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Elimination Voltammetry with Linear Scan: Advantages and Disadvantages
Navrátil, Tomáš ; Trnková, L. ; Hrdlička, Vojtěch ; Li, X.
Elimination voltammetry with linear scan (EVLS) represents an almost traditional\nmathematical method that helps to obtain additional and detailed information about the recorded\nelectrochemical signals and therefore, to better understand the analyzed systems. Although it\nhas been substantially developed and expanded during its existence of more than a quarter of a\ncentury and has found many areas of application, like any other mathematical and experimental\nmethod, it exhibits several advantages and disadvantages. In this contribution, we summarize\nits strengths, weaknesses, opportunities, as well as threats.\n
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Electrochemically Investigated pH-dependent Redox Properties of Copper Complexes of Azamacrocyclic Ligands
Koláčná, Lucie ; Maďar, M. ; Kubíček, V. ; Ludvík, Jiří
Investigated Cu(II) complexes are based on plain or cross-bridged cyclam. The\nelectrochemically inactive cyclam was modified by carboxylate, phosphonate, or phenolate\npendant arms. Cu(II) represents the main redox center of the complexes. Modification of the\nligand causes a changed pattern of complex redox response in buffered aqueous solution.\nIrreversible Cu(II) reduction results in complex decomposition to amalgamated copper and\nligand in excess. After Cu(0) electrochemical in situ re-oxidation, copper and ligand are recomplexed.\nComplexes undergo isomerization, accelerated by increasing the temperature. The\ninfluence of pH on complex isomerization and the reversibility of its reduction was described.
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A polarizable reference electrode
Mareček, Vladimír
New concept of a reference electrode for electrochemical systems resolves a problem of a poor \npotential stability of refence electrodes based on the distribution of a strongly \nhydrophobic common cation between two immiscible electrolyte solutions (TTTES). The use of a \npolarizable metal electrode instead of a classical reference electrode is demonstrated in \n a modified conventional four-electrode cell with TTTES. A simple battery operated potentiostat \ncontrols the working electrode potential in a three-electrode configuration. The working metal \nelectrode then serves as a polarizable reference organic solvent electrode in a four-electrode \nsystem for the polarization of the water/organic solvent interface.\n\n
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Application of In situ TR Spectroelectrochemical Techniques in Determination of Redox Mechanism of Bioactive Compounds
Sokolová, Romana ; Jiroušková, Eliška ; Degano, I. ; Wantulok, J. ; Nycz, J.
The electron transfer reactions play an important role in many natural processes. Reactions such as \ndissociation, protonation, and reactions with water and other small molecules often occur in \nbiotransformation. The reaction schemes involving these chemical reactions coupled to the \nelectron transfer can be determined by cyclic voltammetry. Additionally, in \nsitu spectroelectrochemistry can efficiently contribute to the determination of oxidation or \nreduction mechanism. This technique provides information about the electroactive chromophore during \nthe redox process allowing to identification the first reaction intermediates. The final reaction \nproducts were identified by chromatographic techniques. This study represents a key role of TR \nspectroelectrochemistry in the determination of reaction intermediates in the case of \n1,10- phenanthroline derivative substituted by bioactive phenothiazine unit and \ndrug 3- fluorophenmetrazine (2-(3-fluorophenyl)-3-methylmorpholine, 3-FPM). Co pound 3-FPM\nhave recently appeared as the new psychoactive substance in the drug market.\n
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3D Printed Microfluidic Cell for Spectroelectrochemical Analysis
Šikula, M. ; Vaněčková, Eva ; Hromadová, Magdaléna ; Kolivoška, Viliam
Recent advances in fused deposition modeling 3D printing (FDM 3DP) enabled \nthe manufacture of customized spectroelectrochemical (SEC) devices. Despite significant progress, \nreported designs still rely on conventional optical components (windows and cuvettes). In this \nwork, we apply bi-material FDM 3DP combining electrically conductive and optically \ntranslucent filaments to manufacture a fully integrated microfluidic SEC device. Employing cyclic \nvoltammetric measurements with redox probes, we demonstrate that the platform allows SEC sensing of \nreactants, intermediates, and products of charge transfer reactions in an oxygen- free \nenvironment. Developed approaches pave the way for SEC d vices with dramatically\nreduced costs compared to currently available commercial platforms.\n
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An Enzymatic Biosensor with Amperometric Detection in a Flow Injection Analysis for the Determination of L-lactic Acid: Development and Application
Tvorynska, Sofiia ; Barek, J. ; Josypčuk, Bohdan
An amperometric biosensor consisting of an enzymatic mini-reactor (lactate oxidase covalently\nattached to −NH2 functionalized mesoporous silica powder SBA−15 using glutaraldehyde) and\na silver amalgam-based screen-printed electrode acting as a transducer was developed for the\ndetermination of L-lactic acid (LA) in FIA. The detection potential of −0.9 V vs. Ag pseudoreference\nelectrode was applied for cathodic detection of enzymatically consumed oxygen.\nUnder the optimized conditions, the constructed biosensor enabled selective determination of\nLA with a micromolar limit of detection. Importantly, the proposed biosensor represented\nexcellent operational stability after ≥350 measurements. Finally, it was successfully applied to\nreal sample analysis.
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Analytical Derivatization for Identification of Electrochemical Oxidation Products of Fentanyls
Barták, P. ; Skopalová, J. ; Jerga, R. ; Štolbová, D. ; Navrátil, Tomáš ; Langmaier, Jan
Analytical derivatization and GC-MS analysis were employed for the identification of main\nproducts from the electrochemical oxidation of fentanyl derivatives. Chemical derivatization\nprovides proof of the chemical reactivity of functional groups in oxidation products and serves\nfor the chemical conversion of target compounds into the second series of derivatives to confirm\nthe identification of particular products. Using the direct GC-MS analysis of oxidation products,\nderivatization of aldehydes with cysteamine and derivatization of amides by acidic hydrolysis\nand subsequent reaction with ethylchloroformiate, phenylacetaldehyde, and Nphenylpropanamide\nwere unambigously identified as oxidation products from fentanyl,\nthiophen-2-ylacetaldehyde, and N-phenylpropanamide from sufentanil, and\nphenylacetaldehyde and 2-furanilid from furanylfentanyl.
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