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Analytical evaluation of drugs using chromatographic methods IV.
Spáčilová, Lenka ; Mokrý, Milan (advisor) ; Kastner, Petr (referee)
Analytical evaluation of drugs by using chromatographic methods IV. Diploma Thesis Lenka Spáčilová Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Drug Control Heyrovského 1203, Hradec Králové Rapid analytical methods are described to control quality of honeys, concerning residues of acaricides applied in hives to prevent the mite Varroa jacobsoni infestation. Tau - fluvalinate was analysed by the use of a SGX RP-18C column, 5 µm, a acetonitrile : water (40:60) mobile phase, flow rate of 1 ml/min and a UV detector set at 254 nm. An internal standard was used for quantitative determination. A calibration curve was constructed and verified, by means of which the concentration of tau - fluvalinate in honey can be determined. The elaborated method was validated by detection limit determination.
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HPLC Evaluation of Transkarbam and Its Impurities II
Strašilová, Kateřina ; Sochor, Jaroslav (advisor) ; Mokrý, Milan (referee)
HPLC EVALUATION OF TRANSKARBAM AND ITS IMPURITIES II Rigorózní práce Mgr. Kateřina Strašilová Charles University in Prague, Fakulty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control, Heyrovského 1203, Hradec Králové This work deals with determination of 6-aminohexanoic acid in ointment-base by high performance liquid chromatography with subsequent validation of chromatographic conditions. 6-aminohexanoic acid is one of two main predicted degradation products of transkarbam 12, functioning as an enhancer of transdermal penetration. A pre-column derivatization with 3,5- dinitrobenzoylchloride forerun the quantification of 6-aminohexanoic acid. The analysis was run on the reversed-phase column Separon SGX C-18 (150 x 3 mm I.D., 5 μm) with gradient elution of mobile phase composed of acetonitrile and sodium acetate buffer (20 mM, pH 4,5) with the flow rate 1 ml/min. UV detection was performed at 230 nm. The validation parametres such as precision and accuracy, linearity, selectivity, robustness and limit of detection and limit of quantification were evaluated.
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The employment of separation methods in the field of drug analysis V.
Náplavová, Zdeňka ; Kučera, Radim (advisor) ; Mokrý, Milan (referee)
The employment of separation methods in the field of drug analysis V. Diploma thesis Zdeňka Náplavová Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Drug Analysis High performance liquid chromatography is currently a widely used analytical method. It is a highly selective separation method enabling sample analysis in very small quantities. HILIC - liquid chromatography based on hydrophilic interactions is an alternative method used for separation of polar compounds. It uses a polar stationary phase and a less polar mobile phase. The most commonly used stationary phases are silica , either bare or modified. Sillica gel is characterised by high selectivity, however, it is not stable in the whole pH range and it also loses stability at higher temperatures. Therefore, a priority is gained by a stationary phase with metal oxides, namely titania and zirconia. These sorbents are stable in the pH range 1-14 and at temperatures up to 200 řC. The thesis in hand deals with the stationary phase of carbon-coated zirconium dioxide under the conditions of hydrophilic interaction liquid chromatography. Based on the previously published measurements of bare ZrO2 sorbents and modified polybutadiene zirconia, the thesis offers a comparison of the carbon...
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Rapid quantification of acetylsalicylic acid using HPLC chromatograph
Levínská, Lucie ; Kastner, Petr (advisor) ; Mokrý, Milan (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Drug Control Candidate : Lucie Levínská Supervisor : PharmDr. Petr Kastner, Ph.D. Title of diploma thesis : Rapid quantification of acetylsalicylic acid using HPLC chromatograph In this work, a simple method of quick assessment of acetylsalicylic acid with the use of high-performance liquid chromatograph (HPLC) equipped with an UV detector set to the wavelength 265 nm was described and validated. The mobile phase was composed of methanol and water in the ratio 10:90. The temperature was set to 25řC, injection 10 µl and the flow rate adjusted to 0.3 ml/min. The method was validated by the following parameters of validation - linearity: r = 0.9999, accuracy: 100.88 % yield and repeatability: standard deviation 1.01%. The resulting values of validation were compared with the validation parameters of a method using a typical spectrophotometer. It was proved that both methods provide reliable results. However, the analysis with the use of HPLC proved to be quicker and simpler.
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HPLC evaluation of selected drugs I
Skryjová, Denisa ; Mokrý, Milan (advisor) ; Sochor, Jaroslav (referee)
61 ABSTRACT HPLC evaluation of selected drugs I. THESIS Denisa Skryjová Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control In this thesis were developed the optimum chromatographic conditions for simultaneous HPLC analysis of tramadol and paracetamol in combined tablet. The chromatographic column Discovery HS F5, 5 µm, 150×3 mm I.D. made by Supelco was chosen as the stationary phase. Mobile phase mixture formed acetonitrile : ammonium acetate solution 0.005 mol/l, acidified with acetic acid at pH 3.2 in the ratio 20:80 (v/v), at a flow rate of 1.0 ml/min. Acetylsalicylic acid was used as an internal standard. Detection took place at λ = 270 nm using a UV detector. The compounds were eluted in order of paracetamol, acetylsalicylic acid and tramadol.
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HPLC evaluation of some drugs IV.
Soukupová, Petra ; Mokrý, Milan (advisor) ; Sochor, Jaroslav (referee)
HPLC evaluation of some drugs IV. THESIS Petra Soukupová Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Analysis This thesis is about looking for the optimal conditions for simultaneous HPLC analysis in combined tablets of perindopril and indapamid with subsequent determination of their content. As the most suitable stacionary phase chromatographic column LiChro CART 250-4 LiChrospher 100, RP18, 5 µm was chosen, and the mobile phase formed by mixture of acetonitrile - ammonium phosphate solution (0,05 mol/l) in the ratio 40:60 with addition of triethylamine (0,1 ml/100 ml) acidified with phosporic acid at pH 3 at a flow rate of 1,4 ml/min and temperature 50o C. Propylparaben was used as the most suitable internal standard. The detection was performed at 215 nm using an UV detector. At the determination of content of medicaments in tablets was found that used compounds were eluted in following order: perindopril, indapamid and propylparaben.
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Metabolomic analysis of urine samples using ultra performance liquid chromatography and high resolution mass spectrometry
Mrvová, Andrea ; Mokrý, Milan (advisor) ; Stariat, Ján (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Drug Control Candidate: Andrea Mrvová Consultants: Prof. Seppo Auriola; Department of Pharmaceutical Chemistry, Faculty of Health Sciences, Kuopio, University of Eastern Finland RNDr. Milan Mokrý, CSc. Department of Pharmaceutical Chemistry and Drug Control, Faculty of Pharmacy in Hradec Králové, Charles University in Prague Title of Thesis: Metabolomic analysis of urine samples using ultra performance liquid chromatography and high resolution mass spectrometry Metabolomics is inquiring into the analysis of small-molecule metabolites within biologic system. This branch promises great progress not only as a diagnostic tool for disease. As suitable objects for the analysis are bio-fluids (e.g. urine, serum, saliva) and as common analytical techniques that are employed for the metabolomic analysis are NMR, GC/MS and LC/MS. Metabolomic analysis provides a great number of data and it is a problematic task to go through it. There is an effort to design system of effective identification. The aim of this work is to find optimal conditions for metabolomic analysis and to test reliability of computer-assisted workflow for the detection and identification of compounds. This should be as the first...
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Evaluation of selected active substances in the product using UHPLC V.
Socha, Adam ; Kastner, Petr (advisor) ; Mokrý, Milan (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Drug Control Candidate: Adam Socha Supervisor: PharmDr. Petr Kastner, Ph.D Title of diploma thesis: Evaluation of chosen active substance in the preparation by UHPLC V In this thesis there was developed and validated UHTLC method for the determination of sodium picosulphate, its related substances and sodium benzoate. The purpose of the project was to reduce the consumption of an organic solvents burdensome environment and simultaneously achieve sufficient sensitivity for the detection and quantification of the test substances. The LiChroCART® 125-4 LiChrospher® 60 RP-select B (5 µm) column with UV detection by 263 nm was used for the separation of substances at high temperature. The mobile phase was consisted of acetonitrile and buffer in the ratio 1:9. The buffer contained a triethylamine (TEA) at a final pH of 5,0 adjusted with acetic acid. The column oven was heated at 100 ř C, the flow rate was set at 0.4 ml / min and 2 µl injection volume was chosen. The method has been evaluated as sufficiently sensitive, precise, accurate, linear and selective. The evaluation of the robustness was tested by using Plackett-Burman design. It was found, that according to the tested parameters...
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Determination of clotrimazol and benzylalcohol in vaginal cream by means of HPLC
Chmurová, Klára ; Kastner, Petr (advisor) ; Mokrý, Milan (referee)
HPLC determination of clotrimazol and benzyl alcohol in vaginal cream Academic dissertation Klára Chmurová Charles University in Prague, Pharmaceutical Faculty in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control The task was to find out a method of simultaneous determination of clotrimazol and benzylalcohol in a vaginal cream. We were looking for proper modification of the pharmaceutical preparation (vaginal cream), then optimization of chromatographic conditions and validation of this HPLC method, too. The best results were obtained with DISCOVERY® HS F5, 5 µm, 4,5 × 150 mm together with the pre-column DISCOVERY® HS C18, 5 µm, 2,1 × 20 mm, mixture of acetonitril and buffer (K2HPO4 0,05mol/l, pH = 6,1 set up by 85% H3PO4) 60 : 40 (v/v) was used as the mobile phase, flow rate was 1 ml/min. Detection was realized by UV detector with wave length 223 nm. Time of analysis was shorter than 10 min.
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