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Analytical and bioanalytical evaluation of drug candidates from the group of aroylhydrazones
Kresová, Jana ; Kovaříková, Petra (advisor) ; Stariat, Ján (referee)
High-performance liquid chromatography (HPLC) is a progressive analytical method used for qualitative and quantitative drug analysis. This work describes various modifications of the chromatographic method for determining of BSIH (isonicotinic acid [2-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)- benzylidene]-hydrazide) and SIH (salicylaldehyde isonicotinoyl hydrazone) in rabbit plasma. BSIH belongs to prochelators which convert to iron chelator SIH in the presence of hydrogen peroxide. Increased stability in plasma and lower toxicity even during repetitive administration is the advantage of BSIH. Separation of BSIH, SIH and internal standard (o-108) was tested on various stationary phases using different chromatographic conditions. However, none of them provided better results than the initial one. Tha analysis was performed on chromatographic column Zorbax Bonus-RP (150 mm x 3,0 mm, particle size 3,5 µm,) with guard column using identical sorbent at a flow rate of 0,3 ml/min. Phosphate buffer (10 mM monosodium phosphate, pH6, adjusted with sodium hydroxide) : acetonitrile with methanol (60:40) (v/v) with the ratio of 60:40 (v/v)) as the mobile phase. Detector response was registered at 297 nm. Linearity of the method was verified in the concentration range of 10 µM to 100 µM for both BSIH and...
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Study on possibility of utilization of alternative sorbents for sample preparation
Kresová, Jana ; Štěrbová, Petra (advisor) ; Kučera, Radim (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Drug Control Candidate Mgr. Jana Kresová Consultant Doc. PharmDr. Petra Kovaříková, Ph.D. Title of Thesis Study on possibility of utilization of alternative sorbents for sample preparation Sample preparation belongs to basic operations during biological sample analysis. Overall success of analytical determination depends on its accomplishment. Nowadays, Solid Phase Extraction (SPE) is positively a dominant technique in the field of biological materials sample preparation. Graphene is one of the new forms of carbonaceous materials. Due to its extraordinary properties (large surface area, structure rich in π-electrons, good thermal and chemical stability) it became a suitable adsorbent in analytic sample preparation. The aim of this work was to evaluate extraction recoveries of several sorbents: ZirChrom® -SHAX (SHAX, polyethyleneimine-coated zirconia), ZirChrom® -SAX (SAX, polyethyleneimine-coated zirconia - less cross-linked than SHAX), ZirChrom® -PEZ (PEZ, ethylendiamine-N,N,N',N'-tetramethylenphosphoric-acid-coated zirconia), aminosilica (AS) both unmodified and graphene-oxide modified followed by thermal reduction. The extraction efficiency was tested using the model mixture containing...
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Analytical and bioanalytical evaluation of drug candidates from the group of aroylhydrazones
Kresová, Jana ; Kovaříková, Petra (advisor) ; Stariat, Ján (referee)
High-performance liquid chromatography (HPLC) is a progressive analytical method used for qualitative and quantitative drug analysis. This work describes various modifications of the chromatographic method for determining of BSIH (isonicotinic acid [2-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)- benzylidene]-hydrazide) and SIH (salicylaldehyde isonicotinoyl hydrazone) in rabbit plasma. BSIH belongs to prochelators which convert to iron chelator SIH in the presence of hydrogen peroxide. Increased stability in plasma and lower toxicity even during repetitive administration is the advantage of BSIH. Separation of BSIH, SIH and internal standard (o-108) was tested on various stationary phases using different chromatographic conditions. However, none of them provided better results than the initial one. Tha analysis was performed on chromatographic column Zorbax Bonus-RP (150 mm x 3,0 mm, particle size 3,5 µm,) with guard column using identical sorbent at a flow rate of 0,3 ml/min. Phosphate buffer (10 mM monosodium phosphate, pH6, adjusted with sodium hydroxide) : acetonitrile with methanol (60:40) (v/v) with the ratio of 60:40 (v/v)) as the mobile phase. Detector response was registered at 297 nm. Linearity of the method was verified in the concentration range of 10 µM to 100 µM for both BSIH and...
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Study on possibility of utilization of alternative sorbents for sample preparation
Kresová, Jana ; Štěrbová, Petra (advisor) ; Kučera, Radim (referee)
Charles University in Prague, Faculty of Pharmacy in Hradec Králové Department of Pharmaceutical Chemistry and Drug Control Candidate Mgr. Jana Kresová Consultant Doc. PharmDr. Petra Kovaříková, Ph.D. Title of Thesis Study on possibility of utilization of alternative sorbents for sample preparation Sample preparation belongs to basic operations during biological sample analysis. Overall success of analytical determination depends on its accomplishment. Nowadays, Solid Phase Extraction (SPE) is positively a dominant technique in the field of biological materials sample preparation. Graphene is one of the new forms of carbonaceous materials. Due to its extraordinary properties (large surface area, structure rich in π-electrons, good thermal and chemical stability) it became a suitable adsorbent in analytic sample preparation. The aim of this work was to evaluate extraction recoveries of several sorbents: ZirChrom® -SHAX (SHAX, polyethyleneimine-coated zirconia), ZirChrom® -SAX (SAX, polyethyleneimine-coated zirconia - less cross-linked than SHAX), ZirChrom® -PEZ (PEZ, ethylendiamine-N,N,N',N'-tetramethylenphosphoric-acid-coated zirconia), aminosilica (AS) both unmodified and graphene-oxide modified followed by thermal reduction. The extraction efficiency was tested using the model mixture containing...
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