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The Use of New Types of Carbon Electrodes for Voltammetric Determination of Organic Compounds
Birhanzlová, Tereza ; Barek, Jiří (advisor) ; Labuda, Ján (referee) ; Ludvík, Jiří (referee)
This Ph.D. thesis is focused on the use of a new type of non-toxic electrode (carbon film electrode - CFE) for voltammetric determination of environmental organic pollutants and on the development and use of a new type of solid electrode modified with carbon nanotubes for the determination of 2-nitrophenol (2-NP) and 8-nitroquinoline (8-NQ). The work is a continuation of the previous study of 5- nitroquinoline (5-NQ) using CFE in author's bachelor and diploma thesis. The determination of 5-NQ based on anodic oxidation is not possible at CFE and thus 2-NP was chosen as a model substance for voltammetric determination in both regions of potential window (cathodic and anodic). Further attention was paid to the development of a new type of carbon electrode with surface containing carbon nanotubes and its application for the determination of 8-NQ using differential pulse voltammetry (DPV) based on cathodic reduction of present nitro group. Silver solid electrode (AgE) as a substrate electrode for following modification was used. At first, the AgE itself was used for determination of 8-NQ in deionized water and in model samples of drinking and river water. Then the possibility of electrode surface modification using different type of carbon nanotubes was investigated. The AgE modified with carboxylated...
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Development of electrochemical methods for study of antibacterial compounds in small volumes
Gajdár, Július ; Barek, Jiří (advisor) ; Šiškanova, Tatiana (referee) ; Labuda, Ján (referee)
Main goal of this Ph.D. thesis is to develop voltammetric methods for the electrochemical study of novel antimycobacterial compounds hydroxynaphthalene- carboxamides. Firstly, this study was focused on the miniaturization of voltammetric methods and construction of an electrochemical microcell due to usually small volume of samples that are associated with an analysis of biologically active compounds in biological matrices. Therefore, all aspects of the voltammetric procedure were studied in a relation to miniaturization. Microcells were based on commercially available electrodes: glassy carbon electrode as a reliable electrode material with well-described characteristics and a novel silver solid amalgam electrode. This study was carried out with analytes 4-nitrophenol, pesticide difenzoquat, and 1-hydroxy-N-(4-nitrophenyl)naphthalene-2-carboxamide. Attention was paid especially to the optimization of oxygen removal procedures in the drop of a solution. Developed miniaturized methods had the same parameters for the determination of studied compounds as in bigger volumes. The proposed electrochemical microcell can be generally used for voltammetric analysis of those samples of biological or environmental origin that are usually available in very limited volumes. Second part of the thesis was focused...
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Development of Novel Electrochemical Methods Using Various Membrane Materials for Monitoring of Selected Anticancer Drugs and Phytochelatins
Skalová, Štěpánka ; Barek, Jiří (advisor) ; Labuda, Ján (referee) ; Trnková, Libuše (referee)
Present Ph.D. Thesis is focused on the development of electrochemical methods for determination of anticancer drugs using various types of membranes for their preliminary separation. Furthermore, this Thesis reports the study of transport mechanisms of heavy metals in the presence of phytochelatins across biological membranes. Sodium anthraquinone-2-sulphonate (AQS) was used as a model compound for its similar structure with anthraquinone-based (AQ-based) anticancer drugs (doxo/daunorubicin) and also due to its better availability. All these compounds can be easily electrochemically oxidized and/or reduced. Redox behaviour of AQS was investigated by cyclic voltammetry (CV) and differential pulse voltammetry (DPV) in a cathodic region on mercury meniscus modified (m-AgSAE) and polished silver solid amalgam (p-AgSAE) electrodes, Obtained results were used for the development of a micro-volume voltammetric cell (MVVC). Its applicability for voltammetric determination of anticancer drugs was verified by using doxorubicin (DX) as a model substance. The second part of this Thesis deals with therapeutic monitoring of anticancer drugs in the blood circulation of the patients. For pilot experiments, a liquid-flow system with dialysis catheter and amperometric detection was used. The flow rate of carrier...
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Voltammetric Techniques for Analysis in a Single Drop of a Solution
Gajdar, J. ; Goněc, T. ; Jampílek, J. ; Brázdová, Marie ; Bábková, Zuzana ; Fojta, Miroslav ; Barek, J. ; Fischer, J.
This contribution describes miniaturization of voltammetric methods and some of the main problems caused by reducing the sample volume to 20 mu L. This study was carried out in dimethyl sulfoxide solutions and buffered aqueous solutions with 10% DMSO at a glassy carbon electrode. A novel antibiotic agent, 1-hydroxy-N-(4-nitrophenyl) naphthalene-2-carboxamide, was used as a model substance. This analyte was determined by cathodic and anodic voltammetry. Elimination of the negative influence of dissolved oxygen was performed in various manners. Two most effective methods were square wave voltammetry that can be used in the presence of dissolved oxygen and removal of oxygen in a microcell with nitrogen atmosphere inside.
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Construction and Application of Flow Amperometric Biosensor Based on Enzymatic Reactor for Determination of Choline
Tvorynska, Sofiia ; Barek, J. ; Josypčuk, Bohdan
In this contribution, a novel fast, simple and stable biosensor with the enzymatic reactor based on choline oxidase (ChOx) was developed and applied for the determination of choline using flow injection analysis with amperometric detection. The preparation of the reactor is based on the covalent immobilization of ChOx with glutaraldehyde to mesoporous silica powder (SBA-15) previously covered by NH2-groups. The experimental parameters affecting the sensitivity and stability of the biosensor were optimized. The proposed biosensor with the newly developed ChOx-based reactor possesses good repeatability, reproducibility, long-term stability, and reusability. It was successfully applied for the determination of choline in commercial pharmaceuticals.
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Electrochemical Enzymatic Biosensors for Determination of Catecholamines in Flow Systems\n
Josypčuk, Bohdan ; Barek, J. ; Josypčuk, Oksana
Several biosensors (BS) based on flow enzymatic mini-reactors containing a mesoporous silica powder covered by enzyme laccase or tyrosinase were used for determination of L-DOPA, dopamine, noradrenaline, and adrenaline. The silica powder of MCM-41 with covalently bonded laccase was found to be the best reactor filling for the detection of catecholamines. Relative current response of such BS was 100 % for dopamine, 32.1 % for L-DOPA, 26.2 % for noradrenaline, and 0.71 % for adrenaline. The practical applicability of Lac-MCM41 biosensor was successfully verified by the determination of dopamine and noradrenaline in medical solutions for infusions.
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