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Method optimization for simultaneous separation of six triazole fungicides in HPLC
Kovač, Ishak ; Martín Miján, P. ; Del Sol Vega Alegre, M. ; Dejmková, H. ; Jaklová Dytrtová, Jana ; Schwarzová, K.
Triazole pesticides are widely used in agriculture against fungi pathogens. Their application is not restricted on just one member of the group; more importantly, the application is usually carried out in the mixture of two or more triazoles. Hence, this work focuses on simultaneous separation and detection of six triazole fungicides: penconazole, tebuconazole, propiconazole, cyproconazole, fenbuconazole, and difenoconazole. Two different columns were tested with different parameters for isocratic and gradient elution in HPLC with UV detector. On Purospher Reverse Phase-18 column with gradient elution isomers of triazoles cyproconazole and propiconazole were successfully separated. However, on this column, there was an overlap of some triazoles. In contrast, the isocratic elution on Kromasil Eternity-5-PhenylHexyl column showed sufficient separation capabilities. In further research, chiral separation of triazoles will be considered using capillary electrophoresis.
Determination of pesticide chlortoluron on carbon felt electrode
Sládková, Šárka ; Dejmková, Hana (advisor) ; Vyskočil, Vlastimil (referee)
This bachelor thesis deals with the optimization of the determination method for pesticide chlortoluron by HPLC coupled with coulometric detection on the carbon felt electrode. As the stationary phase Purospher® RP-18 column (125 x 4 mm, 5 μm) (LiChroCART) was used. The mobile phase was phosphate-acetate buffer pH 4 and methanol 40:60 and the potential applied to the working electrode was 1400 mV. The dependence of the signal on the concentration was monitored in the concentration range from 1·10-4 to 7,5·10-9 mol·dm- 3 . Firstly, this dependence was observed in deionized water. Detection limits obtained by HPLC-UV and HPLC-ED were determined to be 4,42·10-9 mol·dm-3 and 1,26·10-7 mol·dm-3 , respectively. Applicability of the method on the environmental samples was verified on model samples of river water and soil. The limits of detection of river water were determined by HPLC-UV method at 7,76·10-9 mol·dm-3 and by HPLC-ED method at 1,71·10-7 mol·dm-3 . For the soil, the limit of detection was measured by HPLC-UV at 0,198 µg·g-1 . and by method HPLC-ED it was determined as 0,135 µg·g-1 . Assays in model samples giving very similar results as in the pure solvents and this means that the matrix influence on the determination is low.
Modification of carbon felt detector with copper microparticles
Baroch, Martin ; Dejmková, Hana (advisor) ; Schwarzová, Karolina (referee)
The first aim of this work was to develop copper modified carbon felt electrode for detection of amino acids, which are not electrochemically active on ordinary carbon electrodes. Phenylalanine solution at a concentration 1.0 mmol dm-3 was chosen as the testing solution. Electrode modified with electrochemical deposition of copper from mixture of copper(II) sulphate and sodium sulphate provided very low responses which were decreasing during first measurements, apparently because of insufficient amount of copper. Therefore, further experiments were performed using copper microparticles as a modifier. Copper microparticles activated in nitric acid at a concentration 80 mmol dm-3 were applied at carbon felt by several techniques and in different parts of the felt, i.e. by stirring the felt in microparticles suspension, by dripping of the suspension to the part of the felt in contact with capillary (proximal), between two parts of the carbon felt (sandwich) and at a part of the carbon felt in contact with electrolyte in a measuring cell (distal). Electrodes modified in the distal and in the sandwich arrangement were chosen as the best ones. In the last part, calibration dependences for phenylalanine in concentration range from 0.025 mmol dm-3 to 1.0 mmol dm-3 were measured on the last two electrodes....
HPLC-ED/UV for determination of vanillylmandelic acid in human urine after solid phase extraction
Němečková-Makrlíková, Anna ; Dejmková, H. ; Navrátil, Tomáš ; Barek, J. ; Vyskočil, V.
HPLC with electrochemical and spectrophotometric detection (ED/UV) after solid phase extraction (SPE) was used for determination of vanillylmandelic acid in human urine. HPLC-ED was performed at a glassy carbon electrode in a “wall-jet” arrangement in acetate-phosphate buffer at pH = 2.5 and gradient elution (increasing content of\nacetonitrile from 5 to 25% in 10 minutes) was used. Optimized parameters were following: flow rate of mobile phase 1 mL min−1, detection potential +1.1 V, detection wavelength 279 nm, injected volume 20 μL. Dependence of the peak current on the analyte concentration was linear in the concentration range from 10 to 150 μmol L−1, with obtained limits of detection 2.6 μmol L−1 (calculated from peak height) and 1.9 μmol L−1 (calculated from peak area) for HPLC-ED, and 11.0 μmol L−1 (calculated from peak height) and 9.8 μmol L−1 (calculated from peak area) for HPLC-UV.
Determination of antioxidant activity of lichens
Jirásková, Barbora ; Dejmková, Hana (advisor) ; Schwarzová, Karolina (referee)
Antioxidant properties were studied on seven members of the Cladonia lichen family using the DPPH method, Reducing Power method, Folin-Ciocalteu method and two electrochemical methods: cyclic voltammetry (CV) and flow injection analysis (FIA) with amperometric detection.Both electrochemical methods were carried out with the use of glassy carbon electrode (GCE) and carbon paste electrode (CPE), FIA and CV were evaluated on the potential of E = 1,2 V. The carbon paste electrode turned out not to be ideal for these kinds of measurements, possibly for unknown interactions betweeen the carbon paste and the analysed extract. The inapplicability of the electrode took shape of low to zero correlation between this and most of the other methods. Evaluation of the measured data could infer that the studied Cladonia family lichens really contain substances with antioxidant properties, of which the most would probably be of phenolic type.
Utilization of potential programs in flow electrochemical determination of biologically active organic compounds
Bavol, Dmytro ; Dejmková, Hana (advisor) ; Josypčuk, Bohdan (referee) ; Metelka, Radovan (referee)
9 Abstract In this Ph.D. thesis possibilities of using our proposed potential programs for a multiple-pulse amperometry and a fast scan differential pulse voltammetry in combination with flow systems are presented. The development of new sensitive amperometric and voltammetric methods for the determination of oxidisable biologically active organic compounds is another aim of this work. In the first part of the work, the flow injection system and multiple-pulse amperometric detection were employed to develop and optimize a simple, low-cost, and rapid method for the simultaneous determination of natural and synthetic antioxidants. This technique involves the application of an appropriate potential waveform consisting of a suitable sequence of pulses on a single working electrode, thus allowing distinguish the analytes in a mixture with no need of separation. Conditions for the determination of antioxidants and modelling of the potential program were tested and studied, respectively. Second part of the work describes and characterizes the application of the fast scan differential pulse voltammetry (FSDPV) in combination with the flow systems. FSDPV is the electroanalytical technique that use high scan rate to record voltammograms within several milliseconds and ensures high temporal resolution. This technique...
Development of electroanalytical methods for detection of cholesterol and 7-dehydrocholesterol
Benešová, Lenka ; Schwarzová, Karolina (advisor) ; Dejmková, Hana (referee)
The aim of this Thesis is development of electroanalytical methods for determination of cholesterol and 7-dehydrocholesterol on boron doped diamond electrodes based on electrochemical oxidation of products of acid-induced dehydration reaction. Two approches have been applied, relying on their detection in 0,1 mol.l-1 perchloric acid in acetonitril containing variable water content 0,43 % - 40 %. Cyclic voltammetry revealed substantial difference in oxidation peak pontecials for 7-dehydrocholesterol (+850 mV) and cholesterol (+1500 mV) in 0,1 mol.l-1 perchloric acid in acetonitrile containing 5 % of water. The limit of detection using differential pulse voltammetry were 6,19 µmol.l-1 a 19,2 µmol.l-1 for a mixture of 7-dehydrocholesterol and cholesterol, respectively. For flow injection analysis with amperometric detection (FIA-AD) the water content in run buffer, detection potencial and the distance between the capillary outlet and electrode surface in wall-jet arrangement of amerometric flow-through detection cell were optimized. Achieved detection limits are in range of 0,61 - 3,43 µmol.l-1 depending on the detection potencial and water concent in the run buffer. The developed FIA-AD method was used for determination of a model mixture solution of 7- dehydrocholesterol and cholesterol. Key words...

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4 Dejmková, Hana
2 Dejmková, Helena