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Comparison of APSI and ESI ionization for the development of UHPLC-MS/MS method for the determination of steroid compounds estrogens and progestins
Rabatinová, Martina ; Nováková, Lucie (advisor) ; Jáč, Pavel (referee)
In this study a new analytical method for determination of endocrine disruptors is pre- sented. The endocrine-disrupting phenomena is an area of growing concern. Potential ef- fects of endocrine-disrupting pollutants on wildlife and humans has been increased. Since 1980s deformities in fish are observed. Compounds associated to these effects include nat- ural compounds, such es estrogens, progestins and phytoestrogens, synthetic estrogens and a wide variety of organic pollutants, inluding pesticides, surfactants and plasticizers. Among them, estrogens are extraordinary due to their high estrogenic potency, with phys- iological active concentrations ranging from fg/ml to pg/ml. Endocrine disruptors might cause breast cancer in woman, abnormalities in the human reproductive system and differ- ent expressions of biological disorders in wildlife such as hermaphroditism, feminization, and decreased fertility. The presence of numerous endocrine-disrupting compounds in sur- face waters and sediment has been primarily atributed to their incomplete removal in the sewage-treatment process. Determination of these chemicals is required in order to assess their environmental impact. A new ultra high performance liquid chromatography/tandem mass spectrometry method (UHPLC-MS/MS) is presented in this study. The...
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The Development of SPE Extraction Procedure for Isolation of Pravastatin and its Metabolite from Biological Matrix
Rabatinová, Martina ; Nováková, Lucie (advisor) ; Nobilis, Milan (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Mgr. Martina Rabatinová Supervisor: Doc. PharmDr. Lucie Nováková, Ph.D. Title of Rigorous Thesis: The development of SPE extraction procedure for isolation of pravastatin and its metabolite from biological matrix Statins are a class of drugs used to lower cholesterol levels. Statins have an inhibitory activity against 3-hydroxy-3-methylglutaryl coenzyme A reductase. The main purpose of this work was to develop and validate a quantitative method for sensitive analysis of pravastatin and pravastatin lactone. The analytes were extracted from rat urine by a solid phase extraction method. In this method urine samples were prepared on C18 Discovery DSC-18. Washing and elution agents consisted of a mixture of acetonitrile and 0.01 M ammonium acetate buffer, pH 4.5. Number of extraction steps were optimized to eliminate most of matrix effects. The method involved use of ultra high performance liquid chromatography tandem mass spectrometry. Chromatography was carried out on a BEH C18 1.7 µm, 2.1×100 mm column. A mobile phase consisted of a mixture of acetonitrile and 0.5 mM ammonium acetate solution, pH 4.0. Linear gradient conditions were used. Total run time of this anal- ysis was 6 minutes...
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Comparison of APSI and ESI ionization for the development of UHPLC-MS/MS method for the determination of steroid compounds estrogens and progestins
Rabatinová, Martina ; Jáč, Pavel (referee) ; Nováková, Lucie (advisor)
In this study a new analytical method for determination of endocrine disruptors is pre- sented. The endocrine-disrupting phenomena is an area of growing concern. Potential ef- fects of endocrine-disrupting pollutants on wildlife and humans has been increased. Since 1980s deformities in fish are observed. Compounds associated to these effects include nat- ural compounds, such es estrogens, progestins and phytoestrogens, synthetic estrogens and a wide variety of organic pollutants, inluding pesticides, surfactants and plasticizers. Among them, estrogens are extraordinary due to their high estrogenic potency, with phys- iological active concentrations ranging from fg/ml to pg/ml. Endocrine disruptors might cause breast cancer in woman, abnormalities in the human reproductive system and differ- ent expressions of biological disorders in wildlife such as hermaphroditism, feminization, and decreased fertility. The presence of numerous endocrine-disrupting compounds in sur- face waters and sediment has been primarily atributed to their incomplete removal in the sewage-treatment process. Determination of these chemicals is required in order to assess their environmental impact. A new ultra high performance liquid chromatography/tandem mass spectrometry method (UHPLC-MS/MS) is presented in this study. The...
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