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HPLC method development for artificial colorants determination in green beer samples
Stachová, Ivana ; Šatínský, Dalibor (advisor) ; Chocholoušová Havlíková, Lucie (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Bc. Ivana Stachová Supervisor: Doc. RNDr. Dalibor Šatínský, Ph. D. Title of diploma Thesis: HPLC method development for artificial colorants determination in green beer samples HPLC method was used and validated for the simultaneous determination of synthetic water- soluble dyes: E 102 - Tartrazine, E 104 - Quinoline Yellow, E 110 - Sunset Yellow, E 131 - Patent blue, E 132 - Indigo carmine, E 142 - Green S, E 133 - Brilliant Blue FCF and E 143 - Fast Green FCF. The method was applied for direct determination of these dyes in samples of green beers Jarní pivo 11ř (Primátor, Náchod), Krasličák 14ř (Ježek, Jihlava), Zelený král Vratislav 12ř (Konrád, Vratislavice), Velikonoční speciál 14ř (Starobrno, Brno), Velikonoční ležák 12ř (Radniční pivovar, Jihlava) Rohozec 11ř (Rohozec, Malý Rohozec), Zelená nefiltrovaná 12ř (Žlebské Chvalovice), Velikonoční zelený ležák 12ř (Purkmistr, Plzeň), Velikonoční kopřivová 12ř (Modrá Hvězda, Dobřany), Valášek 12ř (Valášek, Vsetín), Podkováň 12ř (Podkováň, Dolní Cetno). Analytical Chromolith Performance CN 100 x 4.6 mm column and guard column Chromolith CN 5 x 4.6 mm Merck were used and mobile phase contained 40% (v/v) methanol / 2% (v/v) acetic acid...
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Development and validation of method for determination of clotrimazole in cream using HPLC
Poláčková, Jitka ; Matysová, Ludmila (advisor) ; Chocholoušová Havlíková, Lucie (referee)
The topic of my work was to optimalize and to validate the method for determination of capacity of the Clotrimazol, degradeted product (2-chlorophenyl) diphenylmethanol and conservations (methylparaben and propylparaben) in the preparation Clotrimazol ointment. My effort for this work was to develop the method that could half for total separation the particular defined substance in this sample, in the acceptable time, to find inside standard, to optimalize the conditions of separation and the method verify. The optimum chromatographic conditions were found on column Zorbax SB - Phenyl, 3,5 μm, 4,6 x 75 mm in the flow of mobile phase 0,5 ml per minute and wave - length 210 nm. Composition of the mobile phase was acetonitrile - water (55:45), pH water component was modified by acid phosphoric 5 % on 3,2. If these conditions are used, this method is validating. The testing parameters were accuracy, correctness, linearity, selectivity, robustness, detection and quantitative limit and test if the chromatographic system is acceptable.
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Stanovení obsahu residuí kofeinu v povrchových vodách metodou HPLC s UV detekcí
Glosová, Ivana ; Solich, Petr (advisor) ; Chocholoušová Havlíková, Lucie (referee)
The occurence of caffeine residues was investigated in superrficial waters. The aim of this study was to obtain a first overview about contamination of waters from Mondego River and from source fontains near Coimbra city ( Portugal) with caffeine. The samples were preconcentrated by SPE ( Solid Phase Extraction) with Oasis polymeric column procedure and analysed by Liquid Chromatography (LC) with UV detektor ( 280nm). Mobile phase consist of 190 ml acetic acid glacial 100% and 810 ml of LC water (adjusted to pH 3.0 with acetate sodium) A total of twelve samples were collected in different site of Mondego River and from fountains near Coimbra city during three month's periods. A total of twelve samples of caffeine were analysed under the conditions described and none of them showed to be contaminated with caffeine.
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Development and validation of HPLC method for the determination of ketoprofen in suppositories
Zahálka, Lukáš ; Matysová, Ludmila (advisor) ; Chocholoušová Havlíková, Lucie (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Lukáš Zahálka Supervisor: PharmDr. Ludmila Matysová, Ph.D. Title of Diploma Thesis: Development and validation of HPLC method for the determination of ketoprofen in suppositories The purposes of diploma thesis were development and validation of HPLC method for the determination of ketoprofen in Ketonal® 100 mg suppositories. Ketoprofen belongs to NSAID and it is used for symptomatic therapy of inflammatory, degenerative and metabolic rheumatic diseases and for palliative therapy of some urgent or chronic painful syndromes. During development of determination of ketoprofen in suppositories were used two methods, which were developed at the Faculty of Pharmacy in Hradec Králové. Method for determination of diclofenac in suppositories was default for sample preparation and method of HPLC determination of ketoprofen, methylparaben and propylparaben in gel was basic for conditions of HPLC analysis. Development of method consisted in modification of origin sample preparation method; chromatographic conditions have not been changed. During the experimental work was found to determine what influence has the various steps of sample preparation and extraction temperature. The time of extraction...
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Monitoring of Retention "U-profiles" of Selected Substances on Pentafluorophenyl Stationary Phase
Havlátová, Michaela ; Šatínský, Dalibor (advisor) ; Chocholoušová Havlíková, Lucie (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Analytical Chemistry Department Candidate: Mgr. Michaela Havlátová Consultant: Doc. RNDr. Dalibor Šatínský, PhD. Rigorous Thesis Title: Retention "U" profiles testing of selected substances on pentafluorophenyl stationary phase Retention "U" profiles were examined on pentafluorophenyl stationary phase at selected substances. For testing there were chosen substances from the group of tetracycline antibiotics (oxytetracycline, minocycline), neuroleptics (thioridazine, perphenazine), local anesthetics (lidocaine, prilocaine), methylxanthine derivates (caffeine, theophylline), ß-sympatholytics (acebutolol, bopindolol) and aniline. During the analysis the retention profiles of the tested substances were observed as influenced by the character of methanol mobile phase. Three analysis series were carried out at all of the tested substances. In analysis series number 1 the mobile phase methanol - water was used. For analysis series number 2 it was the mobile phase methanol - phosphoric acid 0,085% and for analysis series number 3 it was the mobile phase methanol - acetate buffer solution pH 7. In each analysis the methanol percentage in the mobile phase was changed. In the group of the tested substances the U-shaped retention profile was...
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Study of influence of mobile phase composition on selectivity and retention of the analytes on HILIC stationary phases
Štětková, Kateřina ; Vlčková, Hana (advisor) ; Chocholoušová Havlíková, Lucie (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Kateřina Štětková Supervisor: RNDr. Hana Vlčková, Ph.D. Title of Diploma thesis: Study of influence of mobile phase composition on selectivity and retention of the analytes on HILIC stationary phases This graduation thesis deals with an influence of concentration of ACN, pH and buffer concentration in mobile phase on retention of selected analytes and on selectivity of Atlantis HILIC Silica column (3 μm, 2,1 mm x 100 mm) and Luna NH2 column (3 μm, 2,0 mm x 100 mm). A set of 35 analytes including neutral, basic and acidic compounds were chosen for this study. Detection was performed by PDA detector at the wave-length of 245 nm. Measurements were carried out using isocratic flow 0.4 ml.min-1 of mobile phase ACN/water (buffer). The column temperature was set up to 30 řC, auto sampler temperature to 4 řC and injection volume to 2 µl. For easier evaluation of results, measured data are presented in charts and tables. These were used to evaluation of columns in terms of selectivity and retention of the individual groups of analytes. The typical HILIC behavior, an increasing retention of analytes with increasing ACN concentration in mobile phase, was observed for Atlantis HILIC Silica column....
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Development of HPLC method for the determination of 6-gingerol, capsaicin, 8-gingerol, 6-shogaol and 10 gingerol in Zingiber officinale samples
Urbanová, Martina ; Chocholoušová Havlíková, Lucie (advisor) ; Matysová, Ludmila (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Martina Urbanová Supervisor: PharmDr. Lucie Havlíková, Ph.D. Title of Diploma Thesis: Development of an HPLC method for the determination of 6-gingerol, capsaicin, 8-gingerol, 6-shogaol and 10-gingerol in Zingiber officinale samples The diploma thesis was focused on the development of an HPLC method for the determination of 6-gingerol, capsaicin, 8-gingerol, 6-shogaol and 10-gingerol in Zingiber officinale samples. At first, freshly prepared rhizome samples of ginger were selected. Afterwards, levels of analytes in model dried ginger powder samples were evaluated. 6-gingerol had always showed highest response in both fresh rhizome samples of ginger and dried ginger powder samples. Capsaicin has not been found in any sample. 6-shogaol has only been found in dried ginger powder samples. Extraction of other substances depended on the methodology of preparation of particular samples. During the optimization of this method, various mobile and stationary phases were examined. The suitable mobile phase was composed of acetonitrile and water in 50/50 (v/v) ratio. Ascentis® Express Phenyl-Hexyl analytical column (100 x 4.6 mm; 2.7 µm) was chosen as a stationary phase for analysis, which was also...
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The Development and Validation of HPLC Methods for Determination of Ketoprofen in Pharmaceutical Preparations
Bajcurová, Lucie ; Matysová, Ludmila (advisor) ; Chocholoušová Havlíková, Lucie (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Mgr. Lucie Bajcurová Consultant: PharmDr. Ludmila Matysová, Ph.D. Title of Thesis: The Development and Validation of HPLC Methods for Determination of Ketoprofen in Pharmaceutical Preparations The already developed method for determination of ketoprofen in the pharmaceutical preparation "PRONTOFLEX" - a 10% skin spray has been validated. The precision expressed as relative standard deviation was 1.43 %. The accuracy expressed as recovery was 101.52 %. The correlation coefficient R was more than 0.999. The method for determination of ketoprofen in the pharmaceutical preparation "Ketonal" - a 5% cream has been further developed. The already developed method has been validated. The chromatographic separation was performed on a SUPELCO Discovery C18 column (150 mm x 4.6 mm, 5 µm). The mobile phase consisted of a mixture of acetonitrile, water and a phosphate buffer pH 3.5 (39:59:2, v/v/v). At a mobile phase flow rate of 1.5 ml/min, injection volume of 5 μl and UV detection at a wavelength of 233 nm, the total time of analysis was less than 10 minutes. Ethylparaben was used as an internal standard. The precision expressed as relative standard deviation was 0.64 %. The accuracy expressed as...
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Determination of vitamine C and dehydroascorbic acid using UHPLC-MS method
Proroková, Zuzana ; Nováková, Lucie (advisor) ; Chocholoušová Havlíková, Lucie (referee)
A coupling of Ultra High Performance liquid chromatography with mass spectrometry provides a technique, which is rapid and sensitive. This thesis is focused on the use of UHPLC-MS for the determination of ascorbic acid (AA) and dehydroascorbic acid (DHA). AA is a small polar molecule that acts as an antioxidant. After oxidation AA creates DHA. AA/DHA ratio is an indicator of a redox state of organism. For the determination of AA and DHA several methods have been developed, which usually do not allow the simultaneous analysis, but require multistep subtraction procedure. The optimization of UHPLC-MS method for the determination of AA and DHA include the choice of mobile and stationary phase and mass spectrometry detector set- up. The choice of appropriate conditions depended mainly on retention time and the detector response. The effect of stationary phase, concentration, pH, composition of mobile phase on retention of AA and DHA was observed. Effect of mobile phase on stability of AA and DHA was observed as well. BEH Shield RP C18, BEH HILIC and BEH Amide column were compared. The best results were achieved on column BEH Shield RP C18. Measurements with 0.1%, 0.05%, 0.01% formic acid, 0.1%, 0.05%, 0.01% acetic acid, ammonium formate at pH 3.5 and amonium acetate at pH 4.4 and 6.8 as a water...
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