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Development of LC-MS method for the study of topotecan
Mudrová, Barbora ; Širc, Jakub (advisor) ; Kozlík, Petr (referee)
4 Abstract Topotecan (TPT) is a chemotherapeutic agent used to treat retinoblastoma, the most common malignant primary intraocular tumor in children. This drug undergoes a pH-dependent hydrolysis of the lactone ring creating an open-ring carboxylate form, while only the lactone form exhibits an antitumor activity. For clinical studies, it would be useful to develop a highly sensitive analytical method to monitor the concentration of both forms of TPT. In this thesis, the method of determination of the TPT forms by liquid chromatography with fluorescence or tandem mass detection were investigated. A rapid, selective and highly sensitive ultra-high performance liquid chromatography (UHPLC-MS/MS) method was developed for the determination of both forms of TPT in water, porcine plasma and vitreous humor. The separation was performed at 15 řC on a Waters Acquity-UPLC BEH C18 column (2.1 mm × 50 mm, particle size 1.7 µm) with a linear gradient elution. The method showed an excellent linear range of 0.4-120 ng/ml for TPT lactone and 0.8-120 ng/ml for TPT carboxylate in blood plasma and vitreous. In water, the linear range was 0.5-100 ng/ml for the lactone form of TPT and 1.0-100 ng/ml for TPT carboxylate. The effect of pH of TPT aqueous sample and the pH of the aqueous component of the mobile phase on the change...
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Morphological characterization of monolithic columns
Širc, Jakub
1 High performance liquid chromatography (HPLC) is currently one of the most widely used analytical separation techniques. Although the most of applications use standard chromatographic columns packed with particles, these stationary phases has some disadvantages and limits. A promising alternative are monolithic columns. In contrast to the packed stationary phase consisting of many particles, monoliths are composed of one block of porous material. Monoliths are characteristic with communitating macropores, instead of the interparticle spaces of packed columns, which allow the flow of mobile phase carrying the analyte molecules, and small mesopores providing sufficient surface for active sites of stationary phase. The character of the porous structure of the monolith, its specific surface area, quantity, size and shape of pores significantly affect the properties of monolithic columns. The aim of this thesis is to manage the preparation of monolithic chromatographic columns by in situ polymerization within the columns and a description of factors influencing the morphology of the resulting monoliths. Second part of the work is focused on the characterization of the morphology of prepared monoliths, which is essential for the understanding of chromatographic processes that run through them. Describe the...
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Morphological characterization of monolithic columns
Širc, Jakub
1 High performance liquid chromatography (HPLC) is currently one of the most widely used analytical separation techniques. Although the most of applications use standard chromatographic columns packed with particles, these stationary phases has some disadvantages and limits. A promising alternative are monolithic columns. In contrast to the packed stationary phase consisting of many particles, monoliths are composed of one block of porous material. Monoliths are characteristic with communitating macropores, instead of the interparticle spaces of packed columns, which allow the flow of mobile phase carrying the analyte molecules, and small mesopores providing sufficient surface for active sites of stationary phase. The character of the porous structure of the monolith, its specific surface area, quantity, size and shape of pores significantly affect the properties of monolithic columns. The aim of this thesis is to manage the preparation of monolithic chromatographic columns by in situ polymerization within the columns and a description of factors influencing the morphology of the resulting monoliths. Second part of the work is focused on the characterization of the morphology of prepared monoliths, which is essential for the understanding of chromatographic processes that run through them. Describe the...
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Morphological characterization of monolithic columns
Širc, Jakub ; Bosáková, Zuzana (advisor) ; Feltl, Ladislav (referee) ; Vacík, Jiří (referee)
I ntroduction Iligh-perfbnnance liquid chromatography (lIPLC) is currently one of the ntost common anal1'tica| soparation 1cclrtlic1ttcs' Duc to its ability to separate a widc range oÍ'a structurally rlil.Íěrent lorr- and high ntolecular oompourtds o1'polar as rvcll as non-polar nature, tIPLC found application in analylical laboratories in thc field ofrnedicine. plrarrrracy. biology. industry and the environmelt. Although the oonverttional packed colunrns are used in most of ths chronratographic applications, stationary phases in the Íbrnr of.particles have their limitations and disadvňtages. Quality o| the packed colutltns is irrÍluerrced by a rrunrber ol. paranreters' |or exanrple relatiňly conrplicated process ol.lilling I l |' Variances in the particle size and inegularities in their shape have á n!'galive inrpact on thc chrotratoBraphic process. Conrmon problems of the packed oolunrns are an inhomogeucous distribution ol the particles ol'various sizes and their settling in the column u,ith consequent greation of dcad voIuntes' FIighly uniÍbm spherical partic|es prcpared by suspension polynrerization can partlY solve stlnte Iintitations. hor,vever. disadvantagcs arising Íionr the prin|iple of tlrc packcd coluurns still rcntain. Prornising altcmative to thc paoked colunrns are monoliths. made of a block...
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Li+ a H+ vodivé polymerní elektrolyty s kovalentně vázanými anionty
Reiter, Jakub ; Michálek, Jiří ; Přádný, Martin ; Chmelíková, Dana ; Širc, Jakub
New single-ion conducting electrolytes based on methacrylates were prepared using direct, radically initiated polymerisation: copolymers of methacrylic acid (MA) or lithium methacrylate (LiMA) with 2-ethoxyethyl methacrylate (EOEMA) and poly(ethylene glycol) methyl ether methacrylate (EGMEMA) as pure cationically conducting Li+ or H+ electrolytes and covalently bonded carboxylic group. For the conductivity improvement, a set of electrolytes with embedded aprotic solvent (propylene carbonate PC or N,N-dimethylformamide DMF) was prepared.
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