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Multidimensional Liquid Phase Separations
Šesták, Jozef ; Čáslavský, Josef (referee) ; Pulkrabová, Jana (referee) ; Česla, Petr (referee) ; Kahle, Vladislav (advisor)
This dissertation is dedicated to the topic of multidimensional liquid phase separations. This separation techniques are developed for analysis of complex samples containing thermally labile, low volatile or high molecular weight components that can´t be analysed by two-dimensional (2D) gas chromatography. Concepts of peak capacity and orthogonality are explained and various methods of their determination are stated in theoretical part of dissertation. High performance column liquid chromatography (HPLC) and high performance capillary electrophoresis (HPCE) are suggested as the most suitable methods for automated multidimensional liquid phase separations on-line coupled to mass spectrometry. Configuration of simplified miniaturized liquid chromatograph is described in experimental part of this thesis. Original concept of the system has been extended by simple mobile phase gradient generation technique. Correct function was demonstrated on repeatable separation of alkylphenones, peptides, nitroaromatics, and nitroesters. This system has been utilized as a base for a couple of simple two-dimensional separation platforms for HILIC-MALDI-MS analysis of glycans, for separation of peptides based on off-line coupling of isoelectric focusing and capillary liquid chromatography, and finally for on-line IEC×RPLC, RPLC×RPLC, and HILIC×RPLC two-dimensional liquid chromatography. Correct operation of submitted platforms has been proved.
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Aplication of separation methods for determination of biologically active substances
Bílková, Aneta ; Sklenářová, Hana (advisor) ; Česla, Petr (referee) ; Solich, Petr (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: RNDr. Aneta Bílková Supervisor: assoc. prof. PharmDr. Hana Sklenářová, Ph.D. Consultant: assoc. prof. PharmDr. Petr Chocholouš, Ph.D. Title: Application of separation methods for determination of biologically active substances The submitted dissertation thesis presents an annotated set of three publications, focusing on the application of separation methods for the determination of biologically active phenolic substances, pesticide residues in fruits, with regard to the use of modern storage technologies, and the application result - a utility model based again on monitoring the phenolic substances content with respect to different conditions of plant material drying. In the theoretical part, the target analytes are characterized from an analytical point of view, with respect to their physico-chemical properties, stability, antioxidantion activity. It also describes sample preparation methods for the determination of biologically active phenolic substances, selected extraction procedures and an overview of the methods used for the determination of the described substances in plant material. The main part of the dissertation deals with the development, optimization and validation of a rapid...
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Application of nanofibrous sorbents for on-line extraction in liquid chromatography
Háková, Martina ; Šatínský, Dalibor (advisor) ; Česla, Petr (referee) ; Urban, Jiří (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Mgr. Martina Háková Supervisor: doc. RNDr. Dalibor Šatínský, Ph.D. Consultant: doc. PharmDr. Lucie Chocholoušová Havlíková, Ph.D. Title of Doctoral Thesis: Application of nanofibrous sorbents for on-line extraction in liquid chromatography A compilation of ten publications is presented in this dissertation thesis. It is focused on the application of nano and microfibrous polymers as a new extracting material in analytical chemistry. This work was based on close cooperation with the Institute for Nanomaterials, Advanced Technologies and Innovation and the Department of Nonwovens and Nanofibrous Materials at the Technical University of Liberec, where the author took part in designing and preparation of these materials. The first part deals with model studies, based on using polyamide, polystyrene and polycaprolactone nanofibers as sorbents for solid phase extraction in classical off-line mode or in on-line column switching system. It solves practical aspects such as orientation and the formation of the fibers in the extraction system, optimization of fabrication factors affecting applicability of the nanomaterials, suitable solvent systems, stability testing and reusability of the microcolumns. The...
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Application of nanofibrous sorbents for on-line extraction in liquid chromatography
Háková, Martina ; Šatínský, Dalibor (advisor) ; Česla, Petr (referee) ; Urban, Jiří (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Mgr. Martina Háková Supervisor: doc. RNDr. Dalibor Šatínský, Ph.D. Consultant: doc. PharmDr. Lucie Chocholoušová Havlíková, Ph.D. Title of Doctoral Thesis: Application of nanofibrous sorbents for on-line extraction in liquid chromatography A compilation of ten publications is presented in this dissertation thesis. It is focused on the application of nano and microfibrous polymers as a new extracting material in analytical chemistry. This work was based on close cooperation with the Institute for Nanomaterials, Advanced Technologies and Innovation and the Department of Nonwovens and Nanofibrous Materials at the Technical University of Liberec, where the author took part in designing and preparation of these materials. The first part deals with model studies, based on using polyamide, polystyrene and polycaprolactone nanofibers as sorbents for solid phase extraction in classical off-line mode or in on-line column switching system. It solves practical aspects such as orientation and the formation of the fibers in the extraction system, optimization of fabrication factors affecting applicability of the nanomaterials, suitable solvent systems, stability testing and reusability of the microcolumns. The...
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Application of nanofibrous sorbents for on-line extraction in liquid chromatography
Háková, Martina ; Šatínský, Dalibor (advisor) ; Česla, Petr (referee) ; Urban, Jiří (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Mgr. Martina Háková Supervisor: doc. RNDr. Dalibor Šatínský, Ph.D. Consultant: doc. PharmDr. Lucie Chocholoušová Havlíková, Ph.D. Title of Doctoral Thesis: Application of nanofibrous sorbents for on-line extraction in liquid chromatography A compilation of ten publications is presented in this dissertation thesis. It is focused on the application of nano and microfibrous polymers as a new extracting material in analytical chemistry. This work was based on close cooperation with the Institute for Nanomaterials, Advanced Technologies and Innovation and the Department of Nonwovens and Nanofibrous Materials at the Technical University of Liberec, where the author took part in designing and preparation of these materials. The first part deals with model studies, based on using polyamide, polystyrene and polycaprolactone nanofibers as sorbents for solid phase extraction in classical off-line mode or in on-line column switching system. It solves practical aspects such as orientation and the formation of the fibers in the extraction system, optimization of fabrication factors affecting applicability of the nanomaterials, suitable solvent systems, stability testing and reusability of the microcolumns. The...
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Multidimensional Liquid Phase Separations
Šesták, Jozef ; Čáslavský, Josef (referee) ; Pulkrabová, Jana (referee) ; Česla, Petr (referee) ; Kahle, Vladislav (advisor)
This dissertation is dedicated to the topic of multidimensional liquid phase separations. This separation techniques are developed for analysis of complex samples containing thermally labile, low volatile or high molecular weight components that can´t be analysed by two-dimensional (2D) gas chromatography. Concepts of peak capacity and orthogonality are explained and various methods of their determination are stated in theoretical part of dissertation. High performance column liquid chromatography (HPLC) and high performance capillary electrophoresis (HPCE) are suggested as the most suitable methods for automated multidimensional liquid phase separations on-line coupled to mass spectrometry. Configuration of simplified miniaturized liquid chromatograph is described in experimental part of this thesis. Original concept of the system has been extended by simple mobile phase gradient generation technique. Correct function was demonstrated on repeatable separation of alkylphenones, peptides, nitroaromatics, and nitroesters. This system has been utilized as a base for a couple of simple two-dimensional separation platforms for HILIC-MALDI-MS analysis of glycans, for separation of peptides based on off-line coupling of isoelectric focusing and capillary liquid chromatography, and finally for on-line IEC×RPLC, RPLC×RPLC, and HILIC×RPLC two-dimensional liquid chromatography. Correct operation of submitted platforms has been proved.
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