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The use of capillary electromigration methods in pharmaceutical / / analysis
Petriška, Ivan ; Polášek, Miroslav (advisor) ; Urbánek, Marek (referee) ; Blešová, Marie (referee)
8 SHRNUTÍ Tato práce představuje možnosti využití tří účinných separačních technik založených na elektromigraci analytů, jako jsou kapilární izotachoforéza (ITP), kapilární zónová elektroforéza (CZE) a micelární elektrokinetická chromatografie (MEKC), v analýze farmaceuticky významných látek a to jak syntetického původu v matrici léčivého přípravku, tak především přírodního původu v extraktech léčivých rostlin resp. rostlinných silicích. V teoretické části je věnován poměrně velký prostor popisu těchto metodik a zejména jejich širokému uplatnění ve farmaceutické analýze přírodních látek (tabulky 1, 2 a 3) a dále možnostem ovlivnění separace elektricky neutrálních analytů vlivem přídavku komplexujícího činidla či povrchově aktivní látky do základního elektrolytu. Součástí práce je také přehledná rešeršní publikace (příloha I), shrnující uplatnění elektromigračních metod v kontrole kvality lékopisných rostlinných drog. První experimentální práce (příloha II) ukazuje na možnost použití kapilární izotachoforézy ve farmaceutické analýze ke kontrole obsahu léčivé látky. Stanovení významného sympatomimetika tetryzolinu a antihistaminika antazolinu v hromadně vyráběných nosních a očních kapkách ukazuje, že vyvinutá, optimalizovaná a validovaná ITP metoda poskytuje přesné a správné výsledky. Hlavní výhody navržené...
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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...
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Determination of biologically active substances by sequential injection analysis with chemiluminescence detection.
Štěpánková, Lucie ; Polášek, Miroslav (advisor) ; Sklenářová, Hana (referee)
1.1 Abstrakt A simple and rapid automated method for the assay of norepinephrine by sequential injection analysis (SIA) with chemiluminescence detection was devised and optimised. The optimised parameters were aspirated volumes of the norepinephrine bitartrate sample and reagents, flow rate, composition of the carrier stream and the photomultiplier voltage. Optimum sample volume was 80 μl and the optimum reagent concentrations (and aspirated volumes) were - 25 mM sodium polyphosphate (44 μl), 0,1 M sulphuric acid (24 μl) and 1 mM potassium permanganate (21 μl)., The optimum flow rate (for pushing the luminescent zone to the detector) was 91 μl/s and the photomultiplier voltage was 450 V. The carrier stream was ultrapure water. The calibration curve was rectilinear in the range 1 - 40 µmol/l of norepinephrine bitartrate. The parameters of the calibration curve y = kx + q (where y is the intensity of chemiluminescence in nA and x stands for the concentration of norepinephrine bitartrate in µmol/l) were calculated by the linear regression method. The slope k was 33.923 and the intercept q was 34.839. The correlation coefficient was 0.9997. The relative standard deviations were 2.78 or 1.18 % (n = 10) when determining 4.75 or 18.98 µmol/l norepinephrine bitartrate in pure standard solutions respectively. The...
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Optimization of the Determination of Septonex in Pharmaceutical Preparations by Capillary Zone Electrophoresis with Use of Organic Solvents as Additives in the Background Electrolyte
Šindelková, Martina ; Polášek, Miroslav (advisor) ; Pospíšilová, Marie (referee)
OPTIMIZATION OF THE DETERMINATION OF SEPTONEX IN PHARMACEUTICAL PREPARATIONS BY CAPILLARY ZONE ELECTROPHORESIS WITH USE OF ORGANIC SOLVENTS AS ADDITIVES IN THE BACKGROUND ELECTROLYTE A new method of capillary zone electrophoresis with contactless conductivity detection for the determination of septonex in pharmaceutical preparations was devised. Optimal conditions for the separation and determination of septonex were: background electrolyte 30mM MES of pH 7.0 (adjusted with 200mM TRIS) containing 12.5mg/ml of (2- hydroxypropyl)-β-cyclodextrin and 20% (volume), voltage 25kV, temperature 25řC and sample injection for 6 seconds under the pressure of 50mbar. Arginin (200µg/ml) was used as internal standard. The peak of septonex was satisfactorily separated from the peak of internal standard as well as from the EOF. The analysis was carried out in a fused-silica capillary (internal diameter 50μm, total length 75cm and the length to the detector 45cm). The separation took less than 5 minutes and the overall analysis time involving appropriate rinsing of the capillary was less than 13 minutes. The calibration curve was linear in the range 75µg/ml - 400µg/ml of septonex, correlation coefficient r = 0.9997. The LOD was 13,5μg/ml and LOQ was 45μg/ml of septonex. The method is applicable for qualitative as...
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Chemiluminiscenční hodnocení celkové antioxidační kapacity potravin
Vlčková, Jitka ; Polášek, Miroslav (advisor) ; Solich, Petr (referee)
Diplomová práce 2014 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...
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Determination of Sibutramine in Pharmaceutical Preparations by Capillary Zone Electrophoresis
Korejsová, Tereza ; Pospíšilová, Marie (advisor) ; Polášek, Miroslav (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytická chemie Candidate Mgr. Tereza Korejsová Consultant doc. RNDr. Marie Pospíšilová, CSc Title of Thesis Stanovení sibutraminu ve farmaceutických přípravcích metodou kapilární zónové elektroforézy A simple capillary zone electrophoresis (CZE) with sulfated β - CD as chiral selector has been developed for separation and quantitative analysis of R - and S - sibutramine (SIB). The method was used for the assay of racemic sibutramine in pharmaceutical preparations Meridia®, Lindaxa®, Sibutramin Sandoz® and Sibutramin Teva®. The separation was optimized by testing the parameters such as buffer type and its concentration, buffer pH, type and concentration of chiral selectors, separation temperature and voltage. The analyses were carried out using a polyacrylamide-coated capillary (PAA) with total length 30 cm and 50 µm ID. Optimum conditions for separation of the enantiomers of sibutramine were achieved with 100 mM phosphate buffer of pH 3,0 (adjusted by TRIS) containing 2,0 mM sulfated β - CD. The applied voltage was 15 kV and the capillary temperature was kept constant at 180 C. The total analysis time took about 5 - 6 minutes. Regression equation showed good linear relationships in the range 5 - 250 µg/ml of each...
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Use of capillary electrophoresis with contactless conductivity detection for the analysis of proteins
Vatrasová, Kateřina ; Polášek, Miroslav (advisor) ; Jáč, Pavel (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Bc. Kateřina Vatrasová Supervisor: doc. RNDr. Miroslav Polášek, CSc. Consultant: PharmDr. Klára Petrů, Ph.D. Title of Diploma Thesis: Use of capillary electrophoresis with contactless conductivity detection for the analysis of proteins Nowadays there exist many methods for the determination of proteins. The aim of this work was to develop, optimize and characterize method for the analysis of a model mixture of proteins (α-lactalbumin, β-lactoglobulin, carboanhydrase, lysozyme and ribonuclease) by capillary electrophoresis with conductivity detection and to compare it with conventional capillary electrophoresis with UV detection. The influence of the capillary inner wall coating on the adsorption of proteins, the composition and concentration of convenient background electrolyte, and the voltage and temperature were examined as experimental conditions possibly affecting the separation. A 50-cm fused-silica capillary (effective length 35 cm for conductivity detector and 41.5 cm for UV detector) with internal diameter 50 μm was used for the analysis. The UV detection wavelength was 210 nm. The static coating of the inner capillary wall realized by successive multiple soaking with...
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Determination of septonex in pharmaceutical preparations by capillary zone electrophoresis with conductivity detection.
Šindelková, Martina ; Polášek, Miroslav (advisor) ; Pospíšilová, Marie (referee)
DETERMINATION OF SEPTONEX IN PHARMACEUTICAL PREPARATIONS USING CAPILLARY ZONE ELECTROPHORESIS WITH CONTACTLESS CONDUCTIVITY DETECTION A new method of capillary zone electrophoresis with contactless conductivity detection for the determination of septonex in pharmaceutical preparations was devised. Optimal conditions for the separation and determination of septonex were: background electrolyte 30mM MES of pH 7.0 (adjusted with 20mM TRIS) containing 12.5mg/ml of (2- hydroxypropyl)-β-cyclodextrin, voltage 25kV, temperature 25řC and sample injection for 15 seconds under the pressure of 50mbar. N,N-dimethylethanolamine (200µg/ml) was used as internal standard. The peak of septonex was satisfactorily separated from the peak of internal standard as well as from the EOF. The analysis was carried out in a fused-silica capillary (internal diameter 50μm, total length 75cm and the length to the detector 45cm). The separation took less than 4 minutes and the overall analysis time involving appropriate rinsing of the capillary was less than 16 minutes. The calibration curve was linear in the range 75µg/ml - 300µg/ml of septonex, correlation coefficient r = 0.9976. The LOD was 9μg/ml and LOQ was 30μg/ml of septonex. Unsuitable repeatability of peak areas of septonex (caused probably by insufficient elimination of...
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