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Analytical Evaluation of Drugs and Drug Candidates from the Group of Iron Chelating Agents
Stariat, Ján ; Klimeš, Jiří (advisor) ; Šatínský, Dalibor (referee) ; Šišpera, Luděk (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Department of Pharmaceutical Chemistry and Drug Control Candidate Mgr. Ján Stariat Supervisor Prof. RNDr. Jiří Klimeš, CSc. Title of Doctoral Thesis Analytical evaluation of drugs and drug candidates from the group of iron chelating agents High performance liquid chromatography (HPLC) ranks among the most important analytical techniques in the field of pharmaceutical analysis thanks to its robustness and the ability to separate and qualitatively and quantitatively analyse the compounds presented in various samples. The ongoing progress in the development of novel stationary phases and detection techniques allows rapid analysis and to get comprehensive characterization of the analytes presented in the complex samples even at very low concentrations. Cancer still remains a leading cause of death, thus the need for novel, efficient treatment strategies is of crucial importance. The mechanism based on iron chelation (Fe) inside the tumour cells represents one of the most promising strategy which could enhance the prognosis of patients suffering from cancer resistant to standard chemotherapy. Thiosemicarbazone iron chelators are currently under intensive development as novel anticancer drugs. Their strong antiproliferative...
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Development and applications of affinity carrier for isolation of human carbonyl-reducing enzymes
Andrýs, Rudolf ; Wsól, Vladimír (advisor) ; Šebela, Marek (referee) ; Šatínský, Dalibor (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Biochemical Sciences Candidate: Mgr. Rudolf Andrýs Supervisor: Prof. Ing. Vladimír Wsól, Ph.D Title of dissertation thesis: DEVELOPMENT AND APPLICATION OF AFFINITY CARRIER FOR ISOLATION OF HUMAN CARBONYL-REDUCING ENZYMES For several millennia the human medicine is based on application of small bioactive molecules that are administered in the form of plant extracts or synthetic compounds. However, their use in modern medicine is not possible without a detailed understanding of their biochemical effects and identification of their molecular targets. Chemical proteomics based on the specific recognition between the bioactive molecule and the target molecule is currently the most widely used techniques for identification of molecular targets of small molecules. Compared to conventional biochemical methods (e.g. 2D electrophoresis), chemical proteomics represents particularly sensitive and very selective technique that enable successful identification of biomolecules from complex biological samples that are naturally presented in very small concentrations. Carbonyl- reducing enzymes, which play an important role in physiology due to their involvement in metabolism of various endogenous (e.g. prostaglandins, steroid...
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The possibilities of utilization of alternative stationary phases in pharmaceutical analysis
Kalafut, Peter ; Klimeš, Jiří (advisor) ; Šatínský, Dalibor (referee) ; Chládek, Jaroslav (referee)
University Charles University in Prague Faculty Faculty of Pharmacy in Hradec Králové Department Department of Pharmaceutical Chemistry and Drug Control Candidate Mgr. Peter Kalafut Supervisor Prof. RNDr. Jiří Klimeš, CSc. Title of Doctoral Thesis The possibilities of utilization of alternative stationary phases in pharmaceutical analysis. The significance of metal-based HPLC stationary phases, mainly the zirconia, has arisen, recently. Zirconia-based phases came in the awareness of professional community mainly thanks to the versatile stability in different mobile phases and high temperatures as well as to the ability to provide very different selectivity as compared to common silica concurents. The theoretical part of this doctoral thesis provides general overview of liquid chromatography and also describes the recent instrumentation. The main part is devoted to a bibliographic search dealing in detail with the properties of zirconia-based stationary phases and consequent applications in the analytical practice. The fundamental of this thesis is represented by the experimental part, which studies the chromatographic behaviour of some chosen types of zirconia-based stationary phases and their potential use in HPLC analysis emphasizing especially on the pharmaceutical-analytical practice. The...
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HPLC in quality control of food supplements based on goldenrod and containing rutin and chlorogenic acid
Kotyková, Klára ; Šatínský, Dalibor (advisor) ; Chocholoušová Havlíková, Lucie (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Klára Kotyková Supervisor: prof. RNDr. Dalibor Šatínský, Ph.D. Title of the diploma thesis: HPLC in quality control of food supplements based on goldenrod and containing rutin and chlorogenic acid In this diploma thesis, a high-performance liquid chromatography (HPLC) method was developed and validated for the separation and determination of chlorogenic acid, 3,5- dicaffeoylquinic acid, rutin, quercetin, and kaempferol. This method was applied to the analysis of food supplements based on goldenrod: drops Celík zlatobýl (Valdemar Grešík), Celík obecný BIO (Bylinné kapky), Celík obecný (Bylinné kapky), Zlatobýl (Green Idea), Zlatobýl - tinktura z pupenů (Serafin), Zlatobýl - tinktura z bylin (Serafin), Zlatobýlová směs (Dědek kořenář), Zlatobýl (Inca Botanica), and capsules Celík (Ex Herbis). Furthermore, two food supplements containing rutin (Solgar and Walmark®) and a food supplement Zelená káva (Botanic) containing chlorogenic acid were analyzed. An Ascentis® Express 90 Å AQ-C18 150 × 4.6 mm column with 2.7 µm particles was selected for analysis. A gradient elution with a mobile phase of acetonitrile/0.085% phosphoric acid was used. Detection was performed with a diode array detector at...
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Development of an HPLC method for quality control of food supplements based on valerian extract
Bílková, Veronika ; Šatínský, Dalibor (advisor) ; Sklenářová, Hana (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Veronika Bílková Supervisor: prof. RNDr. Dalibor Šatínský, Ph.D. Title of the diploma thesis: Development of a HPLC method for quality control of food supplements based on valerian extract In this diploma thesis, a new chromatography method for separation and determination of apigenin-7-glucoside, luteolin, acetoxyvalerenic acid, hydroxyvalerenic acid, valerenic acid, acevaltrate, and valepotriate in valerian extract was developed and validated. The chromatography method was subsequently used to determine the content of the active substances in food supplements: Advance Calmin, Allnature Kozlík bylinný extrakt, Anxiolan from Green-Swan Pharmaceuticals CR a.s., Barnys HypnoX forte from Biopol GN, Dr. Max Happy Sleep, Epiderma Spi v klidu, Kneipp Kozlík plus, NatureVia Sleepnox forte, Naturvita Antistres, Neospan forte od Simply You Pharmaceuticals a.s. and Terezia Spánek & Relax. To compare the content of substances, registered medicinal products were analyzed: Kneipp Kozlík 500 mg, Persen forte - Zentiva Group, a.s.. The method was also applied for quality control of liquid medicinal forms (drops, tinctures): Dr. Popov Kozlík lékařský, Green idea Kozlík lékařský extrakt and Tinctura valerianae...
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Determination of contaminants using online hyphenation of extraction and liquid chromatography via column-switching system
Čeřovský, Tadeáš ; Lhotská, Ivona (advisor) ; Šatínský, Dalibor (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Tadeáš Čeřovský Supervisor: PharmDr. Ivona Lhotská, Ph.D. Title of the diploma thesis: Determination of contaminants using online hyphenation of extraction and liquid chromatography via column-switching system This diploma thesis is focused on testing new types of nanofibers as sorbents for extraction and their online connection with liquid chromatography using a column- switching system. In this work, polyamide nanofibers (PA) were tested, including types PA 6, PA 11, PA 4/6, PA 6/12, and PA 6(3)T. PA 4/6 nanofibers, which exhibited the best extraction properties, were applied for a method optimization using the online connection of extraction and liquid chromatography via a column-switching system for the determination of contaminants in natural waters. During the method optimization, a suitable analytical column was selected. Furthermore, optimal gradient elution was determined experimentally, and the process of packing the extraction column, manually filled with polyamide nanofibers, was optimized. Parameters such as duration of washing, valve switching time, and sample volume were also optimized. Detection was carried out using a DAD detector at a wavelength of 220 nm. The result of the work...
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Chiral separations of borane cluster compounds.
Horáček, Ondřej ; Kučera, Radim (advisor) ; Šatínský, Dalibor (referee) ; Bednář, Petr (referee)
Univerzita Karlova, Farmaceutická fakulta v Hradci Králové Katedra farmaceutické chemie a farmaceutické analýzy Kandidát: Mgr. Ondřej Horáček Školitel: doc. PharmDr. Radim Kučera, Ph.D. Název: Chirální separace klastrových sloučenin boru Anorganické trojrozměrné klastrové sloučeniny boru se staly předmětem zájmu vědců zejména díky svým zajímavým vlastnostem, např. výjimečné tepelné, biologické a chemické stabilitě, neobvyklé třístředodové dvouelektronové vazbě a trojrozměrné aromaticitě. Podtřídou boranových klastrů jsou karborany, které mají v kleci inkorporován alespoň jeden atom uhlíku, čímž kombinují vlastnosti anorganických a organických látek v jedné molekule. Atom uhlíku umožňuje modifikaci klastru různými organickými substituenty, což vede k existenci nepřeberného množství derivátů. Z tisíců těchto sloučenin byly důkladně zkoumány deriváty aniontového bis(dikarbolidu) kobaltu ([Co(C2B9H11)2]- ), a to zejména ve farmaceutické chemii, chemii materiálů, elektrochemii a analytické chemii. Zvýšený zájem o [Co(C2B9H11)2]- je obvykle vysvětlován jeho rozpustností ve vodě, chemickou a biologickou stabilitou, nízkou toxicitou, skrytým amfifilním charakterem a podobností s chemií ferrocenu. Mnoho derivátů [Co(C2B9H11)2]- uvedených v literatuře je chirálních. Navzdory jejich potenciálnímu využití ve...
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Modern extraction techniques in connection with HPLC for analysis of contaminants
Kholová, Aneta ; Šatínský, Dalibor (advisor) ; Ventura, Karel (referee) ; Malíř, František (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Training Workplace Department of Analytical Chemistry Doctoral Degree Program Bioanalytical Methods Candidate Mgr. Kholová Aneta Supervisor prof. RNDr. Dalibor Šatínský, Ph.D. Advisor PharmDr. Ivona Lhotská, Ph.D. Title of Doctoral Thesis Modern extraction techniques in connection with HPLC for analysis of contaminants A compilation of six publications is presented in this dissertation thesis. The work focuses on applying and comparing extraction sorbents to analyze contaminating substances in food and food supplements. The main aim of this thesis was to present micro and nanofibers as suitable extraction sorbents for use in analytical chemistry. For this purpose, the fibers were compared with other, mostly commercial, extraction sorbents suitable for the type of matrix tested. All experiments were carried out in the on-line connection of the extraction sorbent through the selection valve with the analytical column in the chromatographic system. A crucial part was also the use of the extraction properties of nanofibers for the analysis of real-life samples. In the first part, the extraction efficiency was studied on liquid matrices, where no need for complex matrix purification was required. The main aim was sufficient retention and...
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Quality control of food supplements with melatonine using separation methods
Chalupníková, Natálie ; Šatínský, Dalibor (advisor) ; Lhotská, Ivona (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Natálie Chalupníková Supervisor: prof. RNDr. Dalibor Šatínský, Ph.D. Title of the diploma thesis: Quality control of food supplements with melatonine using separation methods In this diploma thesis, an HPLC method was developed and validated for the simultaneous determination of melatonin and pyridoxine. The developed method was applied to the determination in food supplements, Tozax Sleep Trip (mcePharma s. r. o.), Clinical Melatonin B6 syrup (Clinical nutricosmetics s. r. o.), Fast Sleep oral spray with melatonin (EmergoPharm Sp. z o. o. Sp. K.), Melatonin Rapid complex 5 mg ODT (Salutem Pharma s. r. o.), Allegra Melatonin 3 mg (Woykoff a. s.), Clinical Melatonin Forte (Clinical nutricosmetics s. r. o.), Melatonin 2 mg (Allnature s. r. o.), Melatonin new extra 5 mg (Nutricius s. r. o.), Clinical Melatonin B6 Gummies (Clinical nutricosmetics s. r. o.). The method was based on the use of a SUPELCO Ascentis Express C-18 chromatography column (100*4.6 mm, particle size 2.7 µm). The separation was carried out under gradient elution, using a mobile phase of acetonitrile and 0.085% phosphoric acid at pH 2.2, flow rate 1 ml/min and constant temperature 30řC. A detection wavelength of 278 nm was chosen...
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Advanced extraction materials for sample preparation in chromatographic analysis
Zatrochová, Slavomíra ; Šatínský, Dalibor (advisor) ; Solich, Petr (referee) ; Ševčík, Juraj (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Training Workplace Department of Analytical Chemistry Doctoral Degree Program Pharmaceutical Analysis Candidate Mgr. Slavomíra Zatrochová Supervisor Prof. RNDr. Dalibor Šatínský, Ph.D. Advisor PharmDr. Ivona Lhotská, Ph.D. Title of Doctoral Thesis Advanced extraction materials for sample preparation in chromatographic analysis The submitted dissertation presents an annotated set of publications focusing on advanced extraction materials in analytical chemistry and their prospective use as sorbents in sample preparation prior to HPLC analysis. The work was created based on the cooperation with the Technical University of Liberec and the University of Valencia in Spain. In the first part, a new sorbent based on a hybrid monolith with a metal-organic framework (MOF) was developed for conventional Teflon-coated magnetic stir bars, and the resulting hybrid monolith was evaluated as a stir bar sorptive extraction (SBSE) sorbent for the extraction of estrogens in water and urine samples. In the second part, the work was focused on nanofibrous and microfibrous polymers and the production of fibers by alternating current (AC) electrospinning. The extraction efficiency, selectivity and stability of different polymer nanofibers were tested. The...
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