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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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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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Aplication of gas chromatography for determination of drug residuals in waters
Lacina, Petr ; Stoupalová, Michaela (referee) ; Vávrová, Milada (advisor)
Diploma thesis is focused on the choose of methods and optimalisation analysis procedure of selected pharmaceuticals (salicylic acid, ibuprofene, naproxene, ketoprofene and diclofenac) in surface and waste water by using gas chromatography with mass spectrometer (GC-MS). Solid-phase extraction (SPE) with Oasis HLB cartridges was used as an extraction method in this analysis. Extraction is followed by derivatization and their optimalization of selected pharmaceuticals. Derivatization and its optimalization were performed by two silylation reagens N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) and N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA). Different volumes of derivatization reagents, different temperatures and different times were used during the procedure. The best combination is then used for analysis of real samples. Real samples of waste water were collected in sewage treatment plants in Brno – Modřice and real samples of surface water were collected from several rivers and one pond in region Moravia. This thesis also presents and tests SPE methods for extraction and concentration selected sulfonamide residues (sulfamethazine, sulfamethoxazole, sulfapyridine and sulfathiazole) from the aquatic environment.
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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).
|
|
|
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).
|
|
|
Aplication of gas chromatography for determination of drug residuals in waters
Lacina, Petr ; Stoupalová, Michaela (referee) ; Vávrová, Milada (advisor)
Diploma thesis is focused on the choose of methods and optimalisation analysis procedure of selected pharmaceuticals (salicylic acid, ibuprofene, naproxene, ketoprofene and diclofenac) in surface and waste water by using gas chromatography with mass spectrometer (GC-MS). Solid-phase extraction (SPE) with Oasis HLB cartridges was used as an extraction method in this analysis. Extraction is followed by derivatization and their optimalization of selected pharmaceuticals. Derivatization and its optimalization were performed by two silylation reagens N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) and N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA). Different volumes of derivatization reagents, different temperatures and different times were used during the procedure. The best combination is then used for analysis of real samples. Real samples of waste water were collected in sewage treatment plants in Brno – Modřice and real samples of surface water were collected from several rivers and one pond in region Moravia. This thesis also presents and tests SPE methods for extraction and concentration selected sulfonamide residues (sulfamethazine, sulfamethoxazole, sulfapyridine and sulfathiazole) from the aquatic environment.
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