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The comparison of different types of stationary phases in HPLC analysis of medicament Diclofenac emulgel
Poláčková, Jitka ; Matysová, Ludmila (advisor) ; Karlíček, Rolf (referee)
The aim of this rigorous work is a comparison of different types of stationary phases for the analysis of the drug Diclofenac emulgel. It is necessary to take into account the many specialized materials from the pharmacopoeias, ICH guidelines and professional scientific journals in solution of the development of HPLC methodology, validation and choice of stationary phase analytical columns. Several types of stationary phases were tested, with the testing of conditions of the separation of active substances from the pharmaceutical formulation - diclofenac emulgel. The best results were placed on Discovery HS-F5 (15 cm x 4.6 mm, 5 m), time analysis was less than 4 minutes; Zorbax SB - CN (4.6 x 150 mm, 5 m) time of analysis was less than 5 min; Chromolith Performance RP - 18e (100 - 3 mm) time analysis was less than 3 minutes.
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Development of HPLC methods for analytical evaluation of drug products and model studies of natural degradation of drug residues.
Nejedlý, Tomáš ; Klimeš, Jiří (advisor) ; Karlíček, Rolf (referee) ; Mikuš, Peter (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Pharmaceutical Analysis Candidate Mgr. Tomáš Nejedlý Supervisor prof. RNDr. Jiří Klimeš, CSc. Title of Doctoral Thesis Development of HPLC methods for analytical evaluation of drug products and model studies of natural degradation of drug residues The presented doctoral thesis describes two areas of pharmaceutical analysis. The first part is focused on development of validated chromatographic methods for pharmaceutical-analytical assesment of drug products and their rutine use in quality control laboratories. The second part deals with the very actual topic of environmental analysis and residues of pharmaceutical substances in sewage and surface water. The first developed method is suitable for quality evaluation of cream dosage forms containing aciclovir active substance. This method is suitable for assay of active substance and its three related substances. In addition it is validated for assay of preservatives contained in cream base. The second chromatographic method is developed for determination of tablets containing 1 mg of risperidone antipsychotic drug per tablet. This method was validated for active substance assay and the four mostimportant pharmacopoeial impurities. The last method is...
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Modern chromatographic techniques in food contamination analysis
Lhotská, Ivona ; Šatínský, Dalibor (advisor) ; Karlíček, Rolf (referee) ; Malíř, František (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate Mgr. Ivona Lhotská Supervisor doc. RNDr. Dalibor Šatínský, Ph.D. Title of Doctoral Thesis Modern chromatographic techniques in food contamination analysis A compilation of seven publications dealing with chromatographic methods for determination of food contamination (particularly mycotoxins and artificial food colorants) is presented in dissertation thesis. All methods were fully validated, complying with the requirements and applied for real samples analysis. The first part describes the methods for mycotoxins determination based on on-line solid phase extraction (SPE) utilizing column-switching system. Reversed phase columns packed with superficially porous particles were chosen for both extraction and separation step during optimization of on-line SPE-HPLC method for ochratoxin A and citrinin determination in beer. In following work, determination of patulin in juices and zearalenone in beer, more selective molecularly imprinted polymers (MIP) were used for on-line extraction. Due to challenging optimization of on-line MIP SPE, the methods were compared to off-line MIP extraction and on-line extraction using conventional C18 phase to confirm the selectivity. The employed commercial MIP...
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Application of modern technologies for treatment of biological samples for HPLC analysis.
Dědečková, Klára ; Solich, Petr (advisor) ; Karlíček, Rolf (referee)
This diploma thesis is dealing with a using of new technologies for the treatment of biological material in the HPLC analysis. The main aim of this thesis was miniaturization of solid phase extraction process of blood serum on classical SPE columns to SPE plates for determination of liposoluble vitamins A and E by high performance liquid chromatography. The new extraction method for vitamin A and E in blood serum using the modern format of SPE plate was developed and optimized. This new method mineralizes a blood serum volume, makes sample treatment easy and can speed up the analysis.
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Determination of mycotoxin citrin using on-line SPE HPLC on molecularly imprinted polymers
Kholová, Aneta ; Šatínský, Dalibor (advisor) ; Karlíček, Rolf (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Bc. Aneta Kholová Supervisor: Doc. RNDr. Dalibor Šatínský, Ph.D. Title of Diploma Thesis: Determination of mycotoxin citrinin using on-line SPE HPLC on molecularly imprinted polymers The aim of this work was to develop a fast method for mycotoxin citrinin (CIT) determination using high performance liquid chromatography (HPLC) and column switching technique in combination with on-line solid phase extraction (SPE) based on citrinin-selective molecularly imprinted polymer (MIP). The most suitable sorbent for selective extraction was chosen from six newly synthetized MIP after evaluation of their binding capacity and selectivity. Selectivity was tested by comparing molecularly imprinted and non-imprinted polymers and the ability of the MIP polymer to selectively separate citrinin from interferences of the test sample. The best MIP (functional monomer of metacrylamide with porogen acetonitrile) was filled into pre-column (20 × 3 mm) and connected to HPLC column-switching system. Three different matrices were injected to chromatographic system. 50 μl of the sample was injected onto MIP extraction column and washed out of interferences with methanol / 0.5% water solution of acetic acid in a ratio of...
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The Use of Modern Chromatographic Approaches and Sample Preparation in the Analysis of Biologically Active Substances
Brabcová, Ivana ; Šatínský, Dalibor (advisor) ; Karlíček, Rolf (referee) ; Tolarová, Jitka (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Mgr. Ivana Brabcová Supervisor: Doc. RNDr. Dalibor Šatínský, Ph.D. Title of thesis: The use of modern chromatographic approaches and sample preparation in the analysis of biologically active substances The presented thesis deals with the modern trends in liquid chromatography and in the analysis of biologically active substances. High performance liquid chromatography (HPLC) is an important analytical tool for separating and quantifying components of mixtures. New trends of HPLC technology tend to development of new stationary phases with better properties. Another trend in analytical chemistry is a miniaturization of the HPLC system and environmentally friendly chromatography. Sample preparation is an essential step in analysis, greatly influencing the reliability and accuracy of analysis. Nowadays, the development is focused on new modern techniques of sample preparation. The developments of these techniques lead up to miniaturization, automatization and preconcentration of target analytes. The theoretical part of the thesis deals with the introduction of modern trends in liquid chromatography and it is divided in several sections. First part describes current trends in fast liquid...
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