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The use of GC/MS for the analysis of drugs
Sýkora, Richard ; Opatřilová, Radka (referee) ; Vávrová, Milada (advisor)
This diploma thesis is based on the current issue of the presence of pharmaceuticals in various components of the environment. Concerning the contamination by residues of pharmaceuticals the most affected environment is the aquatic environment where these substances leaks especially from wastewater treatment plants, which eliminate them during the cleaning process only partially. This work is focused on the selected group of pharmaceuticals, non-steroidal anti-inflammatory drugs (salicylic acid, ibuprofen, caffeine, naproxen, ketoprofen, diclofenac) in waste water. For analysis purposes two types of sampling were used and compared: the conventional spot sampling of wastewater and the sampling using passive samplers POCIS. The sampling took place at the inflow and outflow of the wastewater treatment plant in Brno Modřice. The solid phase extraction (SPE) using Oasis HLB columns was used as the extraction method. Extracted sample was derivatized then. Derivatization agents were: MSTFA (N-methyl-N-(trimethylsilyl)trifluoroacetamid) and BSTFA (N, O-bis(trimethylsilyl) trifluoroacetamid). The final analysis was performed using gas chromatography with mass spectrometric detection Time-of-Flight (GC/TOF-MS).
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Experimental study and modelling of the transdermal penetration of active species from gels
Palanová, Veronika ; Opatřilová, Radka (referee) ; Sedláček, Petr (advisor)
This diploma thesis deals with design and experimental study of transdermal transport of pharmaceutically active agents from gel matrices, which contain humic substance in its structure. A model absorption membrane was represented by the skin of pig´s earlobes. The study of the release of active substances and Lignohumte was performed due to the vertical diffusion cells. The amount of released humic substance was characterized by UV-VIS method and the amount of released active agent from gel matrix was determined by HPLC-DAD. The most interesting finding of this diploma thesis was that Lignohumate enhances transdermal transport of active agents and supports their release from gel samples to the particular environment.
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Determination of drug residuals using separation methods
Vašíčková, Petra ; Opatřilová, Radka (referee) ; Vávrová, Milada (advisor)
Nonsteroidal anti-inflammatory substances became a very frequently used and constantly evolved group of the drugs, particularly in a human medicine. The risk of their penetration into the environment, especially to the water environment, is rising during the recent years. The diploma thesis is focused on a selection of appropriate separation method and optimization of analytical procedure for the identification and determination of the non-steroidal anti-inflammatory drugs in sewage and surface waters. Salicylic acid, ketoprofen, diclofenac and ibuprofen were chosen from the wide range of NSAIDs as the most widespread agents of this drugs group in the medical practice. The method was optimized and elaborated using the model water samples. This method was used for determination of the analytes contained in the real water samples. Waste water samples were taken from the large-scale wastewater treatment plant in Brno-Modřice and surface water samples were taken from the Highlands river Křetínka. Solid phase extraction (SPE) was used for the real samples treatment and preconcentration, the determination was performed using the high performance liquid chromatography with mass spectroscopy method (LC-MS).
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Determination of drugs by HPLC with different detectors
Benešová, Markéta ; Opatřilová, Radka (referee) ; Vávrová, Milada (advisor)
This diploma thesis deals with the determination of macrolide antibiotics in wastewater, especially with erythromycin, clarithromycin and roxithromycin. In this time are these pharmaceuticals prescribed quite frequently. Solid phase extraction (SPE) was used for the isolation and the purification of selected analytes from an aqueous matrix; as the suitable procedure was found the using Oasis HLB cartridges. High performance liquid chromatography with mass spectrometry detection (HPLC-MS) was optimized for its analysis of selected pharmaceuticals. The optimized method was used for the determination of pharmaceuticals in real water samples, which was taken at the inflow and the outflow of the urban wastewater treatment plant in Brno-Modřice.
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Application of separation methods for the determination of selected pharmaceuticals in waters
Burešová, Jitka ; Opatřilová, Radka (referee) ; Vávrová, Milada (advisor)
Antibiotics are widely used pharmaceuticals in human and veterinary medicine. These compounds are biologically active. They decrease efficiency of biological processes in wastewater treatment plants. Antibiotics are not eliminated from sewage water completely and they are discharged as contaminants into the receiving waters. Several methods exist for the determination of antibiotics in sewage water. In the first place liquid chromatography, gas chromatography and capillary electrophoresis are used. The aim of this thesis was to developed a suitable izolation technique and an optimal analytical method for identification and determination of penicillins in wastewater. For determination was selected amoxicillin, ampicillin and benzylpenicillin (penicillin G). These are very often used penicillins. An optimized method was used for determination of these penicilins in real samples from a wastewater treatment plant situated in Veterinary and pharmaceutical university in Brno and from the large-scale wastewater treatment plant in Brno-Modřice. Real samples were concentrated using SPE (solid phase extraction). For penicillins determination were used high performance liquid chromatography with diode array detection (HPLC/DAD).
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Use of Capillary Zone Electrophoresis for Determination of Selected Analgetics in Water
Čapka, Lukáš ; Opatřilová, Radka (referee) ; Márová, Ivana (referee) ; Vávrová, Milada (advisor)
From viewpoint of environmental analysis in the whole world became popular in the latest years the question of drugs’ breakthrough to the component of environment. These contami-nants belong to the biological active compounds, with different physical-chemical and biolog-ical properties and evince great tendency to bioaccumulation. They penetrate to the environ-ment because of their increasing of usage and wrong techniques of liquidation. The most often use drugs are preparations against pain – analgetics, and from this category there are non-steroidal anti-inflammatory drugs. The frequent usage of this compounds relate to their easy accessibility. From this large group of compounds was chosen for monitoring: diclofenac, ibuprofen, ketoprofen, salicylic acid, naproxen and acetaminophen; because they include in favorite preparations. The monitoring matrix was the wastewater from two waste water treat-ment plants (WWTP). The sampling was performed in inflow and outflow because the com-paring of concentration of selected contaminants and discovering of efficiency of removing the polutants reliance on treatment technology. For extraction of selected contaminants was used solid phase extraction (SPE) and for determination was used capillary zone electrophore-sis (CZE) with diode array detection (DAD). There was identified and quantified all of se-lected analgetics in inflow and so in outflow of WWTP. That means, this polutants infuse into surface water and then into other components of environment.
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Chiral analysis of drug residuals in waste waters
Svobodová, Dagmar ; Opatřilová, Radka (referee) ; Čáslavský, Josef (advisor)
The theoretical part shortly describes chirality with focus on chiral pharmaceuticals. The processes of their absorption, distribution, metabolism and elimination in human body are discussed. These points are very important to understand possible fate of chiral drugs in the environment as there is only little data concerning their environmental behaviour. The occurrence and enantioselective toxicity of chiral drugs is also discussed here. One of the chapters describes non-steroidal anti-inflammatory drugs, as they are analyzed in the wastewater in the experimental part, and their occurrence in the environment. The experimental part describes optimization of the enantioselective HPLC method using Chiralpak AD as column for ibuprofen and ketoprofen. Reproducible separation of enantiomers wasn’t achieved for naproxen. Optimized methods were then applied for analysis of samples from municipal wastewater treatment plant in Brno-Modřice.
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The Usage of Separation Methods for Research of Biologically Active Substances in Waters
Vydrová, Lucie ; Friedl, Zdeněk (referee) ; Opatřilová, Radka (referee) ; Chýlková,, Jaromíra (referee) ; Vávrová, Milada (advisor)
Pharmaceuticals are biological active compounds with different functional groups, physico-chemical and biological properties. These chemical compounds are called as “new contaminants” which cumulate in various environmental components. These contaminants input to environment from industrial processes, hospitals and health care institutions or household sources and these pollutants can to negatively interact with environmental components. Pharmaceuticals are separated according to structure and their effects to live organisms. On the basis of drug consumption in Czech Republic the non-steroidal anti-inflammatory drugs are the most using pharmaceuticals, because these drugs can be obtain without prescriptions. The choosing analgesics for study were monitored in waste water from waste waters treatment plant (WWTP Brno – Modřice) and in surface water from two sampling sites of river Kretinka. Pharmaceuticals were monitored in surface waters in Czech Republic, in Scotland (river Thurso) and in Taiwan (river Erren, Agongdian, Yanshuei and canal of Tainan) Solid phase extraction (SPE) is used for extraction of study pharmaceutical from water system. The high performance liquid chromatography (HPLC) with diode array detection or mass spectrometry was used for determination of drugs in surface waters from Czech Republic. The water samples from Scotland and Taiwan were analysed and the high performance liquid chromatography with mass spectrometry (HPLC/MS) was used for determination of pharmaceuticals. The method of HPLC/MS enables the determination of study compounds in the very low range of concentrations (ng ? l-1). All monitored pharmaceuticals were identified and quantified in water samples from river Kretinka in Czech Republic, river Thurso (Scotland) and rivers Erren, Agongdian, Yanshuei and canal of Tainan in Taiwan and the obtained data were compared.
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Removal of organic pollution using advanced oxidation processes
Přibilová, Petra ; Kučerík, Jiří (referee) ; Chýlková, Jaromíra (referee) ; Opatřilová, Radka (advisor)
The presented doctoral thesis deals with the use of advanced oxidation processes combining hydrodynamic cavitation (HC) to produce hydroxyl and sulfur-based radicals. The investigated micropollutants are selected natural estrogens estrone (E1), 17-estradiol (E2), estriol (E3) and synthetic 17-ethinylestradiol (EE2). The theoretical section includes information on the properties of estrogens, their occurrence and effects in the environment on non-target organisms across trophic levels; and list of options for their removal from wastewater. The advanced oxidation processes themselves are also discussed and current knowledge in this area is summarised. In the research section, used analytical methods (LC-MS/MS and spectrophotometry), designs of individual experiments and results of tested processes are described. In addition monitoring the efficiency of different combinations of hydrodynamic cavitation and other agent and the suitability of the materials used on the experimental unit were also investigated. The sorption/desorption onto the surface of selected plastic materials (SBR, EPDM, PTFE, Tygon S3TM, PVDF and PVC) was also evaluated. Based on the results, the material for the unit - on which the degradation experiments were carried out - was selected. The methods chosen for the removal of estrogens from water were HC/H2 O2 , HC/O3, HC/percarbonate, HC/persulfate, hydrodynamic cavitation alone, and H2O2 alone. The design of the experiments was created to minimize the time required to treat the water, ideally one cycle per unit (4 seconds), which corresponds to the flow-through arrangement of the system.
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Development of Electrophoretic Methods for the Analysis of Biologically Active Compounds using Complex Formation
Široká, Jitka ; Polášek, Miroslav (advisor) ; Štěrbová, Petra (referee) ; Opatřilová, Radka (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate Mgr. Jitka Široká Supervisor Doc. RNDr. Miroslav Polášek, CSc. Title of Doctoral Thesis Development of electrophoretic methods for the analysis of biologically active compounds using complex formation The disertation is dealing with the development of capillary electrophoretic methods with spectrophotometric detection for the determination of biologically active substances in forensic, clinical and pharmaceutical fields. Theoretical background to the individual experimental parts is presented in the Introduction. Basic principles of capillary electrophoresis are explained, problems of separation selectivity and sensitivity are discussed and the analytes under study are characterised. The first experimental part is devoted to electrophoretic determination of chlorophenylpiperazine isomers (ortho, meta, para) in confiscated pills using cyclodextrins as selectors in acidic phosphate buffer. The second experimental part is devoted to the determination of urinary 8-hydroxy-2'-deoxyguanosine (an oxidation stress biomarker) using complex formation with borate including sample pretreatment prior analysis and on-line preconcentration by sample stacking in a detection cell with long optical path....
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