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The Use of Liquid Chromatography for Determination of Drug Residues
Dvořáková, Petra ; Hajšlová, Jana (referee) ; Chýlková, Jaromíra (referee) ; Sokol, Jozef (referee) ; Vávrová, Milada (advisor)
This work is based on the occurrence of drug residues in the environment. This study is focused on the development and optimization methods for determination of selected drugs in the surface water, aquatic sediment and sewage sludge from waste water treatment plant. From the group of drugs were chosen antibiotics. Antibiotics presented in the environment can cause adverse effects including toxic effects, immunity disorders and indirect bioalteration effects. Sulfonamide antibiotics, which are used in the treatment of urinary and respiratory tract infections as well as in the treatment of other infectious diseases, were chosen as a target compounds. Three optimized analytical methods for determination of sulfonamide antibiotics were developed. For the optimization of extraction were tested: solid phase extraction, pressurized solvent extraction, microwave extraction and ultrasonic extraction. For the final analysis was used liquid chromatography with two detectors - diode array detector and mass spectrometer. These optimized methods were applied for the analysis of real samples. The surface water and sediment samples were collected from two Moravian rivers (the Svratka river and the Svitava river). Samples of sewage sludge were collected from waste water treatment plant Brno-Modřice. Fish samples from the Svratka river were also collected. It was observed that all the selected sulfonamide antibiotics are present in real sediment samples (ug.kg-1). Simultaneously presence of some target analytes in real surface water (ug.l-1) and in sewage sludge (ug.kg-1) samples has been confirmed. In samples of surface water from the Svitava river and in fish samples sulfonamide antibiotics were not detected or their concentrations were below the limit of detection.
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Study of Exposure PBDE and Perfluorinated Compounds into Aquatic Ecosystem
Vondráčková, Ilona ; Chýlková, Jaromíra (referee) ; Hroch, Martin (referee) ; Kráčmar, Stanislav (referee) ; Vávrová, Milada (advisor)
In the presented PhD. thesis, problems covering occurrence of polybrominated diphenyl ethers (PBDE) and perfluorinated compounds in the environment were solved. The study was focused on identification and further verification of optimal methods in order to determine PBDEs and perfluorinated compounds sampled from the aquatic ecosystem. Polybrominated diphenyl ethers belong to persistent compounds classified as main pollutants; within the environmental constituents, they have been observed particularly in the last decade. For these studies, there were selected surface water matrices and sediments taken in various localities within the river Svratka basin. The analyses were to demonstrate whether they accumulate and remain in these specific matrices for longer time. There we assessed the congeners of polybrominated diphenyl ethers as follows: BDE-28, 47, 66, 85, 99, 100, 153, 154 and 183. In order to isolate them from matrices, various extraction techniques were used, i.e., ultrasonic extraction, microwave extraction, and pressure solvent extraction. Gas chromatography method with electron capture detection (GC/ECD) was selected for determination. The accomplished studies also assessed basic chemical, physical and environmental characteristics of diphenyl ethers in the environmental constituents. The attention was also paid to perfluorooctanoic compounds (PFOA), (PFOS) and (FOSA); physico-chemical properties of these organic pollutants were characterised and their toxicological and environmental aspects were evaluated. Usability of extraction techniques (ultrasonic extraction, pressure solvent extraction, solid phase extraction) applied to PFCs isolation from sediments samples was assessed. Identification and quantification of these analytes were performed using a high performance liquid chromatography/mass spectrometry method (HPLC/MS). After that, the optimized methods applied to real samples. Surface water and sediments were sampled within the river Svratka basin, in particular, from 19 sampling localities. PBDE occurrence was confirmed in sediments samples from the Svratka river (g.kg-1), PBDE were not detected in the surface water samples, their concentrations were below the detection limit, resp.; perfluorinated compounds were not detected in sediments and water samples at all.
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Developement and optimalization of methods for extraction of selected compounds from Hypericum perforatum
Chytil, Dalibor ; Štursa, Václav (referee) ; Pořízka, Jaromír (advisor)
Bachelor's thesis deals with the optimization of processes for extraction of phenolic compounds from St. John´s Wort (Hypericum perforatum). The theoretical part of the work focuses on characterization of this herb, its botanical classification, traditional use, chemical composition and curative effects. Increased attention is further devoted to a theory of preparation of samples for extraction of phenolic compounds and suitable techniques for extraction and characterization of phenolic compounds from extracts of St. John´s Wort. The experimental part of the thesis deals with application of theoretical knowledge. When optimizing the emphasis was on influence of solvent (water acified to pH 4, pH 5, pH 6), influence of extraction technique (ultrasound extraction, subcritical water extraction, maceration) and influence of extraction period (10, 20, 30 min). Extracts were subjected to determination of selected parameters (total phenolic content, total flavonoid content, antioxidant activity) in leaves of St John´s Wort harvested in June 2016 using UV-VIS spectroscopy. The used extraction techniques are significantly different from each other.
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Developement and optimalization of methods for extraction of selected compounds from Hypericum perforatum
Chytil, Dalibor ; Štursa, Václav (referee) ; Pořízka, Jaromír (advisor)
Bachelor's thesis deals with the optimization of processes for extraction of phenolic compounds from St. John´s Wort (Hypericum perforatum). The theoretical part of the work focuses on characterization of this herb, its botanical classification, traditional use, chemical composition and curative effects. Increased attention is further devoted to a theory of preparation of samples for extraction of phenolic compounds and suitable techniques for extraction and characterization of phenolic compounds from extracts of St. John´s Wort. The experimental part of the thesis deals with application of theoretical knowledge. When optimizing the emphasis was on influence of solvent (water acified to pH 4, pH 5, pH 6), influence of extraction technique (ultrasound extraction, subcritical water extraction, maceration) and influence of extraction period (10, 20, 30 min). Extracts were subjected to determination of selected parameters (total phenolic content, total flavonoid content, antioxidant activity) in leaves of St John´s Wort harvested in June 2016 using UV-VIS spectroscopy. The used extraction techniques are significantly different from each other.
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Study of Exposure PBDE and Perfluorinated Compounds into Aquatic Ecosystem
Vondráčková, Ilona ; Chýlková, Jaromíra (referee) ; Hroch, Martin (referee) ; Kráčmar, Stanislav (referee) ; Vávrová, Milada (advisor)
In the presented PhD. thesis, problems covering occurrence of polybrominated diphenyl ethers (PBDE) and perfluorinated compounds in the environment were solved. The study was focused on identification and further verification of optimal methods in order to determine PBDEs and perfluorinated compounds sampled from the aquatic ecosystem. Polybrominated diphenyl ethers belong to persistent compounds classified as main pollutants; within the environmental constituents, they have been observed particularly in the last decade. For these studies, there were selected surface water matrices and sediments taken in various localities within the river Svratka basin. The analyses were to demonstrate whether they accumulate and remain in these specific matrices for longer time. There we assessed the congeners of polybrominated diphenyl ethers as follows: BDE-28, 47, 66, 85, 99, 100, 153, 154 and 183. In order to isolate them from matrices, various extraction techniques were used, i.e., ultrasonic extraction, microwave extraction, and pressure solvent extraction. Gas chromatography method with electron capture detection (GC/ECD) was selected for determination. The accomplished studies also assessed basic chemical, physical and environmental characteristics of diphenyl ethers in the environmental constituents. The attention was also paid to perfluorooctanoic compounds (PFOA), (PFOS) and (FOSA); physico-chemical properties of these organic pollutants were characterised and their toxicological and environmental aspects were evaluated. Usability of extraction techniques (ultrasonic extraction, pressure solvent extraction, solid phase extraction) applied to PFCs isolation from sediments samples was assessed. Identification and quantification of these analytes were performed using a high performance liquid chromatography/mass spectrometry method (HPLC/MS). After that, the optimized methods applied to real samples. Surface water and sediments were sampled within the river Svratka basin, in particular, from 19 sampling localities. PBDE occurrence was confirmed in sediments samples from the Svratka river (g.kg-1), PBDE were not detected in the surface water samples, their concentrations were below the detection limit, resp.; perfluorinated compounds were not detected in sediments and water samples at all.
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The Use of Liquid Chromatography for Determination of Drug Residues
Dvořáková, Petra ; Hajšlová, Jana (referee) ; Chýlková, Jaromíra (referee) ; Sokol, Jozef (referee) ; Vávrová, Milada (advisor)
This work is based on the occurrence of drug residues in the environment. This study is focused on the development and optimization methods for determination of selected drugs in the surface water, aquatic sediment and sewage sludge from waste water treatment plant. From the group of drugs were chosen antibiotics. Antibiotics presented in the environment can cause adverse effects including toxic effects, immunity disorders and indirect bioalteration effects. Sulfonamide antibiotics, which are used in the treatment of urinary and respiratory tract infections as well as in the treatment of other infectious diseases, were chosen as a target compounds. Three optimized analytical methods for determination of sulfonamide antibiotics were developed. For the optimization of extraction were tested: solid phase extraction, pressurized solvent extraction, microwave extraction and ultrasonic extraction. For the final analysis was used liquid chromatography with two detectors - diode array detector and mass spectrometer. These optimized methods were applied for the analysis of real samples. The surface water and sediment samples were collected from two Moravian rivers (the Svratka river and the Svitava river). Samples of sewage sludge were collected from waste water treatment plant Brno-Modřice. Fish samples from the Svratka river were also collected. It was observed that all the selected sulfonamide antibiotics are present in real sediment samples (ug.kg-1). Simultaneously presence of some target analytes in real surface water (ug.l-1) and in sewage sludge (ug.kg-1) samples has been confirmed. In samples of surface water from the Svitava river and in fish samples sulfonamide antibiotics were not detected or their concentrations were below the limit of detection.
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