National Repository of Grey Literature 73 records found  1 - 10nextend  jump to record: Search took 0.00 seconds. 
Analysis of unstable complexes for study of enzymatic methylation of arsenic
Albrecht, Michal ; Petry-Podgórska, Inga (advisor) ; Červený, Václav (referee)
The main aim of this thesis was the development of conjugation of existing methods for analysis of arsenic-glutathione complexes (As-GS complexes) together with simple arsenic species (iAs, MMAs, DMAs) during simple run. The basic technique for analysis of As-GS complexes was the HPLC-ICP-MS method with a reverse phase separation column (C18). The separation problem of simple species has been overcome by extending of system by postcolumn hydride generation with cryotrapping system (HG-CT). The resulting HPLC/HG-CT-ICP-MS system provides a complex analysis of all the above-mentioned analytes. According to the currently available resources, it is an innovative system, where for the first time all the simple arsenic species (iAs, MMAs, DMAs) and the As-GS complexes were separated. Under the given conditions, the detection limit for the As-GS complexes of 1.9 pg cm-3 in the RP-HPLC-ICP-MS system (a quantification limit of 6.5 pg cm-3 ) was achieved at a sensitivity of 468 CPS s pg-1 . The HG-CT-ICP-MS system provided a detection limit for iAs of 1.2 pg cm-3 at a sensitivity of 1121 CPS s pg-1 , for MMAs of 0.043 pg cm-3 at a sensitivity of 895 CPS s pg-1 and for DMAs of 0.076 pg.cm-3 at a sensitivity of 926 CPS s pg-1 . This method was applied to achieve another aim, studying the pathways of enzymatic...
Role of carbohydrate metabolism in defence against oxidative stress induced by arsenic
Kofroňová, Monika ; Lipavská, Helena (advisor) ; Száková, Jiřina (referee) ; Kovalíková, Zuzana (referee)
Heavy metal contamination significantly reduces crop yields, causing serious problems in agriculture and having a major impact on human health if these contaminants enter the food chain. Understanding the mechanisms of plant responses could help to increase their resistance to heavy metals as well as their potential use in phytoremediation. Carbohydrates play an important role in plant growth and development as well as in defense reactions. This work summarizes the results of four publications focused on the effects of arsenic and thorium on antioxidant mechanisms in tobacco plants and horseradish root crops. Attention is paid, among other things, to the dynamics of sugar contents, which are potentially important molecules involved in the fight against oxidative stress. The first publication summarizes arsenic effects on plant physiological parameters, focusing on arsenic tolerance-enhancing mechanisms as well as summarizing the ability of plants to cope with arsenic-induced oxidative and nitrosative stress. Emphasis was placed on, among other things, a topic that was unjustly neglected in previous publications - i.e. carbohydrate metabolism. Further work was already experimental and dealt with the study of arsenic as a trigger of oxidative stress in the root culture of horseradish and...
Speciation analysis of arsenic and mercury using postcolumn generation of their volatile compounds for needs of atomic spectroscopic methods
Linhart, Ondřej
The presented dissertation thesis deals with the use of UV-photochemical generation of volatile compounds (UV-PVG) as a derivatization technique for the combination of high-performance liquid chromatography (HPLC) and atomic absorption spectrometry (AAS) detection. Two model elements arsenic and mercury and their compounds were selected for the speciation analysis. The work was divided into several parts that follow. In the first part of the research, the apparatus for the UV-photochemical generation of the volatile mercury compounds and their detection with a new continuum source and high-resolution atomic absorption spectrometer (HR-CS AAS) with an externally heated detection tube was constructed. The analytical method was adapted for use with atomic fluorescence detection with the aim to improve sensitivity of the determination. Furthermore, apparatus for the electrochemical generation of cold mercury vapor with AAS detection was built. The construction of the apparatus was followed by optimization of the reaction conditions (concentration and flow of electrochemical reagents: sulfuric and hydrochloric acid, mobile phase, carrier medium, flow rate of the carrier gas and localization of its introduction), determination of the analytical figures of merit, and comparation of the methods. Both...
Speciation analysis of arsenic and mercury using postcolumn generation of their volatile compounds for needs of atomic spectroscopic methods
Linhart, Ondřej ; Červený, Václav (advisor) ; Spěváčková, Věra (referee) ; Šíma, Jan (referee)
The presented dissertation thesis deals with the use of UV-photochemical generation of volatile compounds (UV-PVG) as a derivatization technique for the combination of high-performance liquid chromatography (HPLC) and atomic absorption spectrometry (AAS) detection. Two model elements arsenic and mercury and their compounds were selected for the speciation analysis. The work was divided into several parts that follow. In the first part of the research, the apparatus for the UV-photochemical generation of the volatile mercury compounds and their detection with a new continuum source and high-resolution atomic absorption spectrometer (HR-CS AAS) with an externally heated detection tube was constructed. The analytical method was adapted for use with atomic fluorescence detection with the aim to improve sensitivity of the determination. Furthermore, apparatus for the electrochemical generation of cold mercury vapor with AAS detection was built. The construction of the apparatus was followed by optimization of the reaction conditions (concentration and flow of electrochemical reagents: sulfuric and hydrochloric acid, mobile phase, carrier medium, flow rate of the carrier gas and localization of its introduction), determination of the analytical figures of merit, and comparation of the methods. Both...
Speciation analysis of As and Hg in biological material
Petry-Podgórska, Inga ; Matoušek, Tomáš ; Migašová, M. ; Zemanová, Veronika ; Pavlík, Milan ; Pavlíková, D. ; Kratzer, Jan
This work was focused on an analysis of arsenic in selected plants and mercury in hair. A combination of HPLC and ICP-MS was used for analysis of biological tissues extracts. The\nspeciation analysis of low molecular arsenic and mercury species like inorganic iAs3+ and iAs5+, methylarsenic and dimethylarsenic forms was carried out with hydride generation (HG)\ntechnique, arsenic peptides and inorganic mercury (iHg2+) and its methylated form (MHg+) - with reverse phase (RP) chromatography and detected by ICP-MS.
Determination of arsenic species in seafood reference materials by ICP-MS with hydride generation and cryotrapping
Pokorná, Nikola ; Matoušek, Tomáš (advisor) ; Červený, Václav (referee)
The aim of this work was to determine chemical species of arsenic in sea originating certified reference materials. Measurements were done using method of hydride generation. Hydrides were preconcentrated in liquid nitrogen cooled tube and detected using inductively coupled plasma mass spectrometry. During the testing of the method, mutual conversion of arsenic species was observed for inorganic arsenic, monomethyl arsenic and dimethylarsenic. Further study revealed that with presence of matrix and hydrogen peroxide, demethylation occured only in hydride generation phase, not during extraction. Dissociation of hydrogen peroxide in extracts was verified using catalase. End of the demethylation process was proved using measurement with addition of arsenic species standards. The newly invented procedure was used to determine arsenic species in reference materials with sufficient accuracy. Final results are compatible with results from different method, and already published results as well. Key words: speciation analysis, arsenic, hydride generation, seafood, inductively coupled plasma mass spectrometry
Development of Instrumentation and Methodology for Elemental and Speciation Analysis of Arsenic Based on Hydride Generation and on Atomic Fluorescence Spectrometric Detection
Marschner, Karel ; Dědina, Jiří (advisor) ; Kanický, Viktor (referee) ; Spěváčková, Věra (referee)
(EN) The presented dissertation is devoted to hydride generation from arsenic species and its application for speciation analysis based on atomic fluorescence detection. Hydride generation from toxicologically relevant arsenic species was optimized in order to achieve a 100% efficiency. The resulted experimental setup was subsequently used for speciation analysis of arsenic in human urine by high performance liquid chromatography with detection by atomic fluorescence spectrometry. The accuracy of the developed method was verified by comparative analyses of human urine samples collected from five individuals with an independent reference method. The cleavage of As-C bond during the reaction of methylated arsenic species with tetrahydridoborate(1-) (THB) in acidic media was studied in detail. Pronounced demethylation of methylated arsenic species was found during the reaction of THB with HCl, H2SO4, and HClO4 while hydride generation from CH3COOH or TRIS buffer after prereduction with L- cysteine resulted in the exclusive formation of the corresponding hydrides. Firstly, this phenomenon can endanger the accuracy of arsenic speciation which is based on hydride generation of substituted arsanes. Secondly, the more complex arsenic species can be converted to the hydride. That was demonstrated on hydride...
Arsenic determination in beer samples and raw materials for its preparation
Švadlenová, Veronika ; Hraníček, Jakub (advisor) ; Jelínek, Ivan (referee)
This thesis describes the optimization of the method for determination of arsenic by the chemical hydride generation coupled with AAS detection in beer samples and raw materials for its preparation. The beer usually contain arsenic at ultratrace level, however, it is necessary to monitor the concentration of this element in the beer. The routinely used method for determination of arsenic is determination by electrothermal atomization. This approach is time consuming, expensive and less sensitive. It has been developer suitable determination of arsenic as a faster and less expensive method. For this method there was optimized the flow rate of argon to 75 ml·min-1, the optimum flow rate for the reagents was 4.0 ml·min-1 and for the sample 5.0 ml·min-1 . 3 % NaBH4 in 0.5 % NaOH was used as the reducing agent for the determination of arsenic, and HCl diluted 1:1 with distilled water was used to acidify the sample. With this parameter LOD was 0.32 μg·l-1 and LOQ 1.05 μg·l-1 . It has been tested the arsenic determination in samples of barley, malt and potable water as beer raw materials. It has been found that the beer matrix is unsuitable for the hydride generation technique due to a stormy reaction in the gas/liquid phase separator. The effect of pretreatment, which is likely to enhance the effect of...
Synthesis and separation of arsenic-glutathione complexes
Balcárová, Barbora ; Petry-Podgórska, Inga (advisor) ; Červený, Václav (referee)
The arsenic-glutathione complexes are very unstable in solution and tend to decompose during separation in liquid chromatography. The aim of this work was to develop a relatively fast method of the synthesis and storage conditions for the arsenic-glutathione complexes. The thesis is focused on synthesis, stability in-solution and separation of arsenicglutathione complexes. The synthesis was carried out in solution of 2 mM TCEP (tris(2carboxyethyl)phosphine) in water and with excess of the glutathione. Solutions of 20 ppb arsenic-complexes were consecutively measured after 1h, 2h, 3h, 4h and 24 hours of synthesis. The results confirmed stability of the arsenic-complexes in the reaction mixtures over 24 h. The arsenic-glutathione complexes were separated using a reversed phase high performance liquid chromatography (RP-HPLC) coupled with inductively coupled plasma - mass spectrometry (ICP-MS). The chromatographic method was developed using Aeris widepore 3.6u XB-C18 250x2.10mm column. Isocratic and gradient elutions were compared using several compositions of mobile phases and time of the separation. Methods were tested using samples of synthesized arsenic-glutathione complex (DMAs(GS)). An application of the isocratic elution enabled elimination of time needed for the separation and conditioning of...
Anthropogenic pollutioin of the Elbe River sediments
Haismanová, Pavla ; Chalupová, Dagmar (advisor) ; Bernsteinová, Jana (referee)
The thesis focuses on contamination of sediments in fluvial lakes of the Elbe river. The research was conducted in Kluk Lake near Poděbrady which has been artificially isolated from the river and its connection to the Elbe is now limited. The thesis concentrates on chemical composition of old sediments in vertical profile which documents an old anthropogenic pollution of Elbe's floodplain. The individual layers of sediment were analyzed separately. Besides grain size, the research also determined concentration of heavy metals and arsenic (Ag, Cd, Co, Cr, Cu, Hg, Mn, Ni, Pb and Zn). The sediment samples taken near the river contained higher content of elements compared to the more distant sampling site. This finding points out to the various distribution of elements and different settling velocity in the lake. Application of the geoaccumulation index showed that the sediments were very strongly polluted by silver and moderately to strongly polluted by arsenic, cadmium, mercury, lead and zinc. Last, the sediments were unpolluted to moderately polluted by cobalt, chromium, copper, manganese and nickel. According to the methodology of the International Commission for the Protection of the Elbe River (MKOL), the concentrations of silver, mercury, nickel and lead exceeded the upper limit value. Finally,...

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