臺灣博碩士論文加值系統

近年來，抗生素藥物被廣泛的應用於臨床與畜牧業。不僅如此，在現代農藥中也廣泛的使用以提高農業的產能。然而，大量使用抗生素藥物與農藥將會為人類帶來嚴重的環境及水體的品質問題。因此，如何有效應用抗生素藥物或是農藥並監測生物和環境樣品中這些有毒成分的於環境中的含量成為科學界的重要議題。而開發電化學感測器並利用其特性以檢測生物與環境樣品中的有毒或是有機成分顯得十分重要。本邊研究最主要研究：如何利用貴金屬與稀土金屬碳複合金屬氧化物進行電催化用以感測抗生素藥物和有機污染物。將貴金屬和稀土金屬氧化物以共沉澱法及超音合成法與碳製成複合金屬。採用金屬氧化物作為碳載體可提高感測器的催化活性、導電性與物理化學性質。
研究人員投入開發先進以及且具優異電化學性能電催化劑最為有機農藥殘留與抗生素藥物感測。貴金屬和稀土金屬氧化物憑藉其物理化學特性在電化學感測器中引起大家的關注。透過共沉澱法將銀摻入卡羅姆硬幣結構氧化鈷（Ag-Co3O4 NPs），以作為細胞毒性替硝唑（TNZ）的電化學感測。Ag-Co3O4 NPs 修飾電極廢水樣品感測中對TNZ有著低檢測極限、良好的靈敏度、高穩定性以及可觀的回收率。而稀土釤金屬掛載的氧化鈷奈米顆粒（SmCoO3）其特異性與靈敏度以檢測抗精神病藥物：鹽酸異丙嗪（PHY）。由SmCoO3所修飾的電極具有高導電性、寬廣的動態線性範圍、高靈敏度並對PHY有著的良好的檢測極限。即便是在污水中也可獲得良好的回收率。透過超音波法將氧化石墨烯（GO）與錫酸鏑納米片（Dy2Sn2O7）疊合，做為蔬菜樣品中的克百威（CF）電化學檢測材料，從解果中，我們可獲得良好的回收率。接著將感測器應用於奈莫耳級的克百威檢測，並驗證感測器的靈敏度和儲存穩定性。再來將具功能化的碳奈米球 (FCNS)用於製備氧化钆用於環境樣品中的多菌靈 (CBZ) 檢測。以15天做為間格進行實例應用分析，從解果得知所製作的感測器擁有優秀的回收率。將摻入氧化石墨烯 (AgZrO2/GO) 的鋯酸銀奈米薄片利用共沉澱和超音合成進行製備。將修飾電極作為綠原酸（CGA）的特異性和靈敏性感測，經修飾的電極對 CGA有著良好的電催化活性，有著高的靈敏度、寬廣的線性範圍、低檢測極限、高穩定性以及良好的選擇性並在感測生物樣品與水樣品中的CGA時展現出了高回收率。

Recently, antibiotic drugs are widely applicable by many users including clinical and animal husbandry. On the other hand, pesticides are also extensively used in the modern forming to deliver high yield harvest in agriculture. However, the extensive usage of antibiotic drug and pesticide residues could cause severe issues for human beings and affects the quality of environmental and aqueous samples. Thus, the serious impacts of antibiotic drugs and organic pesticides are a prominent topic in the scientific community. Therefore, there is necessary for monitoring the environmental levels of those toxic components in the biological and environmental samples. Instead, the electrochemical sensor is a key method for sensing the toxic/organic components from the biological and environmental samples due to its remarkable properties. This thesis mainly focused on the synthesis and electrocatalytic investigation of various noble and rare earth metal-reinforced metal oxides with carbon composite for electrochemical detection of antibiotic drugs and organic pollutants. The noble and rare earth metal-reinforced metal oxides with carbon composite metal via familiar co-precipitation and ultrasonication methods. The purpose of carbon support in the metal oxides is to boost their catalytic activity, conductivity, and physicochemical properties of the sensor.
Recently, the researcher's are focused on the development of various advanced or newly designed electrocatalyst for the investigation of organic pesticide residues and antibiotic drugs with exceptional electrochemical performance. Specifically, noble and rare earth metal-supported metal oxides were achieved significant interest in the electrochemical sensor due to their remarkable physicochemical characteristics. Therefore, firstly, we designed a silver metal incorporated carrom coin structured cobalt oxide (Ag-Co3O4 NPs) through a simple co-precipitation method and implemented it for the electrochemical detection of cytotoxic Tinidazole (TNZ). The Ag-Co3O4 NPs modified electrode showed a low detection limit, good sensitivity, stability, and appreciable recovery for TNZ in various wastewater samples. Further, the size confined rare earth samarium metal-supported cobalt oxide nanoparticle (SmCoO3) was employed for the specific and sensitive detection of antipsychotic drug promethazine hydrochloride (PHY). The SmCoO3 modified electrode depicts high conducting property, wide dynamic linear range, sensitivity, and good limit of detection toward PHY. Also, given a good recovery result in the presence of various real-time samples. Then, the interlayer effect of graphene oxide (GO) incorporated with dysprosium stannate nanoplatelets (Dy2Sn2O7) was prepared through a facile co-precipitation followed by an ultrasonication method for the electrochemical detection of Carbofuran (CF) in vegetable samples with an acceptable recovery level of CF. In addition, it has given a nanomolar of detection, sensitivity, and excellent storage stability toward the CF. Next, gadolinium oxide (Gd2O3) was prepared with the support of functionalized carbon nanosphere (FCNS) for a portable detection of Carbendazim (CBZ) pesticide in aqueous environmental samples. The real-time application was studied with an in-time interval of 15 days and obtained an acceptable recovery level for the practical applications. Likewise, silver zirconate nanoflakes incorporated with graphene oxide (AgZrO2/GO) was prepared by co-precipitation followed ultrasonication. The modified electrode was employed for the specific and sensitive detection of chlorogenic acid (CGA). The modified electrode improved electrocatalytic activity towards CGA and exhibited higher sensitivity, a wide linear range, a lower limit of detection, appreciable stability, and good selectivity. In addition, the proposed sensor was depicted the appreciable recovery level of CGA in the biological and water samples.

摘要………………………………………………………………………………………………..i
Abstract…………………………………………………………………………………………...iii
CERTIFICATE…………………………………………………………………………………..vi
DECLARATION………………………………………………………………………………..vii
ACKNOWLEDGEMENT………………………………………………………………………viii
Chapter 1 Introduction………………………………………………………………………….....1
1.1 General introduction…………………………………………………………………...1
1.2 Electrochemical sensing……………………………………………………………….3
1.2.1 Conductance and impedance………………………………………………...5
1.2.2 Types of (ECS)………………………………………………………………5
1.2.3 Potentiometry/Voltammetry…………………………………………………8
1.2.4 Choosing of electrodes system……………………………………………….9
1.2.5 Types of voltammetry………………………………………………………..9
1.2.6 Cyclic voltammetry………………………………………………………...10
1.2.7 Differential pulse voltammetry…………………………………………….11
1.2.8 Amperometric sensor………………………………………………………11
1.3 Materials for working electrode………………………………………………………12
1.3.1 Metal and metal oxides……………………………………………………..12
1.3.2 Transition and rare earth metal oxides……………………………………...12
1.4 Binary metal oxides (BMO)…………………………………………………….........14
1.4.1 MOs and BMOs with carbon support……………………….………………14
1.5 Various carbon supports……………………………………………………………...15
1.5.1 Graphene oxide……………………………………………………………..15
1.5.2 Functionalized carbon nanosphere…………………………………………16
1.6 Various analytes……………………………………………………………………...16
1.6.1 Pharmaceuticals…………………………………………………………….17
1.6.1.1 Antibiotic drugs…………………………………………………………..18
1.6.1.2 Antihistamic drug………………………………………………………...19
1.6.2 Pesticides…………………………………………………………………...19
1.6.3 Fungicides………………………………………………………………….20
1.7 Scope of the present work……………………………………………………….........21
1.8 References……………………………………………………………………………23
Chapter 2 Experimental and characterization methods………………………………………….34
2.1Experimental materials and reagents………………………………………………….34
2.2 Synthesis of binary noble and rare earth metal oxide…………………………………34
2.2.1 Synthesis of Carrom coins Ag-Co3O4 NPs………………………………….34
2.2.2 Synthesis of SmCoO3 NPs………………………………………………….36
2.3 Synthesis of binary noble and rare earth metal oxide with carbon composites….........37
2.3.1 Synthesis and fabrication of Dy2Sn2O7/GO composite…………………….37
2.3.2 Preparation and modification of Gd2O3/F-CNS composite…………………39
2.3.3 Synthesis of Ag-ZrO2/GO composite and electrode modification………….40
2.4 Material characterizations……………………………………………………………41
2.4.1 Raman spectroscopy………………………………………………………..41
2.4.2 Fourier transfer infrared spectroscopy……………………………………...42
2.4.3 X-ray diffraction……………………………………………………………43
2.4.4 X-ray photoelectron spectroscopy………………………………………….44
2.4.5 Field emission scanning electron microscopy………………………………44
2.4.6 High resolution transmission electron microscopy…………………………45
2.4.7 Energy-dispersive X-ray spectroscopy……………………………………..46
2.5 Electrochemical characterization………………………………………………….....47
2.6 References…………………………………………………………………………....47
Chapter 3 Novel electrochemical methods for detection of cytotoxic Tinidazole in aqueous media……………………………………………………………………………..…49
3.1 Introduction ……………………………………………………………………..…..50
3.2 Experimental section…………………………………………………………………53
3.2.1 Reagents and materials……………………………………………………..53
3.2.2 Sample collection and storage……………………………………………...53
3.2.3 Synthesis of carrom coins Ag-Co3O4 NPs………………………………….54
3.2.4 Electrode fabrication of Ag-Co3O4 NPs……………………………………55
3.2.5 Characterization of carrom coins structured Ag-Co3O4 NPs........................56
3.3 Result and discussions………………………………………………………………..57
3.3.1 P-XRD, Raman, and FTIR analysis………………………………………...57
3.3.2 XPS analysis………………………………………………………………..58
3.3.3 Morphological studies……………………………………………………... 60
3.3.4 Electrochemical optimization………………………………………………63
3.3.5 Amperometric i-t response of Ag-Co3O4 NPs/GCE towards TNZ………….73
3.3.6 Studies of reproducibility, repeatability, and stability of the sensor………...77
3.3.7 Application…………………………………………………………………78
3.3.7.1 Electrochemical determination of TNZ in water and wastewater samples.78
3.4 Conclusion……………………………………………………………………………82
3.5 References……………………………………………………………………………83
Chapter 4 Designing of perovskite structured samarium cobalt trioxide nanoparticles (SmCoO3 NPs): Regulated as an effective and reliable platform for nanomolar level promethazine hydrochloride………………………………………………………………………….95
4.1 Introduction…………………………………………………………………………..96
4.2 Experimental section ……………………………………………………………99
4.2.1 Materials and reagents …………………………………………………….99
4.2.2 Characterization and electrochemical techniques ……………………….....99
4.2.3 Synthesis of SmCoO3 NPs………………………………………………...101
4.2.4 Fabrication of SmCoO3 NPs modified glassy carbon electrode ………,…101
4.3 Result and discussion………………………………………………………………..102
4.3.1 Characterization of SmCoO3 NPs…………………………………………102
4.3.2. Morphological investigation of SmCoO3 NPs …………………………...104
4.4 Electrochemical analysis…..………………………………………………………..107
4.4.1 Electrochemical behavior of SmCoO3/GCE towards PHY…..……………107
4.4.2 Differential Pulse Voltammetry (DPV) analysis of PHY through SmCoO3/GC………………………………………………………...…………..113
4.4.3 Real-time monitoring……………………………………………………..118
4.5 Conclusion………………………………………………………………………….121
4.6 References……………………………………………………………………..........122
Chapter 5 Rational design and interlayer effect of dysprosium-stannate nanoplatelets incorporated graphene oxide: A versatile and competent electrocatalyst for toxic carbamate pesticide detection in vegetables……..……………………………………………………….131
5.1 Introduction…..……………………………………………………………………..132
5.2 Experimental section…..……………………………………………………………135
5.2.1 Materials and reagents. …………………………………………………...135
5.2.2 Material characterizations..……………………………………………….135
5.2.3 Synthesis of Dy2Sn2O7 nanoplatelets...……………………………………136
5.2.4 Synthesis and fabrication of Dy2Sn2O7/GO composite……………………137
5.3 Results and discussions.……………………………………………………….........138
5.3.1 Structural analysis………………………………………………………...138
5.4 Electro-chemical performance, redox property, and catalytic activity of CF………..144
5.5 Kinetic effects of scan rate and pH……………………………………………..........150
5.6 Determination of CF, interference, and stability analysis…………………………...152
5.7 Real-time analysis of CF…………………………………………………………….157
5.8 Conclusion……………………………………………………………………..........159
5.8 References…………………………………………………………………………..160
Chapter 6 Influence of gadolinium oxide with functionalized carbon nanosphere: A portable advanced electrocatalyst for carbendazim pesticide detection in Aqueous environmental samples……………………………………………………………...170
6.1 Introduction………………………………………………………………………....171
6.2 Experimental section ………………………………………………………………..174
6.2.1 Materials ………………………………………………………………….174
6.2.2 Preparation of Gd2O3 and functionalized carbon nanospheres …………...174
6.2.3 Preparation and modification of Gd2O3/F-CNS composite..……………...175
6.2.4 Characterization …………………………………………………………..176
6.2.5 Electrochemical experiments ……………………………………………..177
6.3 Results and discussion………………………………………………………………177
6.3.1 Structural analysis ………………………………………………………...177
6.3.2 Electrocatalytic analysis …………………………………………………..183
6.3.3 Electrochemical investigation of CBZ ……………………………………186
6.3.4 Optimizations ……………………………………………………………..189
6.3.5 DPV determination of CBZ ………………………………………………193
6.3.6 Reproducibility, repeatability, and stability ………………………………196
6.3.7 Practical application ………………………………………………………198
6.4 Conclusion …………………………………………………………………………206
6.5 References ………………………………………………………………………….206
Chapter 7 A portable advanced electrocatalyst for chlorogenic acid evaluation in real-time samples……………………………………………………………………………...214
7.1 Introduction ………………………………………………………………………...215
7.2 Experimental section………………………………………………………………..218
7.2.1 Materials………………………………………………………………......218
7.2.2 Synthesis of Ag-ZrO2 and GO…………………………………………....219
7.2.3 Synthesis of graphene oxide……………………………………………....220
7.2.4 Synthesis of Ag-ZrO2/GO composite and electrode modification………. 220
7.2.5 Modification of Ag-ZrO2/GO composite………………………………... 221
7.2.6 Characterization………………………………………………………….. 221
7.2.7 Electrochemical experiments…………………………………………….. 222
7.3 Results and discussions…………………………………………………………….. 222
7.3.1 Structural characterizations of Ag-ZrO2/GO nanocomposite……………. 222
7.3.2 Electrocatalytic analysis………………………………………………….. 229
7.3.3 Electrochemical investigation of CGA…………………………………... 231
7.3.4 Optimizations…………………………………………………………….. 231
7.3.5 DPV determination of CGA……………………………………………… 237
7.3.6 Reproducibility, repeatability, and stability……………………………… 239
7.3.7 Practical application……………………………………………………… 241
7.4 Conclusion………………………………………………………………………… 244
7.5 References…………………………………………………………………………..244
Chapter 8 Summary and conclusion……………………………………………………….…...255
List of publications………………………………………………………………....260

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Chapter-6
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Chapter-7
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