutoff of 1000Da for 24h to remove unreacted 2,3-epoxypropyltrimethylammonium chloride, and then freeze-dry to obtain modified polyethyleneimine.
[0048] S3. Add 1g of modified polyethyleneimine and 0.5g of tannic acid to 100mL of deionized water, mix well, then immerse the pretreated tracheal tube in the solution for 5 minutes. After removing the tube, cure it at 120℃ for 1 hour to obtain the antibacterial modified tracheal tube.
[0049] S4. Add 10g of N-vinylpyrrolidone and 3g of modified fucoidan to 100g of 40wt% ethanol aqueous solution, then add 0.5g of benzophenone and mix well to obtain a coating solution. Immerse the antibacterial modified endotracheal tube in the coating solution, remove it after 5 minutes, and perform ultraviolet crosslinking under nitrogen protection. The ultraviolet light intensity is 150mW / cm. 2 The UV cross-linking time is 120s, and then after washing and drying, a tracheal tube with antibacterial and lubricating functions is obtained.
[0050] The modified fucoidan is prepared as follows: 5g of fucoidan is dissolved in 50mL of deionized water to obtain an aqueous phase; 4g of acryloyl chloride and 2g of triethylamine are dissolved in 20mL of dichloromethane to obtain an organic phase; under nitrogen protection, the organic phase is added dropwise to the aqueous phase, and the mixture is stirred at room temperature for 6h. After the reaction is complete, the mixture is precipitated, washed, vacuum dried, and ground to obtain the modified fucoidan.
[0051] Example 2
[0052] A method for preparing an endotracheal tube with antibacterial and lubricating functions includes the following steps:
[0053] S1. Place the tracheal tube to be treated in an oxygen plasma instrument and activate it. The gas flow rate of the oxygen plasma treatment is 150 sccm, the power of the treatment is 100W, the treatment time is 10min, and the treatment pressure is 50Pa to obtain the pretreated tracheal tube.
[0054] S2. Add 10g of polyethyleneimine and 12g of 2,3-epoxypropyltrimethylammonium chloride to 100mL of deionized water, heat and stir at 70℃ for 16h. After the reaction is complete, dialyze with a dialysis membrane with a molecular weight cutoff of 1000Da for 24h to remove unreacted 2,3-epoxypropyltrimethylammonium chloride, and then freeze-dry to obtain modified polyethyleneimine.
[0055] S3. Add 1g of modified polyethyleneimine and 1g of tannic acid to 100mL of deionized water, mix well, then immerse the pretreated tracheal tube in the solution for 5 minutes, remove it and cure it at 120℃ for 1 hour to obtain the antibacterial modified tracheal tube.
[0056] S4. Add 15g of N-vinylpyrrolidone and 6g of modified fucoidan to 100g of a 40wt% ethanol aqueous solution, then add 1g of benzophenone and mix well to obtain a coating solution. Immerse the antibacterial modified endotracheal tube in the coating solution, remove it after 5 minutes, and perform ultraviolet crosslinking under nitrogen protection. The ultraviolet light intensity is 200mW / cm. 2 The UV cross-linking time is 90s, and then after washing and drying, a tracheal tube with antibacterial and lubricating functions is obtained.
[0057] The modified fucoidan is prepared as follows: 5g of fucoidan is dissolved in 50mL of deionized water to obtain an aqueous phase; 4g of acryloyl chloride and 2g of triethylamine are dissolved in 20mL of dichloromethane to obtain an organic phase; under nitrogen protection, the organic phase is added dropwise to the aqueous phase, and the mixture is stirred at room temperature for 6h. After the reaction is complete, the mixture is precipitated, washed, vacuum dried, and ground to obtain the modified fucoidan.
[0058] Example 3
[0059] A method for preparing an endotracheal tube with antibacterial and lubricating functions includes the following steps:
[0060] S1. Place the tracheal tube to be treated in an oxygen plasma instrument for activation treatment. The gas flow rate of the oxygen plasma treatment is 100 sccm, the power of the treatment is 300W, the treatment time is 3min, and the treatment pressure is 50Pa to obtain the pretreated tracheal tube.
[0061] S2. Add 8g of polyethyleneimine and 10g of 2,3-epoxypropyltrimethylammonium chloride to 100mL of deionized water, heat and stir at 80℃ for 12h. After the reaction is complete, dialyze with a dialysis membrane with a molecular weight cutoff of 1000Da for 24h to remove unreacted 2,3-epoxypropyltrimethylammonium chloride, and then freeze-dry to obtain modified polyethyleneimine.
[0062] S3. Add 3g of modified polyethyleneimine and 1.5g of tannic acid to 100mL of deionized water, mix well, then immerse the pretreated tracheal tube in the solution for 5 minutes, remove it and cure it at 120℃ for 1 hour to obtain the antibacterial modified tracheal tube.
[0063] S4. Add 12g of N-vinylpyrrolidone and 4g of modified fucoidan to 100g of a 40wt% ethanol aqueous solution, then add 0.8g of benzophenone and mix well to obtain a coating solution. Immerse the antibacterial modified endotracheal tube in the coating solution, remove it after 5 minutes, and perform ultraviolet crosslinking under nitrogen protection. The ultraviolet light intensity is 200mW / cm. 2 The UV cross-linking time is 90s, and then after washing and drying, a tracheal tube with antibacterial and lubricating functions is obtained.
[0064] The modified fucoidan is prepared as follows: 10g of fucoidan is dissolved in 100mL of deionized water to obtain an aqueous phase; 6g of acryloyl chloride and 3g of triethylamine are dissolved in 40mL of dichloromethane to obtain an organic phase; under nitrogen protection, the organic phase is added dropwise to the aqueous phase, and the mixture is stirred at room temperature for 8 hours. After the reaction is complete, the mixture is precipitated, washed, vacuum dried, and ground to obtain the modified fucoidan.
[0065] Comparative Example 1
[0066] A method for preparing an endotracheal tube with antibacterial and lubricating functions includes the following steps:
[0067] S1. Place the tracheal tube to be treated in an oxygen plasma instrument and activate it. The gas flow rate of the oxygen plasma treatment is 100 sccm, the power of the treatment is 150W, the treatment time is 5min, and the treatment pressure is 50Pa to obtain the pretreated tracheal tube.
[0068] S2. Add 1g of polyethyleneimine and 0.5g of tannic acid to 100mL of deionized water, mix well, then immerse the pretreated tracheal tube in the solution for 5 minutes. After removing the tube, cure it at 120℃ for 1 hour to obtain an antibacterial modified tracheal tube.
[0069] S3. Add 10g of N-vinylpyrrolidone and 3g of modified fucoidan to 100g of 40wt% ethanol aqueous solution, then add 0.5g of benzophenone and mix well to obtain a coating solution. Immerse the antibacterial modified endotracheal tube in the coating solution, remove it after 5 minutes, and perform ultraviolet crosslinking under nitrogen protection. The ultraviolet light intensity is 150mW / cm. 2 The UV cross-linking time is 120s, and then after washing and drying, a tracheal tube with antibacterial and lubricating functions is obtained.
[0070] The modified fucoidan is prepared as follows: 5g of fucoidan is dissolved in 50mL of deionized water to obtain an aqueous phase; 4g of acryloyl chloride and 2g of triethylamine are dissolved in 20mL of dichloromethane to obtain an organic phase; under nitrogen protection, the organic phase is added dropwise to the aqueous phase, and the mixture is stirred at room temperature for 6h. After the reaction is complete, the mixture is precipitated, washed, vacuum dried, and ground to obtain the modified fucoidan.
[0071] Compared to Comparative Example 1 and Example 1, no modification treatment was performed on the polyethyleneimine.
[0072] Comparative Example 2
[0073] A method for preparing an endotracheal tube with antibacterial and lubricating functions includes the following steps:
[0074] S1. Place the tracheal tube to be treated in an oxygen plasma instrument and activate it. The gas flow rate of the oxygen plasma treatment is 100 sccm, the power of the treatment is 150W, the treatment time is 5min, and the treatment pressure is 50Pa to obtain the pretreated tracheal tube.
[0075] S2. Add 5g of polyethyleneimine and 8g of 2,3-epoxypropyltrimethylammonium chloride to 100mL of deionized water, heat and stir at 85℃ for 8h. After the reaction is complete, dialyze with a dialysis membrane with a molecular weight cutoff of 1000Da for 24h to remove unreacted 2,3-epoxypropyltrimethylammonium chloride, and then freeze-dry to obtain modified polyethyleneimine.
[0076] S3. Add 1g of modified polyethyleneimine and 0.5g of tannic acid to 100mL of deionized water, mix well, then immerse the pretreated tracheal tube in the solution for 5 minutes. After removing the tube, cure it at 120℃ for 1 hour to obtain the antibacterial modified tracheal tube.
[0077] S4. Add 10g of N-vinylpyrrolidone to 100g of a 40wt% ethanol aqueous solution, then add 0.5g of benzophenone and mix well to obtain a coating solution. Immerse the antibacterial modified endotracheal tube in the coating solution and remove it after 5 minutes. Perform ultraviolet crosslinking under nitrogen protection with an ultraviolet light intensity of 150mW / cm.2 The UV cross-linking time is 120s, and then after washing and drying, a tracheal tube with antibacterial and lubricating functions is obtained.
[0078] Compared with Example 1, no fucoidan was added in Comparative Example 2.
[0079] Comparative Example 3
[0080] A method for preparing an endotracheal tube with antibacterial and lubricating functions includes the following steps:
[0081] S1. Place the tracheal tube to be treated in an oxygen plasma instrument and activate it. The gas flow rate of the oxygen plasma treatment is 100 sccm, the power of the treatment is 150W, the treatment time is 5min, and the treatment pressure is 50Pa to obtain the pretreated tracheal tube.
[0082] S2. Add 5g of polyethyleneimine and 8g of 2,3-epoxypropyltrimethylammonium chloride to 100mL of deionized water, heat and stir at 85℃ for 8h. After the reaction is complete, dialyze with a dialysis membrane with a molecular weight cutoff of 1000Da for 24h to remove unreacted 2,3-epoxypropyltrimethylammonium chloride, and then freeze-dry to obtain modified polyethyleneimine.
[0083] S3. Add 1g of modified polyethyleneimine and 0.5g of tannic acid to 100mL of deionized water, mix well, then immerse the pretreated tracheal tube in the solution for 5 minutes. After removing the tube, cure it at 120℃ for 1 hour to obtain the antibacterial modified tracheal tube.
[0084] S4. Add 10g of N-vinylpyrrolidone and 3g of fucoidan to 100g of a 40wt% ethanol aqueous solution, then add 0.5g of benzophenone and mix well to obtain a coating solution. Immerse the antibacterial modified endotracheal tube in the coating solution, remove it after 5 minutes, and perform ultraviolet crosslinking under nitrogen protection. The ultraviolet light intensity is 150mW / cm. 2 The UV cross-linking time is 120s, and then after washing and drying, a tracheal tube with antibacterial and lubricating functions is obtained.
[0085] Compared with Example 1, Comparative Example 3 did not involve any modification treatment of fucoidan.
[0086] The endotracheal tube samples prepared in Example 1 and Comparative Examples 1-3 were subjected to performance tests, as detailed below:
[0087] Antibacterial performance test
[0088] The endotracheal tube samples prepared in Example 1 and Comparative Examples 1-3 were cut open to make 0.5cm × 0.5cm samples, and placed in one well of a 24-well multi-well culture plate to fully expose the inner surface. A suspension of *E. coli* bacteria (density 10⁻⁶) was then placed in the plate. 6 CFU / mL) at 3cm 2 Droplets were applied to the sample surface at a ratio of / ml, and then incubated at 37℃ for 24 hours. The bacterial suspension incubated with the experimental material was diluted 1000-fold, and 50 μL of each diluted suspension was evenly spread onto solid bacterial culture (NA) plates and incubated at 37℃ for 24 hours. Bacterial counts were obtained, and the antibacterial rate was calculated. The test was performed three times, and the average result was taken. The test results are shown below. Figure 1 As shown, from Figure 1 As can be seen, in Comparative Example 1, no modification treatment was performed on the polyethyleneimine, resulting in a significant reduction in its antibacterial properties.
[0089] Friction performance test
[0090] The lubrication performance of the surface coatings of the samples prepared in Example 1 and Comparative Examples 1-3 was tested using a pin-disc friction tester. The friction pairs were the prepared sample (0.5cm×0.5cm) and a steel ball (6mm in diameter). The coefficient of friction was measured by linear reciprocating motion in deionized water at room temperature. The applied load was 5N, the sliding speed was set to 5mm / s, and the test was performed 3 times. The average value of the results was taken.
[0091] Durability test: The samples prepared in Example 1 and Comparative Examples 1-3 were immersed in deionized water at 37°C for 7 days, dried, and then subjected to friction performance tests as described above. The test results are as follows: Figure 2 As shown, from Figure 2 As can be seen, when not soaked, the friction coefficients of the samples in Example 1 and Comparative Examples 1-3 are not significantly different because they are covered with a hydrophilic coating. However, after soaking, the hydrophilic coating on the surface of the samples prepared in Comparative Examples 1-3 begins to peel off, resulting in a significant increase in the friction coefficient. The coating prepared in the present invention has good stability.
[0092] Anti-protein adhesion performance test
[0093] The samples prepared in Example 1 and Comparative Examples 1-3 were incubated with 0.1 mg / mL fibrinogen at 37°C for 2 h. After rinsing with PBS, the adhered proteins were ultrasonically eluted in 2 wt% sodium dodecyl sulfate solution. The protein concentration was measured using a BCA protein concentration assay kit, and the amount of protein adhesion was calculated. The test was performed 3 times, and the average value of the results was taken.
[0094] The samples prepared in Example 1 and Comparative Examples 1-3 were then immersed in deionized water at 37°C for 7 days, dried, and then subjected to anti-protein adhesion performance tests according to the above method.
[0095] Test results are as follows Figure 3 As shown, from Figure 3 As can be seen from the data, Comparative Example 2 did not contain fucoidan, and its anti-protein adhesion performance was significantly reduced. Compared with Comparative Examples 1 and 3, the sample prepared in the present invention still has good anti-protein adhesion performance after soaking treatment.
[0096] Finally, it should be noted that the above embodiments do not limit the present invention in any way. Those skilled in the art can make modifications and improvements based on the present invention. Therefore, any modifications or improvements made without departing from the spirit of the present invention are within the scope of protection claimed by the present invention.
Claims
1. A method for producing an endotracheal tube having an antibacterial lubricating function, characterized by, It comprises the following steps: S1, placing the gas tube to be treated into an oxygen plasma instrument, exciting and activating to obtain a pretreated gas tube; S2, adding polyethyleneimine and 2,3-epoxypropyltrimethylammonium chloride into deionized water, heating and stirring to react, after the reaction is completed, dialysis, freeze-drying to obtain modified polyethyleneimine; S3, adding the modified polyethyleneimine and tannic acid into deionized water, mixing uniformly, then immersing into the pretreated gas tube, soaking, taking out and solidifying to obtain an antibacterial modified gas tube; S4, adding N-vinylpyrrolidone and modified fucoidan into an aqueous ethanol solution, then adding an initiator, mixing uniformly to obtain a coating liquid, immersing the antibacterial modified gas tube into the coating liquid, then taking out, performing ultraviolet crosslinking under nitrogen protection, then washing and drying to obtain a gas tube with antibacterial and lubricating functions; The preparation method of the modified fucoidan is as follows: dissolving fucoidan in deionized water to obtain an aqueous phase; dissolving acryloyl chloride and triethylamine in dichloromethane to obtain an organic phase; under nitrogen protection, adding the organic phase dropwise into the aqueous phase, stirring to react, after the reaction is completed, performing precipitation, washing, vacuum drying and grinding to obtain the modified fucoidan.
2. The production method according to claim 1, characterized by, In step S1, the gas flow of the oxygen plasma treatment is 100-150 sccm, the power of the treatment is 100-300 W, the treatment time is 3-10 min, and the gas pressure of the treatment is 10-100 Pa.
3. The preparation method according to claim 1, characterized in that, In step S2, the mass ratio of polyethyleneimine and 2,3-epoxypropyltrimethylammonium chloride is 5-10:8-12.
4. The method of claim 1, wherein, In step S2, the heating and stirring reaction temperature is 70-85℃, and the reaction time is 8-16 h.
5. The preparation method according to claim 1, characterized in that, In step S3, the mass ratio of the modified polyethyleneimine, tannic acid and deionized water is 1-3:0.5-1.5:
100.
6. The method of claim 1, wherein, In step S4, the mass ratio of N-vinylpyrrolidone, modified fucoidan, aqueous ethanol solution and initiator is 10-15:3-6:100:0.5-1, wherein the initiator is selected from benzophenone, 3-methylbenzophenone or 4-methylbenzophenone.
7. The preparation method according to claim 1, characterized in that, The mass ratio of fucoidan, acryloyl chloride and triethylamine is 5-10:4-6:2-3.
8. The method of claim 1, wherein, In step S4, the UV light intensity was 150-200 mW / cm 2 and the UV crosslinking time was 90-120 s.
9. The gas tube with antibacterial and lubricating functions prepared by the preparation method of any one of claims 1-8.
Citation Information
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