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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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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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Sequential injection chromatography - advanced separations of bioflavonoids in food supplements
Pavelková, Kristýna ; Chocholouš, Petr (advisor) ; Šatínský, Dalibor (referee)
Charles University in Prague Faculty of Pharmacy in Hradec Králové Department of Analytical chemistry Candidate: Kristýna Pavelková Supervisor: doc. PharmDr. Petr Chocholouš, PhD. Title of diploma thesis: Sequential injection chromatography - advanced separations of bioflavonoids in food supplements Two methods were developed in the thesis. A primary method of sequential injection chromatography with UV detection was developed for separation of bioflavonoids rutin, hesperidin and diosmin. A second method was developed for adjustment data, which enables to increase sensitivity of first developed method. Chromatographic column YMC-Triart C18 ExRS; 100 mm 4.6 mm; 5 μ, 8 nm was used for separation. The mobile phase consisted of a mixture of acetonitrile with phosphoric acid solution pH 2.0 prepared in a ratio of 25:75. Isocratic elution was chosen; flowrate was 10 μl/s and total length of analysis was 7.9 minutes. Sequential injection chromatography system and computer software SIAsoft was used for analysis. Programs Microsoft Excel and Origin Pro 9 were used for processing and adjustment of data. Developed method was not succesfull in quantification of amount of flavonoids in Hemostop Probio MAX. Method for data adjustment enabled significant reduction of LOD and LOQ. Keywords: flavonoids, rutin,...
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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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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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Study of BTEX determination by microextraction in the Lab-in-syringe system coupled with gas chromatography
Kohániová, Andrea ; Horstkotte, Burkhard (advisor) ; Šatínský, Dalibor (referee)
Charles university Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Bc. Andrea Kohániová Supervisor: M.Sc. Burkhard Horstkotte, Ph.D. Co-supervisor: PharmDr. Ivana Horstkotte Šrámková, Ph.D. Title: Study of BTEX determination by microextraction in the Lab-in-syringe system coupled with gas chromatography Benzene, toluene, ethylbenzene and xylenes are one of the major contaminants in the environmental water samples. Because these compounds are consider to be toxic to humans by World Health Organisation, their determination is critically important. The determination of BTEX using gas chromatography with flame ionisation detection combined with direct single drop microextraction using Lab-in-syringe system was studied. The effective paramateres such as microdroplet volume, extraction time, type and use of salt solution and chromatographic parameters were evaluated. The purpose of this work was automation of the entire process using 3D elements in the system.
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