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Analysis of amino acids and polyamines by HPLC and CZE
Kubíčková, Anna ; Coufal, Pavel (advisor) ; Pacáková, Věra (referee) ; Flieger, Miroslav (referee)
(EN) This work is focused on two specific classes of amines. First group comprises of cyclic polyaminocarboxylates from the DOTA (1,4,7,10-tetraazacyclododecane- 1,4,7,10-tetraacetic acid) family, which are important reaction intermediates in magnetic resonance imaging (MRI) contrast agent synthesis. In the development of new contrast agents, carboxyl groups are very often protected with tert-butyl ester groups. Among these derivatives, tBu3DO3A is of the highest importance. Therefore, reverse-phase high performance liquid chromatographic (RP-HPLC) and non- aqueous capillary zone electrophoretic (CZE) methods were evaluated for qualitative and quantitative analysis of tBu3DO3A (1,4,7,10-tetraazacyclododecan-1,4,7- tris(tert-butylacetate) and two typical reaction by-products, i.e. tBu4DOTA (1,4,7,10- tetraazacyclododecan-1,4,7,10-tetrakis(tert-butylacetate) and tBu2DO2A (1,4,7,10- tetraazacyclododecan-1,4-bis(tert-butylacetate). These optimized methods were successfully applied to monitoring of real reaction mixtures during synthesis of a new MRI contrast agent. No further sample pretreatment was necessary. In the second part of the thesis, proteinogenic amino acids and polyamines were used as model analytes for development of a new post-column solid-phase reactor suitable for on-line derivatization...
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Analysis of amino acids and polyamines by HPLC and CZE
Kubíčková, Anna
(EN) This work is focused on two specific classes of amines. First group comprises of cyclic polyaminocarboxylates from the DOTA (1,4,7,10-tetraazacyclododecane- 1,4,7,10-tetraacetic acid) family, which are important reaction intermediates in magnetic resonance imaging (MRI) contrast agent synthesis. In the development of new contrast agents, carboxyl groups are very often protected with tert-butyl ester groups. Among these derivatives, tBu3DO3A is of the highest importance. Therefore, reverse-phase high performance liquid chromatographic (RP-HPLC) and non- aqueous capillary zone electrophoretic (CZE) methods were evaluated for qualitative and quantitative analysis of tBu3DO3A (1,4,7,10-tetraazacyclododecan-1,4,7- tris(tert-butylacetate) and two typical reaction by-products, i.e. tBu4DOTA (1,4,7,10- tetraazacyclododecan-1,4,7,10-tetrakis(tert-butylacetate) and tBu2DO2A (1,4,7,10- tetraazacyclododecan-1,4-bis(tert-butylacetate). These optimized methods were successfully applied to monitoring of real reaction mixtures during synthesis of a new MRI contrast agent. No further sample pretreatment was necessary. In the second part of the thesis, proteinogenic amino acids and polyamines were used as model analytes for development of a new post-column solid-phase reactor suitable for on-line derivatization...
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Characterization of low-molecular-mass synthetic markers of isoelectric points by capillary zone electrophoresis and capillary isoelectric focusing
Brandejsová, Martina ; Kašička, Václav (advisor) ; Kubíčková, Anna (referee)
High-performance electromigration separation methods, capillary zone electrophoresis (CZE) and capillary isoelectric focusing (CIEF), have been applied to physico-chemical characterization of new synthetic low-molecular mass markers of isoelectric points. Amphoteric compounds on the basis of aminomethylnitrophenols, their derivatives and other structurally related substances were analyzed by CZE in a series of background electrolytes in a wide pH range, 1.86 - 11.18. From the measured pH dependencies of effective electrophoretic mobilities of analytes (beforehand corrected to reference temperature of 25 řC), their isoelectric points (pI) were determined. In addition, using the non-linear regression analysis of the above dependencies, acid-base dissociation constants (pKa) of ionogenic groups of selected analytes were calculated. Subsequently, the analytes with sharply defined isoelectric points were analyzed by CIEF. CIEF confirmed applicability of these compounds as markers of isoelectric points for calibration of pH gradient in CIEF in the determination of pI of amphoteric compounds, especially peptides and proteins. The determined pKa values of ionogenic groups in particular compounds will be utilized in the development of new pI markers with desired pI values.
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The issue of child soldiers in international law with regard to the African regional regulation
Kubíčková, Anna ; Honusková, Věra (advisor) ; Bayerová, Monika (referee)
The main purpose of this thesis was to give a general overview of the problem of child soldiers and their protection among international law conventions and among regional law agreements with the focus on the African continent. The use of child soldiers in armed conflict is qualified as one of the worst forms of child labour.The majority of child soldiers are active in Africa and, to a lesser extent, in the Middle East and Asia. Besides introduction and conclusion, the study consists of five chapters. The first chapter describes the protection of child soldiers on the international level. Therefore it is focused on individual conventions, especially on Geneva Conventions, Additional Protocols to the Geneva Conventions, the Convention on the Rights of the Child, the Optional Protocol to the Convention on the Rights of the Child on the involvement of children in armed conflict, the Optional Protocol to the Convention on the Rights of the Child on a Communications Procedure, but as well on the International Labour Convention No. 182 or the Rome Statute. The soft law represents Paris principles. Discussed is particularly the question of the age limit for child participation in armed conflict. The second chapter is concerned with the international control mechanisms, resulting from the above-mentioned...
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Automatic Analysis of Heart Rate Variability Signals
Kubičková, Alena ; Halámek, Josef (referee) ; Lhotská, Lenka (referee) ; Kozumplík, Jiří (advisor)
This dissertation thesis is dedicated to the heart rate variability and methods of its evaluation. It mainly focuses on nonlinear methods and especially on the Poincaré plot. First it deals with the principle and nature of the heart rate variability, then the ways of its representation, linear and also nonlinear methods of its analysis and physiological and pathophysiological influence on heart rate variability changes. In particular, there is emphasis on the metabolic syndrome. In the next section of the thesis there are compared and evaluated different ways of representation of the heart rate variability and further are tested selected methods of heart rate variability analysis on unique data from patients with the metabolic syndrome and healthy subjects provided by the Institute of Scientific Instruments, Academy of Sciences of Czech Republic. In particular, they are used the Poincaré plot and its parameters SD1 and SD2, commonly used time domain and frequency domain parameters, parameters evaluating signal entropy and the Lyapunov exponent. SD1 and SD2 combining the advantages of time and frequency domain methods of heart rate variability analysis distinguish successfully between patients with the metabolic syndrome and healthy subjects.
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Mobilization of neutral compounds by inorganic and small organic ions in capillary electrophoresis
Křížek, T. ; Martínková, E. ; Kubíčková, A. ; Hladílková, Jana ; Coufal, P. ; Heyda, J. ; Jungwirth, Pavel
The present study shows that neutral low-molecular-mass compounds that are presumed to possess zero electrophoretic mobility and are thus used as markers of electroosmotic flow in capillary electrophoresis can acquire electrophoretic mobility due to ion-specific interactions with constituents of background electrolyte. Therefore, these neutral markers, such as thiourea or dimethyl sulfoxide, can be separated in electric field and their migration order can vary depending on background electrolyte composition. This observation has some important implications for analytical and physico-chemical measurements using capillary electrophoresis because the choice of the marker-background electrolyte combination can influence the results of the measurement.
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Preprocessing of R-R interval tachogram
Had, Filip ; Kozumplík, Jiří (referee) ; Kubičková, Alena (advisor)
Heart rate variability (HRV) is a parameter, which monitors variability of the time intervals between consecutive heart beats. Signal HRV contains artefacts and trends, which is necessary to remove before further processing. This work contains a brief information about the HRV and ECG signal processing. Further on the most frequently methods of heart rate variability preprocessing are described. The work includes a brief assessment of each method. Further on, several of the mentioned preprocessing algorithms are realized and described in this work. The last part is testing an evaluating of programmed algorithms on generated data and then demonstration on real data.
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Noise map
Lokaj, Jiří ; Kubičková, Alena (referee) ; Rozman, Jiří (advisor)
The aim of this paper is to introduce the measurement of noise and create a noise map in a geographic information system. The first part is focused on describing the physical properties of sound in space, atmospheric and physiological acoustics. It also deals with the physiological effects of noise on the human body and technology needed for measure and process noise. Other part describes the structure of a geographic information system and noise map. The last part is about the practical creation of noise maps, includes a description of the real measurement results and evaluation
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