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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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The metod development for determination of diazodinitrofenol explosive
Ihnát, Lukáš ; Šatínský, Dalibor (advisor) ; Chocholoušová Havlíková, Lucie (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Consultant: Doc. RNDr. Dalibor Šatínský, PhD. Diploma Thesis Title: The method development for determination of diazodinitrofenol explosive A new HPLC method for determination of diazodinitrophenol alongside with sodium picramate was developed and optimized. Column Ascentis® Express C18 10cm x 3mm; 2.7µm particles was select as most suitable one. Detection of compounds was performed at 220 nm using UV detector. Mobile phase consist of mixture 0.085% H3PO4 and acetonitrile in ratio 70/30. Flow rate was determined at 0.8 ml/min. Column oven temperature was set to 50řC. Retention times under these condition was tDDNP=1.324 min a tPikNa=4.012 min. Keywords: determination, diaziodinitrophenol, sodium picraminate, HPLC, chromatography, dinol, DDNP
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Forced degradation studies of anthelmintics in the process of stability testing of pharmaceuticals
Kameníčková, Marcela ; Chocholoušová Havlíková, Lucie (advisor) ; Šatínský, Dalibor (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Marcela Kameníčková Supervisor: PharmDr. Lucie Havlíková, Ph.D. Title of Diploma Thesis: Forced degradation studies of anthelmintics in the process of stability testing of pharmaceuticals The goals of this thesis were to perform stress tests of selected anthelmintic praziquantel in the preparation process of stability studies of Caniverm®. The samples were exposed to extreme conditions to accelerate the chemical decomposition of a drug substance. The content of active substances and the formation of degradation products were observed. The aims of the tests were to determine the basic properties of a substance or product in model stress situations, simulating the extreme conditions during production, storage, transport and effects of external influences, to characterize degradation products and to verify the suitability of methods for analysis of degradation products. The developed method was partially validated by parameters linearity and precision. Praziquantel is stable in methanol and water. Degradation product "RP 1" has been formed in the 2% sulfuric acid solution. RP 1 is characterized by retention time of tR 4.5 min. Degradation product "RP 2" with retention time of tR 4.9 min...
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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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Detekce a kvantifikace trinitrotoluenu v reálných vzorcích s použitím metody ELISA
Hanusová, Lucia ; Chocholoušová Havlíková, Lucie (advisor) ; Chocholouš, Petr (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of: Analytical chemistry Candidate: Lucia Hanusová Supervisor in Hradec Králové: PharmDr. Lucie Havlíková Ph.D Supervisor in Bologna: Prof. Steffano Girotti Title of Diploma Thesis: Detection and quantification of trinitritoluene in real samples by using ELISA method. The 2,4,6-trinitrotoluene (TNT) is a widely used explosive. TNT has been used extensively in the manufacture of explosives since the beginning of last century. It could be found as a contaminant in environment, contaminates air, water and soil. It is accumulated in plants and fishes, and could affect human health. A reliable and sensitive method is needed to get the information about pollution in environment, to detect exposion in human organism or to identify the explosive after explosion. A new rapid method of indirect competitive Enzyme-Linked ImmunoSorbent Assay method with chemiluminescent detection (CL-ELISA) for determination of trinitrotoluene in real samples was successfully applied. The immunological analysis using many antibodies was performed after extraction to methanol (MeOH). The antibody labelled with horse-radish peroxidase was added to reaction and after combination with luminescent mixture the light was developed and we were able to...
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Vývoj imunochromatografického stanovení pro testování reálných vzorků obsahujících TNT
Kosařová, Lucie ; Chocholouš, Petr (advisor) ; Chocholoušová Havlíková, Lucie (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical chemistry Candidate: Lucie Kosařová Supervisor: PharmDr. Petr Chocholouš, Ph.D. Title of diploma thesis: Development of lateral flow immunoassay for testing real samples containing TNT Obtaining results very fast is requested more often these days. This is particularly true for dangerous and potentially dangerous compounds. One of these compounds is 2,4,6,-trinitrotoluene (TNT), which was tested in this research. TNT has been extensively used as a military explosive and is still one of the most widely used explosives. Its advantages, such as low manufacturing costs, safety of handling and fairly good explosive power can be tempting for abuse by terrorists. In addition, TNT is a well known pollutant because of its toxicity and low biodegradability. It can contaminate surface and ground waters, soils and sediments, thus causing environmental and health problems. According to these facts there is a requirement to detect this nitroaromatic compound in minimal concentrations very fast and outside the laboratory. These demands could be met by the lateral flow test. In this research lateral flow immunoassay (LFIA) based on colloidal gold nanoparticle labels was developed for detection of TNT in real samples. The...
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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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HPLC method devolopment for betacarotene determination in nutraceuticals
Hlaváčková, Markéta ; Šatínský, Dalibor (advisor) ; Chocholoušová Havlíková, Lucie (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Bc. Markéta Hlaváčková Consultant: Doc. RNDr. Dalibor Šatínský, Ph.D. Diploma Thesis Title: Development of HPLC Method for the Determination of Betacarotene in Nutritional Supplements A new HPLC method was optimized and developed for the determination of betacarotene contents in nutritional supplements Betakaroten Farmax, GS Betakaroten FORTE (GreenSwan pharmaceuticals), Walmark Betakaroten, Bioaktivní karoten (Pharma Nord Denmark), Beta karoten Max, BETAVID + LUTEIN (Naturvita), Karovit (Vitabalans Oy), SELZINK PLUS (PRO.MED.CS), Pupalkový olej (Aromatica). The method is based on using Ascentis Express C18 column (30 x 4.6 mm; 2.7 µm) and UV detection at 450 nm. There was used isocratic elution of the mobile phase 100% methanol at a flow-rate of 1.5 ml/min. Column oven temperature was set at 60 řC during the measurement. The retention time of betacarotene under the optimized and validated conditions was 2.185 min. Keywords: betacarotene, HPLC, Betakaroten Farmax, GS Betakaroten FORTE (GreenSwan pharmaceuticals), Walmark Betakaroten, Bioaktivní karoten (Pharma Nord Denmark), Beta karoten Max, BETAVID + LUTEIN (Naturvita), Karovit (Vitabalans Oy), SELZINK PLUS (PRO.MED.CS), Pupalkový olej...
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Nová HPLC metoda pro stanovení nafazolinu v očních přípravcích
Dulavová, Martina ; Chocholoušová Havlíková, Lucie (advisor) ; Matysová, Ludmila (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Martina Dulavová Supervisor: PharmDr. Lucie Havlíková, Ph.D., Ass.Prof. Hannelore Kopelent Title of Diploma Thesis: A New Selective and Stability Indicating HPLC Assay for the Determination of Naphazoline in Preparations for Ocular Use Naphazoline is a 2-imidazolidine derivated drug and alpha-adrenergic agonist with vasoconstrictive and decongestive properties. Naphazoline is indicated for the therapy of rhinitis, sinusitis or allergic conjunctivitis. Naphazoline is used in liquid formulations for ophthalmic and nasal application. Naphazoline is marketed in a number of commercially available products; for example, it is contained in Coldan® Augentropfen. Due to economic and therapeutic reasons, hospital pharmacies produce miscellaneous in-house preparations. For our study, two different preparations manufactured in the sterile production of a hospital pharmacy containing naphazoline are investigated. The first formulation is based on two commercially available products and it is a mixture of Coldan® Augentropfen and Okuzell® Augentropfen at a ratio of 1:9. The second formulation is Bor-Naphazolin Augentropfen and it is completely prepared in a hospital pharmacy. In addition to...
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Development of GC Metod for the Determination of Vitamine E Acetate in Nutritive Supplements
Kymlová, Helena ; Šatínský, Dalibor (advisor) ; Chocholoušová Havlíková, Lucie (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Mgr. Helena Kymlová Consultant: Doc. RNDr. Dalibor Šatínský, PhD. Title of Thesis: Development of GC metod for the determination of vitamine E acetate in nutritive supplements A GC method was developed for the determination of content of vitamine E acetate in nutritive supplements. The method was optimised and validated. The column Capillary GC, Equity Columns, Equity TM - 5 poly (5 % bifenyl / 95 % dimethylpolysiloxan); 0,32 mm ID x 30 m; 1,0 mm dr was used for the analysis. Helium was used as a carrier. Split was 1 : 100. Flame-ionization detector was used for detection. Optimal conditions for analysis: temperature of column 340 řC, temperature of injection 340 řC, temperature of detector 320 řC, flow-rate 2 ml/min. Fenoxycarb was chosen as an internal standard. The method was used for an analysis of vitamine E acetate in nutritive supplements Geladrink Forte pulverized drink - pineapple and Chondrotin MSM 2600. Determined concentration of vitamine E acetate was re-counted to the content of vitamine E declared by producer.
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