Lubricant and Anti-fouling Coatings for Silicone Catheter

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范曉梅(Pham Thi Mai) 查詢紙本館藏

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化學工程與材料工程學系

論文名稱

(Lubricant and Anti-fouling Coatings for Silicone Catheter)

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至系統瀏覽論文 (2029-7-31以後開放)

摘要(中)

矽膠具有優異的機械性質、低毒性和低生產成本，因此廣泛應用在醫療領域。然而，矽膠的疏水性在人體植入過程中會引發生物污損問題，限制其應用性。為了解決此困境，本研究採用簡單而有效的兩步塗層工藝來提升矽膠導管的表面性能。
第一層作為基底層，將矽膠導管浸泡在由四種單體合成之共聚物溶液中，各具特定功能： 2-甲基丙烯醯氧基乙基三甲基氯化銨 (TMAEMA) 為季銨鹽，具有抗菌性能；甲基丙烯酸十二烷基酯 (DMA) 可促進與矽膠表面間的疏水作用力；3-甲基丙烯醯氧基-2-羥丙基-4-氧基二苯甲酮 (MHPBP) 含有苯甲酮基團，能在紫外線照射下通過烴基插入交聯反應 (CHic) 與矽膠表面進行交聯；乙烯基吡咯烷酮 (NVP) 作為除氧劑，可提高交聯效率。
隨後，在基底層上以兩種不同的溶液作為功能性塗層，分別是聚乙烯吡咯烷酮(PVP) 及含有2-甲基丙烯醯氧基乙基磷醯膽鹼和甲基丙烯酸十二烷基酯的共聚物 (MPC-DMA)，這些溶液用於誘導矽膠表面使其具有親水性和抗污性。本研究詳述合成共聚物的方法，並使用水接觸角儀、摩擦力測試、FTIR和AFM對塗層表面進行鑑定及分析，這些分析證實雙層塗層在矽膠表面的成功塗佈。此外，還進行細菌黏附測試、蛋白質吸附測試、溶血測試和細胞毒性測試，以評估塗層矽膠表面的抗污和生物相容性。結果顯示，PVP和MPC-DMA在上述實驗中具有卓越的性能，適合作為仿生的矽膠基材醫用塗層。

摘要(英)

Silicone is a widely used material in medical applications due to its excellent mechanical properties, low toxicity, and low production cost. However, the hydrophobicity of silicone limits its medical implementation due to biofouling concerns which can cause challenges during prolonged human implantation. In this study, a simple and effective two-step coating process was employed to enhance the surface properties of silicone catheters. In the first step for the primer layer, silicone catheters were immersed in a solution containing a copolymer. This copolymer, synthesized from four monomers, serves distinct functions: 2-methacryloyloxy ethyl trimethylammonium chloride (TMAEMA) acts as a quaternary ammonium, known for its antibacterial properties; dodecyl methacrylate (DMA) facilitates hydrophobic-hydrophobic interactions with the silicone surface; 3-methacryloyloxy-2-hydroxypropyl-4-oxybenzophenone (MHPBP) contains a benzophenone group that can induce crosslinking with silicone surface under UV irradiation condition via C-H insertion crosslinking reactions (CHic); and n-vinyl-2-pyrrolidone (NVP) acts as oxygen scavenger to make the crosslinking efficiency. Subsequently, in the second step for functional layer, the two distinct solutions were utilized: one comprising polyvinylpyrrolidone (PVP) and the other containing a copolymer (2-methacryloyloxy phosphorylcholine-co-dodecyl methacrylate) (MPC-DMA). These solutions were employed to induce hydrophilic and antifouling properties on the silicone surface. The methods to synthesize copolymers were also described. Furthermore, the coated surfaces were characterized using water contact angle measurements (WCA), friction test, Fourier-transform infrared spectroscopy (FTIR), and atomic force microscope (AFM). These characterization techniques confirmed the successful deposition of dual layers onto the silicone surface and allowed assessment of their surface properties. Additionally, bacterial adhesion test, protein adsorption test, hemolysis test, cytotoxicity test, and encrustation test were conducted to evaluate the anti-fouling and biocompatibility abilities of the coated silicone surface. Following all the tests, both PVP and MPC-DMA exhibited good lubricity, excellent antifouling, and biocompatibility properties, rendering them suitable as medical coatings on silicone substrates.

關鍵字(中)

★ 矽膠
★ 醫療塗層
★ 烴基插入交聯反應 (CHic)
★ 聚乙烯吡咯烷酮 (PVP)
★ 2-基丙烯醯氧基乙基磷醯膽鹼 (MPC)
★ 3-甲基丙烯醯氧基-2-羥丙基-4-氧基二苯甲酮 (MHPBP)

關鍵字(英)

★ Silicone
★ Medical coatings
★ C-H insertion crosslinking reaction (CHic)
★ Polyvinylpyrrolidone (PVP)
★ 2-methacryloyloxy phosphorylcholine (MPC)
★ 3-methacryloyloxy-2-hydroxypropyl-4-oxybenzophenone (MHPBP)

論文目次

Table of Contents
中文摘要 ii
Abstract iii
Acknowledgment v
Table of Contents vi
List of figures ix
List of tables xi
List of Abbreviations xii
Chapter 1. Introduction 1
1.1. Silicone material 1
1.1.1. Silicone and its medical applications 1
1.1.2 Problems with silicone in biomedical implants 3
1.1.2.1 Bacterial biofilm infections 3
1.1.2.2 Nonspecific protein adsorption 4
1.1.3 Catheter - associated urinary tract infection (CAUTI) 6
1.2 Anti-fouling materials 7
1.2.1 Poly (ethylene glycol) (PEG) 7
1.2.2 Poly(N-vinylpyrrolidone) (PVP) 8
1.2.3 Zwitterionic polymer 9
1.3 Methods for modifying silicone surface 11
1.3.1 Photoinduced-grafting method 12
1.3.2 MHPBP and C, H-insertion crosslinking reaction (CHic) 14
Chapter 2. Research objective 16
Chapter 3. Materials and methods 18
3.1 Materials and equipment 18
3.1.1 Materials 18
3.1.2 Equipment 21
3.2 Material preparations 22
3.2.1 Synthesis of 3-methacryloyloxy-2-hydroxypropyl-4-oxybenzophenone (MHPBP) 22
3.2.2 Synthesis of TDMN random copolymer 23
3.2.3 Synthesis of random MD copolymer and P(MPC) polymer 24
3.2.4 Preparation of silicone catheter 25
3.2.5 Preparation of LB agar and LB broth 25
3.2.5.1 Preparation of LB agar 25
3.2.5.2 Preparation of LB Broth 25
3.3 Methods 25
3.3.1 Hydrogen-1 Nuclear Magnetic Resonance (1H-NMR) 25
3.3.2 Gel permeation chromatography (GPC) 26
3.3.3 Attenuated total reflectance (ATR-FTIR) for catheter surface characterization 26
3.3.4 Water contact angle measurement (WCA) 26
3.3.5 Surface tension of the coating solution 27
3.3.6 Viscosity of the coating solution 27
3.3.7 Atomic Force Microscope (AFM) 28
3.3.8 Preliminary lubricity test 28
3.3.9 Dynamic friction coefficient test 28
3.3.10 Hemolysis test 29
3.3.11 Bacterial adhesion test 30
3.3.12 Protein adsorption test 31
3.3.13 Cytotoxicity test 32
3.3.14 Encrustation test 33
3.4 Standard coating procedure 35
3.4.1 Range of coating component concentration. 35
3.4.2 Standard coating procedure. 35
Chapter 4. Results 36
4.1 Hydrogen-1 Nuclear Magnetic Resonance (1H-NMR) results 36
4.1.1 1H-NMR result of MHPBP monomer 36
4.1.2 1H-NMR result of TDMN copolymer 37
4.1.3 1H-NMR result of MPC-DMA copolymer (P(MPC-DMA)) 39
4.2 Lubricious coatings and dynamic friction coefficient test. 41
4.2.1 One-step coating process on silicone catheter. 41
4.2.2 Two-steps coating process on silicone catheter. 43
4.2.2.1 TDMN/PVP coating and dynamic friction coefficient test. 44
a) Investigation of different coating component for TDMN/PVP 44
b) Investigation of different UV irradiation time for TDMN/PVP 48
c) Investigation of different drying temperature for TDMN/PVP 49
4.2.2.2 TDMN/MD coating and dynamic friction coefficient test. 52
a) Investigation of different coating component for TDMN/MD 52
b) Investigation of different UV irradiation time for TDMN/MD coating 57
c) Investigation of different drying temperature for TDMN/MD 59
4.2.3 Optimal coating conditions for TDMN/PVP and TDMN/MD coatings 61
4.3 Stability of the coatings in DI water and PBS solution 62
4.4 Viscosity and surface tension of the coating solutions 65
4.5 Surface characterization for modified silicone catheter 66
4.5.1 Attenuated total reflectance (ATR-FTIR) for catheter surface characterization 66
4.5.2 Topography of the coatings on the silicone surface by AFM 67
4.5.3 Water contact angle 69
4.6 Anti-fouling test for unmodified/modified silicone catheters 70
4.6.1 Bacterial adhesion test 70
4.6.2 Protein adsorption test 72
4.7 Hemolysis test 73
4.8 Biocompatibility of the modified silicone catheter 74
4.9 Encrustation test of the unmodified/modified silicone 75
Chapter 5. Conclusions 78
Chapter 6. Future works 79
References 80

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指導教授

黃俊仁(Chun-Jen Huang)

審核日期

2024-7-18

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