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Application of modern analytical methods for the study of selected boron coordination compounds
Hrušková, Helena ; Jelínek, Ivan (advisor) ; Dian, Juraj (referee)
This thesis is focused on the study of boron coordination compounds, specifically boron pyrogallol and 2,3-dihydroxynaphthalene ligand complexes. In the introductory part of the work are discussed the properties of boron compounds, their preparation, the possibility of separation by capillary electrophoresis and methods of structural characterization. In the first part of the thesis, the methods of preparation of complexes are discussed and for each complex the optimal yield response is chosen. The resulting products were studied by low resolution mass spectrometry. In the second part of the thesis, structures of complexes, including their modeling in the Gaussian program, were described more precisely. Furthermore, the complexes were characterized by high resolution mass spectrometry. The complexes were also studied by 11 B, 1 H and 1 H COSY NMR and IR spectroscopy. The third part was devoted to the separation of these substances from the mixture after the reaction. CE-UV and CE-MS techniques were used for this purpose. To convert the results, the separation method was developed in ammonium formate buffers that are compatible with both instruments. The equilibration between complexes and ligands was also monitored by CE-UV. A special chapter is the study of pyrogallol autooxidation by UV-VIS and...
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Development of capillary electrophoretic method for determination of phosphorylated components of bacterial cell membranes
Červinková, Jana ; Čabala, Radomír (advisor) ; Coufal, Pavel (referee)
Title: Development of capillary electrophoretic method for determination of phosphorylated components of bacterial cell membranes Author: Jana Červinková Department: Department of analytical chemistry Supervisor: RNDr. Radomír Čabala, Dr. Abstract: The bachelor work reviews the present state of knowledge of the analyses and determination of phosphorylated compounds present in the bacterial cell membranes. This group of compounds is represented mainly by phosphatidylglycerol, cardiolipine, and phosphatidylethanolamine and minority phosphatidylserine, phosphatidic acid and lysylphospatidylglycerol. Together with fatty acids these substances are the main components of cell membranes and they could be, to a certain degree, applied to either identification of bacteria or the study of bacterial behaviour at different conditions. Partially or fully non-aqueous capillary electrophoresis analytical method with spectrophotometric detection would be developed for their determination. Optimum experimental conditions for the separation of standards of selected compounds should be found within the framework of the bachelor thesis. Keywords: phosphorylated compounds, bacterial cytoplasmic membrane, capillary electrophoresis, thin layer chromatography, Bacillus subtilis.
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Determination of Lithium in Mineral Waters Using Electrophoresis in Short Capillary.
Makrlíková, Anna ; Opekar, František (advisor) ; Tůma, Petr (referee)
The aim of this study was determination of lithium ion concentration in mineral waters "Vincentka" and "Bílinská kyselka" using capillary electrophoresis with contactless conductivity detection. A specialized laboratory-made apparatus designed for separations in short capillaries was first tested for separation of model solution of common inorganic cations and then for analysis of mineral water samples. Lithium ion concentration was determined using method of standard addition. The results obtained were compared with those obtained from atomic absorption and emission spectroscopy; standard addition method as well as the method of calibration graph were used in spectroscopic methods. A good agreement was obtained between experimentally determined concentrations of lithium and those declared in the labels on the mineral water bottles. Keywords Capillary electrophoresis, contactless conductivity detection, mineral waters, lithium, atomic absorption spectroscopy, atomic emission spectroscopy
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The application of high-efficiency separation methods for chiral and achiral separations
Šubová, Martina ; Bosáková, Zuzana (advisor) ; Jelínek, Ivan (referee) ; Fischer, Jan (referee)
In the first part of the doctoral thesis, the capillary electrophoresis was used to test the potential chiral separation properties of monosubstituted cyclodextrin derivatives, namely PEMEDA- and PEMPDA-β-cyclodextrins for the group of selected analytes. Both selectors exhibited excellent enantioseparation properties for N-boc-D,L-tryptophan, where the enantiomers were completely separated even at 0.5 mmol·l-1 concentration of the cyclodextrin derivative in the background electrolyte. However, the differences between the enantiodiscrimination properties of individual derivatives were minimal. The second test group consisted of two cyclodextrin derivatives, namely 2-O- and 3-O- cinnamyl-α-cyclodextrins. These derivatives are able to form supramolecular polymers in aqueous solutions that disintegrate at elevated temperature. The formation of these polymers was tested by NMR and DLS experiments. None of the tested cyclodextrin derivatives showed enantiodiscrimination properties towards a group of selected analytes. In the frame of antipredatory study, HPLC-MS/MS method working in HILIC mode was used for separation of ten pterin derivatives and riboflavin, which can be present as pigments in insects, reptiles or amphibians as a part of their warning coloration. The developed methodology was applied for...
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Influence of the interacting constituent of the background electrolyte on electrophoretic separation
Müllerová, Ludmila ; Dubský, Pavel (advisor) ; Kašička, Václav (referee) ; Petr, Jan (referee)
Capillary electrophoresis is a widely used separation method of analytical chemistry. Addition of a selector into the background electrolyte extends its applicability to separation of enantiomers or of compounds of similar physicochemical properties. In analytical practice, mixtures of selectors are also commonly used - either prepared intentionally to achieve better separation or because commercially available selectors may be mixtures of compounds differing in the degree of substitution and substituent positions. Mathematical description of these systems, which are highly relevant in analytical practice, can simplify search for optimal separation conditions. Also, it provides a useful insight into the separation mechanism. In this work, a model of electromigration of an analyte interacting with a mixture of two selectors is proposed and experimentally verified. This model results from a more general description of systems with an arbitrary number of selectors. The model shows that a selector mixture can be treated as a single selector if the ratio of the respective selector concentrations is kept constant. When the mixture is prepared intentionally, this description predicts, how separation potential of the mixture changes with its composition. Thus it allows the optimal composition and total...
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Chiral separation of diquats and determination of stability constants of their complexes with cyclodextrins by capillary electrophoresis
Bílek, Jan ; Kašička, Václav (advisor) ; Jelínek, Ivan (referee)
Capillary zone electrophoresis was used for chiral separation of eleven diquat derivatives. These N-heteroaromatic dications containing structural motif of 2,2'-bipyridine have recently been studied for their interesting electrochemical properties as well as for the axial chirality of their molecules. The combination of these properties could potencially lead to interesting applications in the future. For enantioseparation of diquats (DQ) commercially available randomly sulfated α-, β-, and γ-cyclodextrins with high degree of substitution were used. A succesfull chiral separation was achieved using all of the three sulfated cyclodextrins as chiral selectors (CS). Baseline enantioseparation was achieved for 82 %, 91 % respectively 100 % of the analyzed DQ in the presence of HS-α-CD, HS-β-CD, HS-γ-CD respectively. The highest separation efficiency and resolution were obtained in the backround electrolyte containing 22 mmol/L NaOH, 35 mmol/L H3PO4 (pH2,5) and 6 mmol/L HS-β-CD. Using three available nonracemic DQ an identification of the particular M- and P-enantiomers was done for the three corresponding DQ structures. Apparent stabillity constants of complexes of the DQ derivatives with above mentioned cyclodextrins as CS were determined by means of capillary affinity electrophoresis. The stability...
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Modification of capillary wall by graphene for separation applications
Ptáčková, Aneta ; Lochman, Lukáš (advisor) ; Kučera, Radim (referee)
CHARLES UNIVERSITY FACULTY OF PHARMACY IN HRADEC KRÁLOVÉ Department of Pharmaceutical Chemistry and Pharmaceutical Analysis Candidate: Aneta Ptáčková Supervisor: PharmDr. Lukáš Lochman, Ph.D. Title of thesis: Modification of capillary wall by graphene for separation applications Capillary electrophoresis (CE) is a highly efficient separation method. Substances are separated due to their different mobility in an electric field. The CE modes of operation can be modified in different ways, e.g. capillary electrochromatography or micellar electrokinetic capillary chromatography. Modification of the inner wall of the capillary is believed to help improve separation efficiency and selectivity. Graphene is carbon with a hexagonal structure in form of two-dimensional sp2 single-atom-thick sheets. Graphene seems to be a suitable material for separation application due to its excellent properties such as large surface area and affinity to aromatic ring through π-π interactions. Our work is focused on the modification of the capillary wall by graphene. One of the methods of capillary wall modification is the Layer-by-Layer method via layering of differently charged substances bounded by electrostatic forces. Another method is chemical coating employing covalent interactions. Different combinations of polymers...
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Analysis of potasium tetrachloroaurate by capillary electrophoresis
Lebertová, Lucie ; Sobotníková, Jana (advisor) ; Křížek, Tomáš (referee)
This bachelor thesis describes the optimalization of condition for the analysis of potassium tetrachloroaurate by capillary zone electrophoresis with spectrophotometric detection. The theoretical part at first introduces the principle of capillary electrophoresis. The following are basic information about gold and its tetrachloroaurate compound. The experimental part at first describes the procedure of optimization the composition of the basic electrolyte and problems with the instability of the base line. As the most suitable conditions for the analysis of tetrachloroaurate, have been chosen the subsequent experimental conditions: fused silica capillary with a total length of 80 cm, effective length 71.6 cm and inner diameter 50 µm; applied separation voltage -20 kV; applied pressure during analysis 20 mbar; injection with 20 mbar for 20 s; background electrolyte containing 0.01 mol dm-3 HCl and 0.04 mol dm-3 NaCl; detection vawelength at 230 nm. Subsequently, the repeatability of the measurement, and the stability of the tetrachloroaurate stock solution were evaluated. Also the calibration dependence were measured and the limit of detection and the limit of quantification were determined for the optimized experimental conditions. The value of LOD was 7.49 ∙ 10-6 mol dm-3 and the value of LOQ was...
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Optimization of a method for the determination of inorganic ions using capillary electrophoresis
Špačková, Simona ; Bezděková, Jaroslava (referee) ; Vaculovičová, Markéta (advisor)
Inorganic ions are one of the most important group chemicals. Their importance is crucial for all living organisms on the planet and monitoring of their content is essential for this purpose in clinical or environmental analysis but also in the food industry, agriculture or many other industries. Many analytical methods for ion detection have been designed and used, depending on the area of their use. Recently, numerous methods have been adapted to areas where not primarily intended. One such methods may be, for example, laser ablation with inductively coupled plasma mass spectrometry, which has recently begun to affect the analysis of biological samples. As a complementary method, able to detect also non-metallic ions is capillary electrophoresis. In this master thesis, the possibility of applying capillary electrophoresis with indirect photometric detection for the separation of inorganic ions in cell lysates of HeLa cells by capillary electrophoresis was verified. Main attention was paid to chloride ions. The ability to separate inorganic compounds in cellular material using salicylic acid as an absorbing anion in the base electrolyte was tested.
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Use of capillary electrophoresis to determine a selected group of flavonoids
Tran Xuan, Tiep ; Mravcová, Ludmila (referee) ; Řezáčová, Veronika (advisor)
In recent years, the use of natural medicinal properties of plants has again come to the forefront of interest of the public. Because of their therapeutic properties, these plants are commonly used in alternative treatments for minor ailments. This thesis deals with the determination of polyphenolic acids in extracts from aronia, echinacea, tetradenia and centella. One of the aims of the thesis was to compare the amount of polyphenolic acids in individual plants with their antioxidant properties. The theoretical part includes a general introduction to flavonoids, introduction to polyphenolic acids, introduction to the principles of capillary zone electrophoresis and a summary of selected foreign studies for the determination of flavonoids. An important chapter of the theoretical part is a description of individual plants with an explanation of their possible therapeutic use. The experimental part is devoted to the process of optimization of electrophoretic determination of selected polyphenolic acids and evaluation of their content. It was found that in the extracts six representatives of polyphenolic acids occur in minimal amounts, often below the limit of quantification or detection of the method.
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