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Studying the distribution of substituents in derivatives based on hyaluronane
Sedláček, Jakub ; Šatínský, Dalibor (advisor) ; Zimčík, Petr (referee) ; Chmelař, Josef (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate Ing. Jakub Sedláček Supervisor doc. RNDr. Dalibor Šatínský, Ph.D. Title of Doctoral Thesis Studying the distribution of substituents in derivatives based on hyaluronan Derivatives based on hyaluronan have found applications in various areas of medicine. Prepared derivatives are commonly characterized by their molar mass and their degree of substitution, however, such parameters are unable to distinguish among derivatives with different distributions of substituents along the chain, which may exhibit different macroscopic properties. For this reason, methods to determine the distribution of substituents along the chain are needed. The presented thesis deals with the determination of distribution of amino groups in deacetylated hyaluronan. The theoretical part starts with a description of hyaluronan structure and of its derivatives. Next, the application, the preparation, and the characterization of deacetylated hyaluronan are discussed, focusing particularly on its depolymerisation into oligosaccharides using deaminative cleavage or enzymes that degrade hyaluronan. Finally, examples of liquid chromatographic methods used to analyse hyaluronan oligosaccharide are presented. The experimental part...
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Monitoring the profile of phenolic substances in different parts of apple trees by HPLC
Šilhavá, Kristýna ; Šatínský, Dalibor (advisor) ; Sklenářová, Hana (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Bc. Kristýna Šilhavá Supervisor: doc. RNDr. Dalibor Šatínský, Ph.D. Consultant: Mgr. Anežka Adamcová Title of Diploma Thesis: Monitoring the profile of phenolic substances in different parts of apple trees by HPLC This diploma thesis covers the performance of a quantitative analysis of phenolic compounds in ten different cultivars in Malus. Specifically, the presence of phloridzin, phloretin, rutin, quercitrin and chlorogenic acid was monitored. Extracts of buds, flowers, leaves and bark in each species were analyzed during the four different vegetation periods. Further, the presence of phenolic compounds in samples of wood chips and fruits was monitored. The determined analytes displayed a different content profile depending on the plant material, apple cultivar and the period in which they were collected. Except for fruits, phloridzin was the dominant component in all varieties and in all materials. The highest total concentration of phenolic compounds was found in the leaves in the spring March-April 2020 in species 'Rubinstep'. This diploma thesis used a developed and validated HPLC-DAD method for a large number of extracts. A YMC-Triart C18 ExRS column (150 × 4.6 mm × 5 µm, 8 nm) was chosen...
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Optimization of the screening strategy for the detection of so-called new drugs of the synthetic cannabinoid group
Ozsvaldová, Silvia ; Šatínský, Dalibor (advisor) ; Plachká, Kateřina (referee)
Charles University Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Bc. Silvia Ozsvaldová Supervisor: prof. RNDr. Dalibor Šatínský Ph.D. Consultant: PharmDr. Viktor Voříšek Titel of diploma thesis: Optimization of the screening strategy for the detection of so-called new drugs of the synthetic cannabinoid group Our diploma thesis pursues the main aim of optimizing the screening strategy of the capture of synthetic cannabinoids. In the theoretical part, we described the history of synthetic cannabinoids, their classification, and their effects on human health status. Next, we describe the determination, using the ultra-high liquid chromatography joined with mass spectrometry, which uses the principle of OrbitrapTM as a mass analyzer. We performed on our spiked sample of the JWH-018 N-(4-hydroxypentyl) on three different columns in the experimental part. There were Phenyl Hexyl Kinetex®, Luna Omega® Polar C18 and Arion® Polar C18 UHPLC columns. Also, we performed specific PRM scans on Luna and Arion columns. Samples on all three columns were measured in triplets, in duplicate during the PRM. We constructed calibration dependences, based on acquired values from which the parameters LOD and LOQ were calculated. Subsequently, we present these analytical control quality...
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Optimization of conditions for qualitative and quantitative analysis of farnesol and tyrosol using UPLC-MS/MS.
Greguš, Petr ; Nováková, Lucie (advisor) ; Šatínský, Dalibor (referee)
Direct activation of C-H bond in tetrazoles Richard Lubojacký, 5th grade Supervisor: Prof. RNDr. Milan Pour, Ph.D. Department of Inorganic and Organic Chemistry, Faculty of Pharmacy in Hradec Králové Within the framework of this diploma thesis, direct arylation and alkenylation of 1- substituted tetrazoles at C5 was developed and optimized. An economical preparation of a range of 1,5-disubstituted tetrazoles was thus made possible. In these reactions, Pd-catalysis in the presence of CuI and Cs2CO3 was found as optimal. Contrary to similar reactions of imidazoles and purines, it was necessary to incorporate phosphine ligands in order to stabilize Pd - intermediates and prevent them from a premature decomposition into cyanamides. A library of 1,5-disubstituted tetrazoles with very promising yields has been prepared using this method.
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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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Two dimensionalk separations in Sequential Injection Chromatography low pressure system
Válová, Olga ; Šatínský, Dalibor (advisor) ; Chocholouš, Petr (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Biochemical Sciences Candidate: Bc. Olga Válová Supervisor: Doc. RNDr. Dalibor Šatínský, Ph.D. Title of diploma thesis: Two Dimensional Separation in the Low Pressure System of Sequential Injection Chromatography The subject of this work was to construct a new method for separation of two analytes, which are different in their chemical properties and lipophilicity. Newly described method named Two Dimensional Sequential Injection Chromatography (2D-SIC) for isocratic system was applied in this work for the analysis of pharmaceutical preparation Otobacid N, which contains active substances Dexamethasone and Cinchocaine, i.e. substances with different chemical properties. The separation was carried out in two dimensions of two columns. In the first dimension for separation of Dexamethasone was used column 25 x 4.6 mm C-18 monolithic column with mobile phase acetonitrile/water in ratio of 35/65, flow rate 15 µl/sec. In the second dimension for separation of Cinchocaine was used column 10 x 4.6 mm C-18 monolithic column with precolumn 5 x 4.6 mm C-18 with mobile phase acetonitrile/water in ratio 60/40, flow rate 15 µl/sec. Optimal wavelength at 240 nm was chosen by spectrophotometric detection. Relative standard deviation...
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Evaluation of properties of new HILIC stationary phases for pteridins using UHPLC-FD method
Kaufmannová, Iva ; Nováková, Lucie (advisor) ; Šatínský, Dalibor (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of analytical chemistry Candidate: Iva Kaufmannová Supervisor: PharmDr. Lucie Nováková, Ph.D. Title of Doctoral Thesis: Evaluation of properties of new HILIC stationary phases for pteridins using UHPLC-FD method The subject of this thesis was to evaluate the characteristics of three new types of HILIC stationary phases for the identification and quantification of biologically active substances biopterin, neopterin, dihydrobiopterin and dihydroneopterin by UHPLC with fluorescence detection. Neopterin is used as a marker of immune system activation and inflammatory diseases. Its early detection in urine or plasma may indicate a pathological immune activity. Elevated concentration of neopterin is described in viral or bacterial diseases, in autoimmune diseases in HIV infection or in malignant tumors. 7,8 - dihydroneopterin is able to prevent proteins and lipoproteins from oxidative damage. Hydrophilic Interaction Liquid Chromatography (HILIC) is a chromatographic method that can be used to improve retention of very polar compounds. It uses a polar stationary phase and mobile phase containing a certain amount of water and polar solvents. UHPLC is the most advanced separation technology to develop a pressure of about 100 MPa....
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Using of HPLC for illegal colorants determination in food
Šmidrkalová, Tereza ; Šatínský, Dalibor (advisor) ; Sklenářová, Hana (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Tereza Šmidrkalová Supervisor: Doc. RNDr. Dalibor Šatínský, Ph.D. Title of Diploma Thesis: Using of HPLC for illegal colorants determination in foods. This thesis deal with looking for optimal conditions for determination of Sudan dyes. High performance liquid chromatography (HPLC) was used for determination. During searching several various columns and mobile phases were tested. For validation of separation conditions Ascentis Express F5 column (100 x 4,6 mm, 2,7 μm) was used. Detection was measured at a wavelength of 500 nm and 426 nm. Separation used gradient elution with mobile phase of acetonitrile - water at a flow rate 1 ml/min. Injection volume was set to 5 μl. During measuring validation parametres was used on-line SPE extraction in HPLC system on precolumn Ascentis Express C18 (5 x 4,6 mm, 2,7 μm) with washing mobile phase 5% solution of acetonitril - water before separation. Optimalization and validation used only standards and method was suggested for other testing and using real samples. Keywords: high performance liquid chromatography (HPLC), Sudan dyes
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