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Utilization of mass spectrometry for analysis of biologically active compounds
Kaliba, David
This PhD thesis provides a commented set of four publications. These publications are focused on capillary electrophoresis, liquid chromatography, and UV/Vis spectrometry used to study complexes of rhenium with aromatic ligands. The methods of mass spectrometry with soft ionization techniques, 1 H and 13 C nuclear magnetic resonance, and infrared spectrometry were used for structural characterization of the individual complexes. The complexes were synthetized in reactions of the rhenium precursor tetrabutylammonium tetrachlorooxorhenate with the corresponding ligand under both aerobic and anaerobic conditions. In the course of the research, it was revealed that the prepared complexes (with Re in the oxidation number +V and +VI) are unstable and their oxidation numbers change to another more stable form (Re+VII ). Sub-projects which were successfully implemented during the research were as follows: Design and successful realization of the process of synthesis of selected rhenium complexes with aromatic ligands 1,2-dihydroxybenzene, 1,2,3-trihydroxybenzene, and 2,3-dihydroxynaphthalene in reactions with and without air access, and their structural characterization by ESI-MS, APPI- MS, LDI-MS, ESI-MS/MS, NMR, and IR. ESI-MS SRM and UV/Vis time studies of the behaviour of primary rhenium complexes...
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Utilization of mass spectrometry for analysis of biologically active compounds
Kaliba, David
This PhD thesis provides a commented set of four publications. These publications are focused on capillary electrophoresis, liquid chromatography, and UV/Vis spectrometry used to study complexes of rhenium with aromatic ligands. The methods of mass spectrometry with soft ionization techniques, 1 H and 13 C nuclear magnetic resonance, and infrared spectrometry were used for structural characterization of the individual complexes. The complexes were synthetized in reactions of the rhenium precursor tetrabutylammonium tetrachlorooxorhenate with the corresponding ligand under both aerobic and anaerobic conditions. In the course of the research, it was revealed that the prepared complexes (with Re in the oxidation number +V and +VI) are unstable and their oxidation numbers change to another more stable form (Re+VII ). Sub-projects which were successfully implemented during the research were as follows: Design and successful realization of the process of synthesis of selected rhenium complexes with aromatic ligands 1,2-dihydroxybenzene, 1,2,3-trihydroxybenzene, and 2,3-dihydroxynaphthalene in reactions with and without air access, and their structural characterization by ESI-MS, APPI- MS, LDI-MS, ESI-MS/MS, NMR, and IR. ESI-MS SRM and UV/Vis time studies of the behaviour of primary rhenium complexes...
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Utilization of mass spectrometry for analysis of biologically active compounds
Kaliba, David ; Jelínek, Ivan (advisor) ; Pacáková, Věra (referee) ; Smrček, Stanislav (referee)
This PhD thesis provides a commented set of four publications. These publications are focused on capillary electrophoresis, liquid chromatography, and UV/Vis spectrometry used to study complexes of rhenium with aromatic ligands. The methods of mass spectrometry with soft ionization techniques, 1 H and 13 C nuclear magnetic resonance, and infrared spectrometry were used for structural characterization of the individual complexes. The complexes were synthetized in reactions of the rhenium precursor tetrabutylammonium tetrachlorooxorhenate with the corresponding ligand under both aerobic and anaerobic conditions. In the course of the research, it was revealed that the prepared complexes (with Re in the oxidation number +V and +VI) are unstable and their oxidation numbers change to another more stable form (Re+VII ). Sub-projects which were successfully implemented during the research were as follows: Design and successful realization of the process of synthesis of selected rhenium complexes with aromatic ligands 1,2-dihydroxybenzene, 1,2,3-trihydroxybenzene, and 2,3-dihydroxynaphthalene in reactions with and without air access, and their structural characterization by ESI-MS, APPI- MS, LDI-MS, ESI-MS/MS, NMR, and IR. ESI-MS SRM and UV/Vis time studies of the behaviour of primary rhenium complexes...
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Electrophoresis in short capillary with dual detection.
Kaliba, David ; Opekar, František (advisor) ; Jelínek, Ivan (referee)
Capillary zone electrophoresis is an analytical method frequently used in many laboratories for solving various analytical problems. This diploma thesis describes one of many applications of capillary zone electrophoresis using a unique laboratory apparatus composed of a short capillary and dual conductivity/UV detector placed in one detection point of the separation capillary. In the first part of this thesis, the laboratory apparatus was tested by the separation of small inorganic and organic ions. Sodium, potassium, tyramine and histidine ions were used to test the two parts of the dual detector. Experimentally obtained mobilities of these ions were compared with those calculated from the tabulated values. In the second part, the apparatus was used for determination of analytes in samples with more complex matrixces, pharmaceuticals Acylcoffin and B-komplex produced by Zentiva, a.s. One analyte was chosen from each pharmaceutical preparation for determination of its concentration in the preparation, caffeine from Acylcoffine and thiamine from B-komplex. The concentrations were calulated using three different calibration methods and the experimentally obtained values were compared with those specified by the pharmaceuticals producer. Key words: capillary electrophoresis; short capillary;...
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