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"The optimalization and validation of LC/MS method for the determination of selected diureticsin human blood serum"Optimization and validation of LC/MS method for quantitative determination of diuretics in human blood serum
Světlíková, Zuzana ; Nobilis, Milan (advisor) ; Kovaříková, Petra (referee)
A new method was developed and fully validated for the quantification of hydrochlorothoazide and chlorthalidone, both diuretic and anti-hypertensive agents, in human serum. This liquid chromatography-tandem mass spectrometry method (LC/MS/MS) is rapid, simple, accurate and selective. The analytes and the internal standard were extracted by liquid-liquid extraction (LLE) with ethylacetate-dichlormethane (80:20, v/v). The chromatographic separation was performed on a reversed-phase column C8 with a mobile phase acetonitrile-formic acid (0,2 %), the elution was gradient. The analytes were quantitated by linear ion trap mass spectrometry with an electrospray ionization interface (ESI). The diuretics were analysed in negative ion monitoring mode, the internal standard in positive ion monitoring mode. The assay exhibited a linear dynamic range of 0,5-200 ng/mL for hydrochlorothiazide and 0,5-500 ng/mL for chlorthalidone in human serum. Acceptable precision and accuracy were obtained for QC samples with concentration over the standard curve ranges. This developed and validated method has been used in the toxicological laboratory in the Institution of Clinical Biochemistry and Diagnosis in Hradec Králové.
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The employment of HPLC in the field of drug analysis IV.
Krejčí, Tereza ; Kučera, Radim (advisor) ; Kovaříková, Petra (referee)
Employment of HPLC in the field of drug analysis IV. Diploma thesis Tereza Krejčí Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control Heyrovského 1203, Hradec Králové. The diploma thesis is targeted to usage of High Performance Liquid Chromatography in the field of Quality control of drug substances. Methylergometrine is a derivative of ergometrine that belongs to Ergot alkaloids. These native origin substances have strong pharmacological effects on different human body systems already in low concentrations. Active components from ergot are acquired by extraction and subsequent separation of individual components from a mixture. These substances are repurified. It is very expensive to produce totally pure substances and thus final substances may contain defined amount of impurities. In case of methylergometrine Related substances are analysed according to the valid European pharmacopoeia. Nine substances are in the specification of possible analysed components, tenth component (-)methylergometrinine has not been described in the pharmacopoeia so far. This thesis deals with development of chromatographic conditions for qualitative separation of a mixture of methylergometrine and its impurities on zirconia based stationary...
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HPLC analysis of drugs and drug candidates in biological material
Luňáková, Veronika ; Kovaříková, Petra (advisor) ; Mokrý, Milan (referee)
High-performance liquid chromatography (HPLC) is currently one of the most progressive separation methods, permitting, simultaneously, both quantitative and qualitative analysis. An important area for the utilisation of HPLC is the identification of drugs and their metabolites in biological materials. This study was focused on the development of chromatographic conditions appropriate for HPLC analysis of two new potential drugs derived from aroyl-hydrazone, HNAF-INH and 4,6DAR-INH, in biological material and its subsequent application in the assessment of the stability of these substances in plasma. Analysed chelators were prepared by the modification of the structure of salicylaldehyde isonicotinoyl hydrazone (SIH) with the purpose of improving the stability of the substance in plasma. As a suitable stationary phase the HPLC column LiChroCART® HPLC - cartridge LiChrospher®100 RP - 18e (15μm) with the pre-column LiChroCART® 4-4 Purospher® RP - 18 (5μm) was chosen. The mobile phase in this case represented by a HNAF-INH compound: phosphate buffer (0,01 mol/l aqueous solution of NaH2PO4 · 2 H2O with 2 mmol/l EDTA, pH 3) : methanol, 42:58 (v/v). The temperature in the column was 25řC, the flow rate 1,0 ml/min and UV detection was performed at 288 nm; SIH was used as an internal standard. The mobile...
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Analytical evaluation of drugs and novel drug candidates using HPLC
Kovaříková, Petra ; Klimeš, Jiří (advisor) ; Nobilis, Milan (referee) ; Blešová, Marie (referee)
High performance liquid chromatography (HPLC) is one of the most frequently used analytical techniques for the analysis of drugs. HPLC methods are widely employed in all fields of the modern pharmaceutical analysis - new drugs development, quality control and assurance, the analysis of drugs and metabolites in a biological material (e.g. therapeutic drug monitoring, bioequivalence). The theoretical part of this thesis deals with the main specifics and aspects associated with HPLC analysis of drugs. The experimental part is consisted of six original research papers with appropriate comments divided in to two sections (The analysis of the drug candidates from the group of aroylhydrazone iron chelators and The stability study on selected drugs). The first section concerns with development, validation and application of new HPLC methods in the analysis of drug candidates from the group of iron chelators - pyridoxal isonicotinoyl hydrazone (PIH), salicylaldehyde isonicotinoyl hydrazone (SIH) and pyridoxal 2-chlorobenzoyl hydrazone (o-108). Aroylhydrazone iron chelators are under the investigation as promising drug candidates. Despite these chelators have demonstrated number of interesting pharmacological effects, in fact there were no modern analytical techniques suitable for the analysis of these drug...
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Effect of Expansion of Modern Information Technologies on the Aviation Industry
Kovaříková, Petra ; Vaško, Martin (advisor) ; Valentová, Jana (referee)
This diploma thesis is focused on modern information technologies and its direct effect on the aviation industry. Comparing the state of the industry without technologies and nowadays; describing changes in consumer behaviour as well as in the matter of providing services by companies; pointing out that these changes were caused mainly by growing number of Internet and mobile technologies users all over the world. The last chapter is dedicated to projection of future trends regarding aforementioned area.
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