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Voltammetric Determination of Nimesulide Using Graphite Composite Electrode
Hubáčková, Monika ; Vyskočil, Vlastimil (advisor) ; Fischer, Jan (referee)
This Diploma Thesis deals with the study of the electrochemical behaviour of the nonsteroidal anti-inflammatory drug nimesulide. The aim of this work is to find optimal conditions for the determination of nimesulide using voltammetric techniques direct current voltammetry (DCV) and differential pulse voltammetry (DPV) in oxidation and reduction potential regions. An ultra-trace graphite electrode (UTGE) was used as the working electrode. The pH dependence was measured to select the optimal pH, the probable mechanism of reactions was determined, the repeatability of the measurements was checked, and finally the calibration dependences were constructed and evaluated in the selected media. BR buffer media of pH 2 and 4 for DCV and pH 2 and 5 for DPV were selected to measure calibration curves in the concentration range of 0.1-100 µmol L−1 . The detection limits for both methods DCV and DPV at the UTGE were in order of about 10−7 mol L−1 , which are values corresponding to alternative voltametric methods that also use unmodified working electrodes.
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Voltammetric Determination of Chloramphenicol and Chlorambucil on Amalgam Electrodes
Havlíková, Štěpánka ; Fischer, Jan (advisor) ; Zima, Jiří (referee)
This diploma thesis is focused on the determination of chloramphenicol by differential pulse voltammetry (DPV), DC voltammetry (DCV), cyclic voltammetry (CV) and adsorptive stripping voltammetry (AdSV) on a meniscus modified silver solid amalgame electrode (m- AgSAE). For the determination of chloramphenicol the optimum conditions were found and under these conditions concentration dependences were measured and then limits of quantification were determined. The influence of pH of BR buffer was tested. For determination of chloramphenicol by DCV pH 7 was chosen as an optimum background and pH 8 was chosen as an optimmum for DPV determination. Under these conditions linear dependences were obtained in the concentration range of 1·10-6 - 1·10-4 mol·l-1 . The limit of detection of chloramphenicol by DCV was 2.3·10-6 mol·l-1 . The limit of detection of chloramphenicol by DPV was 2.1·10-6 mol·l-1 in distilled water, 2.9·10-6 mol·l-1 in river water and 4.2·10-6 mol·l-1 in drinking water. Electrochemical behavior of chloramphenicol was studied by cyclic voltammetry in BR buffer with pH 2, 6, 8, 12 and then mechanism of reduction of chloramphenicol was propose based on available literature. Chloramphenicol was determined in drug Spersadex by DPV in BR buffer with pH 8. The optimal conditions for determining...
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Electrochemical Oxidation of Selected Bille Acids in Acetonitrile
Klouda, Jan ; Nesměrák, Karel (advisor) ; Rychlovský, Petr (referee)
The use of voltammetry for determining bile acids and similar compounds is described in literature, but in most cases separation precedes. The goal of this bachelor's thesis was to develop a method for direct determination and identification of seven selected bile acids. The experiments were carried out in non-aqueous medium of acetonitrile using DC voltammetry. As the working electrode a rotating disc platinum electrode and a rotating disc glassy carbon electrode were employed. Platinum electrode proved not to be suitable for this kind of use. The GCE on the other hand showed some potential, but the chemical properties of the bile acids exclude its use in terms of identification.
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The study of electrochemical reduction of chenodeoxycholic acid at stationary mercury-based electrodes
Patáková, Adéla ; Schwarzová, Karolina (advisor) ; Fischer, Jan (referee)
Chenodeoxycholic acid is the most common representative of bile acids in the human body. This work studies its electrochemical reduction at stationary mercury- based electrodes using the DC voltammetry and differential pulse voltammetry. These were performed on a silver solid amalgam electrode modified by a mercury meniscus (m-AgSAE) and a hanging mercury drop electrode (HMDE). On the scale of pH 4.0 - 12.0 offers CDCA one reduction signal in the area of highly negative potentials around −1400 mV. There is a distinctive change in the behavior of CDCA for buffers of pH lower than 6.0, compared to other pH values. This change is observable on both m-AgSAE and HMDE through the DC voltammetry and DPV methods. This happens due to protonization of carboxyl group on C24. This change is strongest with pH of 4.0. For that reason, CDCA was studied in two environments - a 0.04 mol.l−1 borat buffer (pH 9.1) - methanol (9:1) and in a BR buffer (pH 4.0) - methanol (9:1). In both environments, the lowest detection threshold has been reached through the DC voltammetry method on HMDE. The cyclic voltammetry method was used to study the electrode process. Again, measuring in pH 9.1 and pH 4.0 was done. For pH 9.1, this is a quasireversible process controlled by adsorption of both electrodes studied. For pH 4.0 is...
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Voltammetric Determination of 5-Nitroimidazole - The Structural Unit of Nitroimidazole Drugs
Šmídková, Monika ; Vyskočil, Vlastimil (advisor) ; Fischer, Jan (referee)
Presented Diploma Thesis deals with the study of electrochemical behavior of 5-nitroimidazole (5-NI), with the search for optimal conditions for its determination using techniques of DC voltammetry (DCV) and differential pulse voltammetry (DPV) at a mercury meniscus modified silver solid amalgam electrode (m-AgSAE) and at a boron-doped diamond film electrode (BDDFE), and with the comparison of reached limits of quantification (LQs). The optimal conditions found for measuring calibration dependences of 5-NI at the m-AgSAE in deionized water were as follows: Britton-Robinson buffer of pH 7.0 and 10.0 for DCV and DPV, respectively. At both thechniques, it is advisable to use an electrochemical regeneration of the electrode surface by the application of a couple of regeneration potentials Ereg,1 = 0 mV and Ereg,2 = −800 mV. The calibration dependences were measured in the concentration range from 1·10−6 to 1·10−4 mol·l−1 , with the LQs of 1.0·10−6 mol·l−1 for DCV at the m-AgSAE and 1.5·10−6 mol·l−1 for DPV at the m-AgSAE. The concentration dependences of 5-NI at the BDDFE were measured using the DCV technique in the BR buffer of pH 3.0. For the DPV technique, the optimal medium seemed to be the BR buffer of pH 2.0, however, because of the presence of an interfering peak in the supporting electrolyte,...
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Electrochemical determination of 6-thioguanine at boron doped diamond film electrod
Humpolíková, Jiřina ; Fischer, Jan (advisor) ; Schwarzová, Karolina (referee)
This master's thesis is focused on the determination of 6-thioguanine (6-T) by DC voltammetry (DCV), differential pulse voltammetry (DPV) and flow injection analysis with electrochemical detection (FIA-ED) on a boron doped diamond electrode (BDDFE). The optimum conditions for determination of 6-T were found and under these conditions, concentration dependences were measured and the limits of quantification (LOQ) were calculated for each method. Medium of 60% methanol and phosphate buffer (PB) pH 2,0 was chosen as optimum for DCV and DPV determination of 6-T at BDDFE. For both DCV and DPV, the linear concentration dependences were obtained in concentration ranges of 6-T from 2 µmol·l-1 to 10 µmol·l-1 with LOQ 0,9 µmol·l-1 for DCV and 1,5 µmol·l-1 for DPV. Lower LOQ was achieved in PB pH 2,0, where LOQ was 0,6 µmol·l-1 for both DCV and DPV, but the problem was lower repeatability. In PB pH 2 6-T was determined by DCV in drinking and river water with LOQ 1,3 µmol·l-1 in both drinking and river water. The possibility of solid phase extraction was investigated as a method for preliminary separation of 6-T from urine. For FIA under optimized conditions (polarization potential 1300 mV, flow rate 5 ml·min1 and sample volume 50 µl) the linear concentrations dependences were obtained in concentration ranges...
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Large-Surface Carbon Film Electrode - A Novel Sensor for Voltammetric Determination of Electrochemically Oxidizable Organic Compounds
Šmejkalová, Hana ; Vyskočil, Vlastimil (advisor) ; Dejmková, Hana (referee)
of the Diploma Thesis In this Diploma Thesis, the electrochemical behavior of 4-nitrophenol (4-NP) was studied at a newly prepared large-surface carbon film electrode (ls-CFE) using techniques of DC voltammetry (DCV) and differential pulse voltammetry (DPV) with the aim to develop sensitive analytical methods for its determination. Voltammetric behavior of 4-NP was investigated in the region of anodic potentials, in dependence on the pH of the medium used (realized using Britton-Robinson buffer). The optimum pH values for the determination of 4-NP were chosen as follows: pH 3.0 (for DCV) and pH 7.0 (for DPV). During anodic oxidation of 4-NP on the ls-CFE at the concentration of the analyte of 1·10-4 mol/l, the passivation of the electrode surface occurred. Thus, it was decided to record series of measurements always at a new carbon film. Using the sample of 4-NP (at the concentration of 1·10-4 mol/l), the repeatability of the application of individual carbon films was tested, with obtained RSD values of 3.7% and 3.6% for DCV and DPV, respectively. Under optimum conditions, the calibration dependences of 4-NP were measured in the concentration range from 1·10-6 to 1·10-4 mol/l, with the limits of quantification (LQs) of 1.5·10-6 mol/l (for DCV at the ls-CFE) and 4.6·10-7 mol/l (for DPV at the...
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QSPR and Electrochemical Oxidation of N-benzylsalicylthioamides
Kohoutová, Petra ; Nesměrák, Karel (advisor) ; Fischer, Jan (referee)
The study of the substituent effect on the voltammetric behaviour of newly synthesized N benzyl-salicylthioamides and the preparation and identification of products of their electrooxidation were the aims of this thesis. The voltametric characteristics were measured by DC voltammetry on a rotating disc electrode in a non-aqueous media. Using QSER, the effect of substituents on the anodic half wave potential was quantified, and statistically valid correlation equations were obtained. The influence of reaction media on the compounds electrooxidation was also studied. Using preparative electrolysis, the electrooxidation products of two selected N benzylsalicylthioamides were obtained. The one (structurally similar) product was identified in both cases. The following general scheme of electrochemical oxidation of N-benzylsalicylthioamides studied was proposed: the electrooxidation starts on sulphur atom by elimination of electrons, followed by translocation of charge on nitrogen atom, then hydrogen sulphite is eliminated, and a new ring is closed between two molecules of appropriate N-benzylsalicylthioamide.
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Voltammetric Determination of Genotoxic 2-Nitrofluorene at Screen-Printed Carbon Electrodes
Jelínková, Lenka ; Vyskočil, Vlastimil (advisor) ; Zima, Jiří (referee)
of the Bachelor Thesis Voltammetric behavior of genotoxic 2-nitrofluorene (NF) has been investigated using direct current voltammetry (DCV) and differential pulse voltammetry (DPV) at a screen- printed carbon electrode (SPCE). The optimum conditions have been found for its determination in a concentration range from 1×10−6 to 1×10−5 mol l−1 for DCV technique and from 1×10−7 to 1×10−5 mol l−1 for DPV technique. An optimum medium for DCV at the SPCE was a 0.1 mol l−1 acetate buffer of pH 4.6, an optimum time of stirring of the sample prior to the analysis was 120 s (the attained limit of quantification (LQ) was 8.5×10−6 mol l−1 of NF). For DPV at the SPCE, the optimum medium was an acidic component part of the Britton - Robinson buffer of pH 2.0; the attained LQs were 6.2×10−7 mol l−1 of NF for the concentration range from 1×10−6 to 1×10−5 mol l−1 (at the stirring time of the sample of 120 s) and 2.0×10−7 mol l−1 of NF for the concentration range from 1×10−7 to 1×10−6 mol l−1 (at the stirring time of the sample of 300 s).
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