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On-line coupling of MEPS with HPLC for determination of pharmaceuticals in urine
Sobek, Vojtěch ; Šatínský, Dalibor (advisor) ; Sklenářová, Hana (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Vojtěch Sobek Supervisor: Doc. RNDr. Dalibor Šatínský, Ph.D. Title of Diploma Thesis: On-line coupling of MEPS with HPLC for determination of pharmaceuticals in urine A new method for on-line coupling of MEPS with HPLC was developed and validated for analysis of metoprolol, propranolol and labetalol in the urine. The column Triart YMC 50 mm x 4.6 mm - 5 µm particle size was used for separation of three β - blockers - metoprolol, labetalol and propranolol. Detection was carried out using a fluorescence detector at excitation wavelength 220 nm and emission wavelength 315 nm and the column temperature was set on 30 řC. Gradient elution with a mobile phase of 0,5% aqueous solution of triethylamine adjusted to pH 4.5 with glacial acetic acid with acetonitrile in ratio 80/20 at a flow rate of 1.0 ml/min was used for separation. Before the analysis, the β - blockers were extracted and preconcentrated from urine matrix with using microextraction to on MEPS column C - 18 SGE Analytical Science using 7% acetonitrile as a washing solution and the washing flow rate of 0.5 ml/min. Original method allows the determination of the three selected β - blockers in the urine matrix without previous sample...
On-line coupling of MEPS with HPLC for determination of pharmaceuticals in urine
Sobek, Vojtěch ; Šatínský, Dalibor (advisor) ; Sklenářová, Hana (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Vojtěch Sobek Supervisor: Doc. RNDr. Dalibor Šatínský, Ph.D. Title of Diploma Thesis: On-line coupling of MEPS with HPLC for determination of pharmaceuticals in urine A new method for on-line coupling of MEPS with HPLC was developed and validated for analysis of metoprolol, propranolol and labetalol in the urine. The column Triart YMC 50 mm x 4.6 mm - 5 µm particle size was used for separation of three β - blockers - metoprolol, labetalol and propranolol. Detection was carried out using a fluorescence detector at excitation wavelength 220 nm and emission wavelength 315 nm and the column temperature was set on 30 řC. Gradient elution with a mobile phase of 0,5% aqueous solution of triethylamine adjusted to pH 4.5 with glacial acetic acid with acetonitrile in ratio 80/20 at a flow rate of 1.0 ml/min was used for separation. Before the analysis, the β - blockers were extracted and preconcentrated from urine matrix with using microextraction to on MEPS column C - 18 SGE Analytical Science using 7% acetonitrile as a washing solution and the washing flow rate of 0.5 ml/min. Original method allows the determination of the three selected β - blockers in the urine matrix without previous sample...

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