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A development of UHPLC-MS/MS method for the determination of pravastatin, rosuvastatin and their metabolites
Mikšová, Alena ; Nováková, Lucie (advisor) ; Vlčková, Hana (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Alena Mikšová Supervisor: Doc. PharmDr. Lucie Nováková, PhD. Title of Graduation Thesis: A development of UHPLC-MS/MS method for the determination of pravastatin, rosuvastatin and their metabolites This graduation thesis is dealing with the development of UHPLC/MS-MS method for the determination of pravastatin, rosuvastatin and their metabolites. The basic parameters were optimized for MS detection - desolvation temperature, ion optics (RF lens and extractor), nitrogen flow at the sample cone, capillary voltage, nitrogen flow and cone voltage, which is specific for each substance. Separation of analytes was performed on BEH C18 analytical column (2.1 x 100 mm, 1.7µm). Triple quadrupole was used for detection. Electrospray ionization was performed in both negative and positive mode. Quantification of analytes was performed using the SRM (selected reaction monitoring). Ion [M+H]+ was chosen for all statins determined in positive ion mode. This ion was the most intense in full scan spectrum. In positive ion mode pravastatin lactone offered also ammonium adduct [M+NH4]+ . All statins determined in negative mode provided a precursor ion [M-H]- . Pravastatin lactone and rosuvastatin lactone...
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A development of UHPLC-MS/MS method for the determination of pravastatin, rosuvastatin and their metabolites
Mikšová, Alena ; Nováková, Lucie (advisor) ; Vlčková, Hana (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Alena Mikšová Supervisor: Doc. PharmDr. Lucie Nováková, PhD. Title of Graduation Thesis: A development of UHPLC-MS/MS method for the determination of pravastatin, rosuvastatin and their metabolites This graduation thesis is dealing with the development of UHPLC/MS-MS method for the determination of pravastatin, rosuvastatin and their metabolites. The basic parameters were optimized for MS detection - desolvation temperature, ion optics (RF lens and extractor), nitrogen flow at the sample cone, capillary voltage, nitrogen flow and cone voltage, which is specific for each substance. Separation of analytes was performed on BEH C18 analytical column (2.1 x 100 mm, 1.7µm). Triple quadrupole was used for detection. Electrospray ionization was performed in both negative and positive mode. Quantification of analytes was performed using the SRM (selected reaction monitoring). Ion [M+H]+ was chosen for all statins determined in positive ion mode. This ion was the most intense in full scan spectrum. In positive ion mode pravastatin lactone offered also ammonium adduct [M+NH4]+ . All statins determined in negative mode provided a precursor ion [M-H]- . Pravastatin lactone and rosuvastatin lactone...
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