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Stanovení residuí fluorochinolonů v půdách metodou LC-FD
Aufartová, Jana ; Solich, Petr (advisor) ; Nováková, Lucie (referee)
7. Abstract Several pharmaceutics used in human and veterinary medicine could be detected in environment. To these compounds belongs Fluoroqinolones. Our work observed 4 fluoroqinolons (ofloxacin, norfloxacin, ciprofloxacin, enrofloxacin) in soils sample. Fluoroquinolones were determinate by LC-FD. For extraction was used mixture of organic compounds (methanol: acetone; 1:1) and 1.0g of EDTA. Sample was 15 minutes shacked, 15 minutes in ultrasonic bath and 15 minutes of centrifugation. After that organic solution was evaporated by gentle stream of nitrogen in water bath. Rest from evaporation was dissolved in mQ-H2O and clean-up was done. After evaporation after clean-up the rest was dissolved in mobil phase. Mobil phase was H3PO4: MeOH: ACN (920: 70: 10) and flow was 1.4mL/min. Limit of quantification (LOQ) is For OFLO 5mg/L, for NOR is 0.083mg/L, for CIP is 0.116mg/L and for ENRO is 0.125mg/L. Mean recoveries ranged between 75% to 121%, for OFLO, NOR, CIPRO and ENRO. At the beginning we tried also acidic type of extraction. Extraction was made with HCL, H2SO4, H3PO4 and HNO3. In all cases we add EDTA because of interferences with other substances in samples. We find out, that no complex is build between flouroquinolones and EDTA. For clean- up from soil samples is better OASIS column HLB 6cc/200mg....
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Stress testing of estradiol and ethynylestradiol
Mašková, Kateřina ; Chocholoušová Havlíková, Lucie (advisor) ; Aufartová, Jana (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Kateřina Mašková Supervisor: PharmDr. Lucie Havlíková, Ph.D. Title of Diploma Thesis: Stress testing of estradiol and ethynylestradiol This diploma thesis is focused on the implementation of stress testing of two estrogenic hormones estradiol and ethynylestradiol. Both substances have been exposed to oxidation and acid and alkaline pH at increased temperature of 70řC for a predefined time period. The results of these tests should have shown a decrease or an increase of the peak area of estradiol and 17α- ethynylestradiol and a potential formation of degradation products. Peak areas and retention times of degradation products were observed by HPLC. The aim of this thesis was to determine the properties of these hormones under various stress conditions like extreme conditions of production, storage, transport and/or under various external influences. Characterization of degradation products and verification of the suitability of methods used for the analysis of degradation products were also aims of this paper. The method was partially validated. In the experimental part there has been found out that estradiol and ethynylestradiol were stable in water as well as in acetonitrile solution...
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Development of New Methods for Monitoring of Occurence of Pharmaceuticals in the Environment
Aufartová, Jana ; Solich, Petr (advisor) ; Fiala, Zdeněk (referee) ; Garcia-Campaña, Ana M. (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate Mgr. Jana Aufartová Supervisor Prof. RNDr. Petr Solich, CSc. Title of Doctoral Thesis DEVELOPMENT OF NEW METHODS FOR DETERMINATION OF SELECTED PHARMACEUTICALS IN ENVIRONMENTAL SAMPLES During last decade, the consumption of pharmaceuticals is increasing substantially. At the same time their occurrence in environment is increasing as well. Pharmaceuticals are released into environment by excretion, as conjugated or unchanged active compounds, as unused pharmaceuticals, which are not disposed according to the recommendations (e.g. thrown away into the rubbish or flushed down the toilet). Other possible sources of pharmaceuticals are in the agriculture, livestock and aquaculture. The current water treatment technologies do not remove all traces of pharmaceuticals in wastewaters. Therefore the monitoring of their occurrence in surface and wastewaters become more important. Antibiotics and steroid hormones are a group of drugs used in human and veterinary medicine. The main problem with these groups of substances is the emergence of bacterial resistance, in the case of antibiotics, and the effect on the endocrine system, including the reproductive cycle, in the case of steroid hormones. The...
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Stress testing of estradiol and ethynylestradiol
Mašková, Kateřina ; Chocholoušová Havlíková, Lucie (advisor) ; Aufartová, Jana (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Kateřina Mašková Supervisor: PharmDr. Lucie Havlíková, Ph.D. Title of Diploma Thesis: Stress testing of estradiol and ethynylestradiol This diploma thesis is focused on the implementation of stress testing of two estrogenic hormones estradiol and ethynylestradiol. Both substances have been exposed to oxidation and acid and alkaline pH at increased temperature of 70řC for a predefined time period. The results of these tests should have shown a decrease or an increase of the peak area of estradiol and 17α- ethynylestradiol and a potential formation of degradation products. Peak areas and retention times of degradation products were observed by HPLC. The aim of this thesis was to determine the properties of these hormones under various stress conditions like extreme conditions of production, storage, transport and/or under various external influences. Characterization of degradation products and verification of the suitability of methods used for the analysis of degradation products were also aims of this paper. The method was partially validated. In the experimental part there has been found out that estradiol and ethynylestradiol were stable in water as well as in acetonitrile solution...
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Development of HPLC method for the determination of amygdalin and serotonin in dietary supplement
Parmová, Martina ; Chocholoušová Havlíková, Lucie (advisor) ; Aufartová, Jana (referee)
The analytical method for the determination of amygdalin and serotonin supplement B17 APRICARC using high-performance liquid chromatography was developed and validated. The 96 % ethanol was used for the extraction to obtain analytes. As a suitable chromatographic column was chosen the column Ascentis Express® OH5 (3 x 100 mm, 2,7 µm). The composition of the mobile phase for the analysis was 10 mM acetate buffer pH 3.8 : acetonitrile 10:90 (v:v). The flow rate was set on 0.8 mL / min, for the detection of amygdalin was used an UV detector (wavelength 215 nm) and for the detection of serotonin was used the fluorescence detector (Ex 280 nm , Em 340 nm ). A suitability test of chromatographic system was performed and these parameters were pursued: column efficiency, resolution peak symmetry factor and repeatability of analysis. Within the actual validation these parameters were pursued: accuracy, linearity, precision, and limit of detection and quantification.
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Development of New Methods for Monitoring of Occurence of Pharmaceuticals in the Environment
Aufartová, Jana ; Solich, Petr (advisor) ; Fiala, Zdeněk (referee) ; Garcia-Campaña, Ana M. (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate Mgr. Jana Aufartová Supervisor Prof. RNDr. Petr Solich, CSc. Title of Doctoral Thesis DEVELOPMENT OF NEW METHODS FOR DETERMINATION OF SELECTED PHARMACEUTICALS IN ENVIRONMENTAL SAMPLES During last decade, the consumption of pharmaceuticals is increasing substantially. At the same time their occurrence in environment is increasing as well. Pharmaceuticals are released into environment by excretion, as conjugated or unchanged active compounds, as unused pharmaceuticals, which are not disposed according to the recommendations (e.g. thrown away into the rubbish or flushed down the toilet). Other possible sources of pharmaceuticals are in the agriculture, livestock and aquaculture. The current water treatment technologies do not remove all traces of pharmaceuticals in wastewaters. Therefore the monitoring of their occurrence in surface and wastewaters become more important. Antibiotics and steroid hormones are a group of drugs used in human and veterinary medicine. The main problem with these groups of substances is the emergence of bacterial resistance, in the case of antibiotics, and the effect on the endocrine system, including the reproductive cycle, in the case of steroid hormones. The...
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Stanovení residuí fluorochinolonů v půdách metodou LC-FD
Aufartová, Jana ; Solich, Petr (advisor) ; Nováková, Lucie (referee)
7. Abstract Several pharmaceutics used in human and veterinary medicine could be detected in environment. To these compounds belongs Fluoroqinolones. Our work observed 4 fluoroqinolons (ofloxacin, norfloxacin, ciprofloxacin, enrofloxacin) in soils sample. Fluoroquinolones were determinate by LC-FD. For extraction was used mixture of organic compounds (methanol: acetone; 1:1) and 1.0g of EDTA. Sample was 15 minutes shacked, 15 minutes in ultrasonic bath and 15 minutes of centrifugation. After that organic solution was evaporated by gentle stream of nitrogen in water bath. Rest from evaporation was dissolved in mQ-H2O and clean-up was done. After evaporation after clean-up the rest was dissolved in mobil phase. Mobil phase was H3PO4: MeOH: ACN (920: 70: 10) and flow was 1.4mL/min. Limit of quantification (LOQ) is For OFLO 5mg/L, for NOR is 0.083mg/L, for CIP is 0.116mg/L and for ENRO is 0.125mg/L. Mean recoveries ranged between 75% to 121%, for OFLO, NOR, CIPRO and ENRO. At the beginning we tried also acidic type of extraction. Extraction was made with HCL, H2SO4, H3PO4 and HNO3. In all cases we add EDTA because of interferences with other substances in samples. We find out, that no complex is build between flouroquinolones and EDTA. For clean- up from soil samples is better OASIS column HLB 6cc/200mg....
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