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Optimization of separation and quantification of prospective products of big bang
Smitka, Jaroslav ; Tesařová, Eva (advisor) ; Kalíková, Květa (referee)
The thesis is a contribution to research aimed at modeling the conditions of the Big Bang and monitoring possible reaction products. As the starting compounds were selected 2- amino-1-butanol, 3-methoxy-1-propanol, 2-methyl-1-butanol, formamide, some of which were subsequently bombarded by PALS at J. Heyrovsky Institute of Physics, Academy of Sciences. Gas chromatography hyphenated with mass spectrometry and liquid chromatography with UV detection were used for analysis. In GC-MS, calibration of 3- methoxy-1-propanol and 2-methyl-1-butanol was carried out and LOD and LOQ were calculated. Comparison of 3-methoxy-1-propanol and bombarded 3-methoxy-1-propanol did not show the emergence of new products since 3-methoxy-1-propanol was in excess. The found compounds can be more likely identified as impurities present in a solvent or in the individual standards. The optimized HPLC system has managed to separate the three standards. Formamide, which is unsuitable for analysis by gas chromatography, due to its high polarity, however, eluted in all tested systems with system peak (the dead time marker). Nevertheless, the bombarded sample was analyzed for comparison with the original standard. Comparison, however, showed no reaction products in the bombarded sample. Key words: big bang laser sparks formamide...
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Study of inclusion complexes of pesticides with cucurbiturils
Smitka, Jaroslav ; Tesařová, Eva (advisor) ; Šteflová, Jana (referee)
In this work we report the formation of inclusion complexes of the pesticides 1-naphthylacetic acid, 1-naphthylacetamide, napropamide and carbaryl with cucurbit[n]uril (n=7 and 8) and -cyclodextrin hosts. We also report results of the photochemistry of these compounds when free in aqueous solution and included within these nano-containers. The formation of inclusion complexes was studied by electrospray ionization mass spectrometry (ESI-MS) which gave us information about stoichiometry of the complexes and about their reactivity in the gas phase. The photodecomposition and formation of products was followed by high performance liquid chromatography coupled to both mass spectrometry (HPLC-MS) and UV/VIS detector, and spectrophotometry. The studied CBs and their host-guest complexes were readily detected in the gas phase by ESI-MS, mainly as single and double charged ions containing either H+ , Na+ or K+ . The assignments were made based on the m/z values of the observed signals and further confirmed by fragmentation (tandem mass spectrometry - MSn ). All pesticides formed 1:1 (host:guest) complexes. Carbaryl, napropamide and 1-naphthylacetamide also formed 1:2 (host:guest) complexes. Under some solution chemistry conditions, namely for concentrations of cucurbiturils above 50 µM and at low acid and...
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Optimization of separation and quantification of prospective products of big bang
Smitka, Jaroslav ; Tesařová, Eva (advisor) ; Kalíková, Květa (referee)
The thesis is a contribution to research aimed at modeling the conditions of the Big Bang and monitoring possible reaction products. As the starting compounds were selected 2- amino-1-butanol, 3-methoxy-1-propanol, 2-methyl-1-butanol, formamide, some of which were subsequently bombarded by PALS at J. Heyrovsky Institute of Physics, Academy of Sciences. Gas chromatography hyphenated with mass spectrometry and liquid chromatography with UV detection were used for analysis. In GC-MS, calibration of 3- methoxy-1-propanol and 2-methyl-1-butanol was carried out and LOD and LOQ were calculated. Comparison of 3-methoxy-1-propanol and bombarded 3-methoxy-1-propanol did not show the emergence of new products since 3-methoxy-1-propanol was in excess. The found compounds can be more likely identified as impurities present in a solvent or in the individual standards. The optimized HPLC system has managed to separate the three standards. Formamide, which is unsuitable for analysis by gas chromatography, due to its high polarity, however, eluted in all tested systems with system peak (the dead time marker). Nevertheless, the bombarded sample was analyzed for comparison with the original standard. Comparison, however, showed no reaction products in the bombarded sample. Key words: big bang laser sparks formamide...
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