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研究生： 柯翰
Ko, Han
論文名稱： 藉由配位子-金屬電荷轉移躍遷提升氧化鐵奈米材料光子能量轉換用於光熱抗菌以及複合性癌症光療法
Enhanced photon energy conversion of iron oxide nanomaterials via ligand-to-metal charge transfer process for photothermal antibacterial activity and combined phototherapy
指導教授： 黃志嘉
Huang, Chih-Chia
學位類別： 碩士
Master
系所名稱： 理學院 - 光電科學與工程學系
Department of Photonics
論文出版年： 2018
畢業學年度： 106
語文別： 英文
論文頁數： 112
中文關鍵詞： 氧化鐵奈米材料 、配位子-金屬電荷轉移 、光熱治療 、光熱抗菌 、癌症光療法
外文關鍵詞： IONP, LMCT, photothermal therapy, antibacterial activity, cancer therapy
相關次數： 點閱：130  下載：0 
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    • 在此篇研究中，我們研究藉由單寧酸與鐵離子的電荷轉移特性以提升商業化的氧化鐵奈米粒子的光熱轉換效率。這是首篇提出以表面修飾富含電子的配位子以配位子—金屬電荷轉移（LMCT）的效應提升光熱轉換效果的研究。水熱合成過程中，我們也首次觀察到磁赤鐵礦（γ-Fe2O3）和磁鐵礦（Fe3O4）於水相系統中相轉換反應，有別以往於高溫高壓固態環境底下的氧化鐵相轉換反應。在此結果上，我們提出了一種簡單且符合綠色化學的方法合成出包含光學活性以及磁性響應的單寧酸修飾氧化鐵奈米粒子（IONP-TNA）。此研究以穿隧式電子顯微鏡（TEM）觀察奈米粒子形貌並計算其粒徑大小分佈，以X-ray繞射分析儀（XRD）以及顯微搭載拉曼光譜儀研究氧化鐵的晶體結構。並以傅里葉轉換紅外光譜（FTIR）、熱重分析（TGA）以及X光光電子能譜儀（XPS）研究奈米粒子表面化學。在光學性質的探討上，我們研究氧化鐵奈米粒子的紫外－可見光吸收光譜（UV-vis）、光熱轉換效應以及轉換效率計算。同時，此研究也將探討不同反應條件如溫度、劑量以及不同種類的氧化鐵或茶多酚進行合成修飾，以說明此研究之通用性。
    在應用端，我們應用IONP-TNA於近紅外雷射照激發光熱抗菌以及結合亞甲基藍分子（MB）作為光敏劑對於膀胱癌細胞進行複合型光治療。在光熱抗菌方面，此研究以甘露糖分子（d-mannose）修飾於IONP-TNA上（IONP-TNA@Man）作為大腸桿菌（E. coli）標靶分子，並以808 奈米近紅外光激發IONP-TNA@Man產生侷限域的高熱殺死鄰近細菌，對於不同種類的大腸桿菌如出血性的O157:H7及抗藥性的ESBL皆有良好的光熱抗菌效果。在癌症複合光療法方面，IONP-TNA展現良好的光敏藥物攜載率並提升光敏藥物於不同環境中的穩定性。此外，其具有降低細胞中穀胱甘肽的效果，作為抵抗細胞內的抗氧化劑藉以提升光動力治療效果。在癌症光熱／光動力複合治療下達到良好的療效。其高度的r2弛緩率也展現了作為核磁共振成像（MRI）顯影劑的潛能，達到結合治療與診斷的功效。

    The photon absorption enhancement inducing photothermal conversion via interfacial ligand-to-metal charge transfer (LMCT) was first proposed in this study. Through a wet-chemistry hydrothermal process of tannic acid (TNA) and commercial iron oxide (γ-Fe2O3) nanoparticles (γ-IONP(c)), the phase transformation from γ-Fe2O3 to form Fe3O4 material. UV-visible, FT-IR, and TGA measurements determined 6.1 % TNA molecules immobilized onto the surface of IONPs (IONP-TNA). Such ligand-assisted complex effect showed an absorption enhancement in the wide visible-NIR wavelengths via interfacial LMCT effect between TNA and IONPs. The different TNA concentrations and reaction temperatures were further studied for demonstrating the preferred co-precipitation and self-assembly of TNA with Fe3+ ions on the NPs surface.
    IONP-TNA was further modified with d-mannose (IONP-TNA@Man) to increase binding affinity toward the membrane molecules of Escherichia coli (E. coli). IONP-TNA@Man could efficiently accumulate on the different strains of E. coli and produce the localized hyperthermia to destroy the bacteria surface directly upon an excitation with a NIR laser. It also sterilized well against Gram-positive bacteria, as the model of Staphylococcus aureus (S. aureus). Considering of eco-friendly concept, IONP-TNA@Man could recycle via external magnetic field-integrated PTA treatment. We prepared methylene blue (MB)-immobilized IONP-TNA (IONP-TNA@MB) for executing combined photothermal-photodynamic therapy (PDT). IONP-TNA@MB was stable in different environment and could deplete the glutathione (GSH), a natural PDT physiological barrier. As an employment of 660 nm light, IONP-TNA@MB acted as a therapeutic nano-mediator for inducing cancer cell death via the iron oxide-mediated phototherapy.

    1. Introduction 1 1.1 Iron oxide nanoparticles 1 1.1.1 Type of iron oxide nanoparticles 1 1.1.2 Phase transformation of iron oxide 2 1.1.3 Optical and band structure of iron oxide nanoparticles 2 1.2 Ligand-to-metal charge transfer systems 4 1.2.1 Interfacial charge transfer in semiconductor applications 4 1.2.2 Metal-phenolic materials 5 1.2.3 Tannic acid 6 1.3 Phototherapy 7 1.3.1 Photothermal therapy in nanotechnology 7 1.3.2 Photothermal therapy with iron oxide nanoparticles 8 1.3.3 Photodynamic therapy 11 1.3.4 Phototherapy with iron oxide in cancer treatment 13 1.4 Antibacterial Activity 14 1.4.1 The antibiotic abuse--problem and solution 14 1.4.2 The adhesion and infection of bacteria 14 1.4.3 The mechanism of antibacterial nanotechnology 15 1.4.4 Antibacterial activity with iron oxide nanoparticles 16 2. Motivation 28 3. Method and Materials 30 3.1 Materials 30 3.2 Equipment 32 3.3 Synthesis and preparations Methods 33 3.3.1 Synthesis of IONP-TNA 33 3.3.2 Synthesis of IONP-TNA@Man 33 3.3.3 Photothermal conversion effect measurement 33 3.3.4 Bacteria incubation method 34 3.3.5 Photothermal antibacterial activity 34 3.3.6 Methylene blue conjugating on IONP-TNA 35 3.3.7 Cell viability of PTT combined PDT against T24 cell 35 3.3.8 Glutathione depletion ability of IONP-TNA@MB 35 3.3.9 Lipid peroxidation of T24 cell after PDT treatment 36 3.3.10 Photothermal conversion efficiency calculation 36 4. Results and discussion 39 4.1 Characteristics 39 4.1.1 Structure of tannic acid immobilized Fe3O4 NPs 39 4.1.2 Optical performance of IONP-TNA 43 4.1.3 TNA immobilization on different type of IONP 45 4.1.4 Synthesis of different polyphenol immobilization 46 4.1.5 Magnetism of iron oxide nanoparticles 46 4.1.6 D-mannose modified iron oxide nanoparticles 46 4.1.7 Ascorbic acid reducing iron oxide nanoparticles 47 4.1.8 Gram-scale synthesis of IONP-TNA 48 4.2 Antibacterial activity 49 4.2.1 Antibacterial activity of TNA and nanomaterials 49 4.2.2 Photothermal antibacterial activity against E. coli 49 4.2.3 The bacteria adhesion study 51 4.2.4 Photothermal antibacterial activity of S. aureus 52 4.2.5 The confirmation of localized hyperthermia 53 4.2.6 Recycle photothermal antibacterial activity 54 4.2.7 Biocompatibility of iron oxide nanoparticles 54 4.3 Combined phototherapy for bladder cancer 55 4.3.1 IONP-TNA as photosensitizer carrier (IONP-TNA@MB) 55 4.3.2 Photothermal and singlet oxygen generation ability of IONP-TNA@MB 56 4.3.3 In vitro cell viability study – MTT assay 57 4.3.4 Cell morphology study – in situ bright field image 58 4.3.5 GSH depletion ability of IONP-TNA@MB 59 4.3.6 The mechanism study – membrane peroxidation 59 5. Conclusion 96

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