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Non-target screening of organic pollutants in waters and sediments
Hamalčíková, Veronika ; Vávrová, Milada (referee) ; Čáslavský, Josef (advisor)
This master thesis deals with the potential influence of the waste dump Hrádek u Pacova and the wastewater treatment plant Brno – Modřice on surroundings using the optimized non-target screening method of organic pollutants in water and sediments. The experimental part is focused on the identification of organic compounds in samples of ground water from monitoring wells, the surface water from stream and pond and in sediment samples collected from streams in the vicinity of municipal waste dump. Organic compounds were also identified in water and sediment samples from the river Svratka near the municipal waste water treatment plant Modřice. The sequential liquid – liquid extraction was used for the isolation of organic compounds in water samples. Organic compounds in sediment samples were isolated by pressurized solvent extraction (PSE) with subsequent fractionation of the extract using column chromatography. Final analysis determination was performed using comprehensive orthogonal two-dimensional gas chromatography with mass spectrometric detection (GCxGC-TOF MS).
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Analysis of volatile organic compounds produced by monocytes during sepsis
Bártová, Adéla ; Řezáčová, Veronika (referee) ; Mravcová, Ludmila (advisor)
This thesis is focused on the possibility of analysis of volatile organic compounds produced by monocytes during sepsis. Method of comprehensive two-dimensional gas chromatography with mass spectrometric detection was chosen for this purpose. Content of the first part was the optimization of the method of two-dimensional gas chromatography for the determination of volatile organic compounds. In this part were gradually adjusted parameters of the gas chromatography method to achieve the maximum efficiency. Further were adjusted conditions of samples preparation. Content of the second part was the usage of already optimized method for the analysis of the samples set of monocytes. Samples were subjected to the action of different inhibitors of the immune system and stimulators simulating bacterial or yeast infection. Based on this analysis were identified some compounds, which are produced by monocytes under condition simulating the infection.
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Application of Gas Chromatography with Mass Spectrometric Detection for the Assessment of Drug-residue Contamination of Wastewaters and Surface Waters
Lacina, Petr ; Čáslavský, Josef (referee) ; Hajšlová, Jana (referee) ; Sokol,, Jozef (referee) ; Vávrová, Milada (advisor)
This work is based on the current issue of increasing concentrations of pharmaceutical residues in various components of the environment. These new environmental contaminants continuously enter the environment. The most affected environmental component is the aquatic environment. This study is focused on the development and optimization of reliable analytical method, which can determine selected drugs in the aquatic environment (waste waters and surface waters) qualitatively and quantitatively. The target compounds were selected mainly from the group of non-steroidal anti-inflammatory drugs (NSAID): salicylic acid, acetylsalicylic acid, clofibric acid, ibuprofen, acetaminophen, caffeine, naproxen, mefenamic acid, ketoprofen and diclofenac. NSAIDs are one of the most used drugs in Czech Republic. For the final analysis of this study was used the comprehensive two-dimensional gas chromatography with mass spectrometric detection Time-of-Flight (GCxGC-TOF MS). It is a very sensitive and reliable analytical method for trace and ultra-trace analysis. Simultaneously, solid phase extraction (SPE) and derivatization are optimized in this work. Optimized analytical method including SPE, derivatization with MSTFA (N-methyl-N-(trimethylsilyl) trifluoroacetamide) and final analysis by GCxGC-TOF MS were applied successfully for the analysis of real samples. Samples of waste water were collected from the waste water treatment plant in Brno – Modřice and samples of surface water were collected from two river streams Svratka and Svitava in Moravian region. The range of concentrations of selected drug residues varied from one to tens of g/L in wastewater and from tens to hundreds of ng/L in surface waters. The degree of wastewater and surface waters contamination by drug residues is assessed in conclusions of the work. Simultaneously, spontaneous degradation of selected drugs in water and removal efficiency of the wastewater treatment plant is assessed in conclusions of the work. The developed method is usable for monitoring and environmental analysis of water ecosystems. It is usable not only for selected drugs, but even for other organic compounds with similar properties.
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Quantitative composition changes of sex pheromone in Anastrepha fraterculus depending on age
Zyková, Kamila ; Kalinová, Blanka (advisor) ; Rezek, Jan (referee)
Males of South American fruit fly Anastrepha fraterculus form leks and release sex pheromone to attract females during the reproductive behavior. The aim of my diploma thesis was to collect samples of volatiles released by variously old males, subsequently to analyze and to determine the changes in the quantitative composition of the sex pheromone depending on age. The volatiles were trapped on adsorbent, eluted with hexane containing internal standard and analyzed by gas chromatography with mass detection. Males release twenty volatiles, including fourteen terpenes: α-pinene, camphene, -pinene, myrcene, Δ3-carene, limonene, (Z)--ocimene, (E)--ocimene, aromadendrene, trans-α-bergamotene, (Z)-β-farnesene, (Z,E)-α-farnesene, germacrene D, (E,E)-α-farnesene; one aldehyde: nonanal; two alcohols: (3Z)-non-3-en-1-ol, (3Z,6Z)-nona-3,6-dien-1-ol and three lactones: suspensolide, anastrephin a epianastrephin. From the list of named compounds there were proved antenal activity of six compounds in previous work, namely trans-α-bergamotene, (Z,E)-α-farnesene, (E,E)-α-farnesene, (3Z)-non-3-en-1-ol, (3Z,6Z)-nona-3,6-dien-1-ol and epianastrephin.
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Analysis of flower scents Clusia blattophila
Mitrovský, Ondřej ; Kalinová, Blanka (advisor) ; Vaníčková, Lucie (referee)
South American plant Clusia blattophila, growing on Nouraghes of French Guiana, produces relatively large amounts of volatile substances in the fragrance of its flowers. C. blattophila is dioecious plant with different flowering time of monosex flowers Male flowers bloom for one night, while female flowers bloom two nights. The volatiles were adsorbed to the adsorbent and washed out with hexane with internal standard. Analysis was performed by two-dimensional gas chromatography with mass spectrometric detection. The aim of my thesis was to determine the qualitative and quantitative characteristics of flower scents of both sexes. I also studied, whether there are differences in production of the major fragrance component, acetoin, during the first night of blooming. The flower fragrance is complex blend of volatiles. In total, 43 different chemicals were identified. Among them were monoterpenes (α-pinene, camphene, β-pinene, myrcene, limonene, (E)-β-ocimene, camphor) sesquiterpenes (α-copaene, β-caryophyllene, cis-α-bergamotene, trans-α-bergamotene, aromadendrene, (E,E)-α-farnesene, δ-cadinene), aldehydes (1-pentanal, 1-hexanal, 1-octanal, n-decanal), also four ketones (acetoin and its dimer, 2,5-hexanedione, 6-methylhept-5-en-2-one), alcohol butane-2,3-diol, carboxylic acid 2-methylpropanoic,...
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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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The application of high-efficiency separation methods for chiral and achiral separations
Šubová, Martina
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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The application of high-efficiency separation methods for chiral and achiral separations
Šubová, Martina
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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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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Analysis of volatile organic compounds produced by monocytes during sepsis
Bártová, Adéla ; Řezáčová, Veronika (referee) ; Mravcová, Ludmila (advisor)
This thesis is focused on the possibility of analysis of volatile organic compounds produced by monocytes during sepsis. Method of comprehensive two-dimensional gas chromatography with mass spectrometric detection was chosen for this purpose. Content of the first part was the optimization of the method of two-dimensional gas chromatography for the determination of volatile organic compounds. In this part were gradually adjusted parameters of the gas chromatography method to achieve the maximum efficiency. Further were adjusted conditions of samples preparation. Content of the second part was the usage of already optimized method for the analysis of the samples set of monocytes. Samples were subjected to the action of different inhibitors of the immune system and stimulators simulating bacterial or yeast infection. Based on this analysis were identified some compounds, which are produced by monocytes under condition simulating the infection.
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