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EI spectra interpretation
Polášek, Miroslav
Introduction to the interpretation of mass spectra. Basic mechanisms of fragmentation reactions in electron ionization. An intensive exercise on selected examples of mass spectra of electron ionization of different classes of organic compounds, which will be carried out in the spirit of the elementary didactic principle of progression from simple to complex with maximum emphasis on the independent work of the participants.\n\n
Determination of rocuronium, vecuronium and pancuronium muscle relaxants by capillary electrophoresis with contactless conductivity detection
Böhmová, Lenka ; Polášek, Miroslav (advisor) ; Pospíšilová, Marie (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Student: Lenka Böhmová Supervisor: Doc. RNDr. Miroslav Polášek, CSc. Title of Diploma Thesis: Determination of rocuronium, vecuronium and pancuronium muscle relaxants by capillary electrophoresis with contactless conductivity detection A new method of capillary zone electrophoresis with contactless conductivity detection for the determination of pancuronium bromide, vecuronium bromide and rocuronium bromide was developed. The separation was carried out in fused-silica capillary with internal diameter 50 µm, total length 75 cm and effective length 45 cm. Optimal background electrolyte was 30mM acetate buffer of pH 5,75 containing 20 mg/ml of hydroxypropyl-γ-cyclodextrin. Phenyltrimethylammonium iodide was used as internal standard. The separation was performed at 25řC, the applied voltage was 20 kV. The samples were injected hydrodynamically at 50 mbar for 6 s. Under such optimal conditions the separation took less than 4 min. Calibration curves were linear for all analytes in the range 50 - 250 µg/ml, the coefficients of correlation were in the range 0,9954 - 0,9983. The limits of detection were 13,2 µg/ml, 11,1 µg/ml and 11,3 µg/ml for pancuronium bromide, vecuronium bromide and rocuronium...
SEQUENTIAL INJECTION ANALYSIS CAPABILITY IN AUTOMATION OF ANALYTICAL PROCESSES
Novosvětská, Lucie ; Sklenářová, Hana (advisor) ; Polášek, Miroslav (referee) ; Hraníček, Jakub (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate (married name/maiden name): Mgr. Lucie Novosvětská / Mgr. Lucie Zelená Supervisor: assoc. prof. PharmDr. Hana Sklenářová, Ph.D. Consultant: PharmDr. Petr Chocholouš, Ph.D. Title of dissertation thesis: Sequential injection analysis capability in automation of analytical processes This dissertation, composed as a commented collection of four scientific articles and one undergoing project, introduces four novel applications in the field of automated flow methods and one application in the field of chromatographic methods used in analytical part of a complex pharmacological study. It the field of pharmaceutical analysis, three works were successfully optimized, validated, and published in scientific journals. Those works include: a) Automation of permeation studies within a sequential injection analysis system connected to a liberation unit and carrying out experiments with living cells. b) Pharmacological study of an antiretroviral drug efavirenz including its determination by fast chromatographic method in three types of sample matrices - in a medium from permeation studies with cellular models, in a Krebs solution from rat placenta perfusions, and in placenta tissue lysates. c) Determination of...
Using of Micellar Electrokinetic Chromatography in the Analysis of Pharmaceuticals
Lípová, Markéta ; Pospíšilová, Marie (advisor) ; Polášek, Miroslav (referee)
In this work, micellar electrokinetic chromatography (MEKC) with UV detection at 214 nm was developed for separation of paracetamol, caffeine, ascorbic acid and chlorphenamin. The validated method was used for selective assay of the active substances in pharmaceutical preparation. The separations were optimised by examining a number of experimental conditions, such as the electrolytic system type and concentration, pH, concentration of sodium dodecyl sulphate (SDS), addition of organic solvents, separation voltage and temperature. The optimal operational system consisted of 40mM boric acid, 70mM SDS and 10% (v/v) of methanol (adjusted to pH* 7.6 with 1 M ammonia solution). Ethylparaben was chosen as an internal standard. The assay of compounds analysed was carried out at 30 kV and 20ř C with 60 cm x 75 µm I.D. fused silica capillary (effective length 50 cm). A single analysis took less than 10 min. The method was suitable for determining the drugs in pharmaceutical preparation TRIGRIP capsules with RSD values from 1,23% to 2,75% (n=3). The MEKC results agreed well with nominal contents of the compounds. The recovery of the method ranged from 90.43% to 99.59%.
Chemiluminiscenční hodnocení celkové antioxidační kapacity potravin
Vlčková, Jitka ; Polášek, Miroslav (advisor) ; Solich, Petr (referee)
Diplomová práce 2009 Abstract_ENG Jitka Vlčková ABSTRACT An investigation presented was concern to measure and evaluate the total antioxidant capacity (TAC) in samples of red wine clarified with four fining agents (polyvinylpolypyrrolidone and three different types of gelatin). All wine samples were treated by concentrations of 10, 20 and 40 g/hL of finings. The main aim was to discover how the particular agents in different dosages influence the TAC. The second part describes relations between changes in TAC in content of single antioxidant components (total polyphenols, anthocyanins, gallic acid and simple phenols). Total antioxidant capacity in red wine samples was evaluated using the Trolox equivalent antioxidant capacity assay (TEAC). A theoretical part of the thesis briefly summarizes basics about luminescence, focused on chemiluminescent reaction. Theory of free radicals and antioxidants, especially those included in red wine are also described. Process of winemaking aimed at fining is also contained in this part. An experimental part describes techniques of determination of the total antioxidant capacity, principle of chemiluminescent assay based on the luminol/peroxidase system. The results show the different behaviour of gelatin from the polyvinylpolypyrrolidone (PVPP). In general gelatin tends to...
Analysis of natural compounds by capillary isotachophoresis and capillary zone electrophoresis.
Černá, Veronika ; Pospíšilová, Marie (advisor) ; Polášek, Miroslav (referee)
It has been designed tITP - CZE method with a reversed electro-osmotic flow for the analysis of seven organic acids of natural origin. It was monitorated the effect of boric buffer concentration, pH effect, the addition of organic solvent, the addition of cyclodextrin, concentration of NaCl as a stacker, and injection time. Measurements were made in voltage - 30 kV in capillary with inner diameter 50 μm and effective length 68 cm. Optimum separation conditions were found at a concentration of 125mM boric buffer, pH 8,2, the addition of 0,001% hexadimethrinbromid and addition of 10mM and 2,6-di-O- methylcyklodextrin. The stacker was used at a concentration of 200mM NaCl and injection time was 90 s. Intracapillary thermal gradient from 20o C to 24řC during electrophoresis has yielded improved resolution for the analytes.
HPLC analýza makrolidových a tetracyklinových antibiotik v nemocničních odpadních vodách
Vrubl, Jaroslav ; Solich, Petr (advisor) ; Polášek, Miroslav (referee)
Analysis of macrolides and tetracyclines in hospital wastewaters by HPLC ABSTRACT Macrolide and tetracycline antibiotics are drugs used for treatment and prevention of infectional illnesses both in human and veterinary medicine. As other environmental contaminats, they can accumulate in environment and induce adverse effects in terrestrial and aquatic organisms. and induce bacterial resistance. The sensitive analytical methods are necessary to quantify their level in wastewaters to rate the risk caused by their presence in environment. The HPLC with MS detection is method mostly used to analysis, because of its high sensitivity. A method using UV or fluorescence detection was tried to be developed as an alternative to HPLC-MS. A method to analyse macrolide using Hichrom Lichrosorb RP 18, 250 x 4.6 mm i. d. and Chromolith Performance column RP 18e, 100 x 4.6 mm i. d. were used. A mobile phase ACN: 0.05M KH2PO4 (pH 7.5) 30:70 (v/v) was used, the detector was set at 215 nm. The method using pre-column derivatization by FMOC-Cl was studied. The analysis was performed on Chromolith Performance column RP 18e, 100 x 4.6 mm i. d. The fluorescence detector was set at excitation wavelength 255 nm and emission wavelength 315 nm. The method to analyse tetracyclines used gradient elution of ACN and 0.02 M oxalic acid....
Determination of flavonoids in food supplements using micellar electrokinetic capillary chromatography
Dvořáková, Martina ; Pospíšilová, Marie (advisor) ; Polášek, Miroslav (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate Mgr. Martina Dvořáková Consultant Doc. RNDr. Marii Pospíšilové, CSc Title of Thesis Determination of flavonoids in food supplements using micellar electrokinetic capillary chromatography A new method of micellar electrokinetic chromatography (MEKC) with UV detection for the simultaneous determination of catechin, epicatechin, rutin, quercetin, luteolin, hesperetin, kaempferol, apigenin and isorhamnetin was devised and validated. The MEKC analysis was optimized for the type, concentration and pH* of the background electrolyte, the concentration of sodium dodecyl sulphate (SDS), the type and concentration of cyclodextrins and organic solvents, applied voltage and operating temperature. The analysis was carried out in a fused-silica capillary (internal diameter 75 µm, total length 60 cm, effective length 50 cm) with UV detection at 210 nm, voltage 30 kV, hydrodynamic sample injection at 50 mbar for 6 s and temperature 20řC. The optimal background elektrolyte of pH* 7.6 (adjusted with 17% of ammonia solution) contained 5 mM potassium dihydrogen phosphate + 30 mM boric acid, 60 mM SDS, 20% (v/v) of methanol, 5% (v/v) of butanol and 8 mM 2-hydroxypropyl-γ-cyclodextrin. The calibration curve of...

National Repository of Grey Literature : 130 records found   1 - 10nextend  jump to record:
See also: similar author names
13 Polášek, Marek
2 Polášek, Martin
2 Polášek, Matěj
2 Polášek, Michal
2 Polášek, Miloslav
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