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HPLC Method for Determination of Lamotrigine and Related Substances in Tablets
Foltinská, Blanka ; Kastner, Petr (advisor) ; Sochor, Jaroslav (referee)
HPLC method for determination of lamotrigine and related substances in tablets Rigorous thesis Mgr. Blanka Foltinská Charles University in Prague, Faculty of Pharmacy in Hradec Králové, Department of Pharmaceutical Chemistry and Drug Control The method for determination of purity and stability of lamotrigine was optimized. Lamotrigine was exposed to such conditions to reach its degradation into degradation products which are also possible impurities of lamotrigine. Several chromatography columns were tested and the composition of mobile phase was optimized. Chromatography column Waters Spherisorb 5 µm Phenyl, 4,6 x 250mm was chosen and mobile phase containing acetonitril : phosphate buffer ( 1,4 g K2HPO4 /l) 35:65, final pH of the mobile phase was adjusted to 6.0 by orthophosphoric acid. Flow rate was 1 ml/min, injected volume 20 µl, column temperature 25žC and UV detection at 309 nm. Linearity of this method was tested under these conditions. This method was worked up to enable its using in determination of content of lamotrigine and related substances in tablets containing lamotrigine. Validation parameters of this method were tested.
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The development of the new type of simple, middle accurate approximations of caloric functions of state of wet steam
Bayer, Zdeněk
The study presents the continuation of the new method of analysis of ideal thermal cycles of the piston combustion engines. The method is based on the following principles: i) use of the temperature ratio of the cycle as the basic thermodynamic parameter, ii) use of the specific performance as an additional criterion (besides the thermal efficiency), and iii) the complex thermodynamic optimization of the cycle. These principles are used to perform the analysis of the cycle in the off-design regimes and the derivation of the most important thermodynamic formulae for the ideal thermal cycle of supercharged engines.
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Determination of septonex in pharmaceutical preparations by capillary zone electrophoresis with conductivity detection.
Šindelková, Martina ; Polášek, Miroslav (advisor) ; Pospíšilová, Marie (referee)
DETERMINATION OF SEPTONEX IN PHARMACEUTICAL PREPARATIONS USING CAPILLARY ZONE ELECTROPHORESIS WITH CONTACTLESS CONDUCTIVITY DETECTION A new method of capillary zone electrophoresis with contactless conductivity detection for the determination of septonex in pharmaceutical preparations was devised. Optimal conditions for the separation and determination of septonex were: background electrolyte 30mM MES of pH 7.0 (adjusted with 20mM TRIS) containing 12.5mg/ml of (2- hydroxypropyl)-β-cyclodextrin, voltage 25kV, temperature 25řC and sample injection for 15 seconds under the pressure of 50mbar. N,N-dimethylethanolamine (200µg/ml) was used as internal standard. The peak of septonex was satisfactorily separated from the peak of internal standard as well as from the EOF. The analysis was carried out in a fused-silica capillary (internal diameter 50μm, total length 75cm and the length to the detector 45cm). The separation took less than 4 minutes and the overall analysis time involving appropriate rinsing of the capillary was less than 16 minutes. The calibration curve was linear in the range 75µg/ml - 300µg/ml of septonex, correlation coefficient r = 0.9976. The LOD was 9μg/ml and LOQ was 30μg/ml of septonex. Unsuitable repeatability of peak areas of septonex (caused probably by insufficient elimination of...
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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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Determination of the Biologically Active Substances using Liquid Chromatography XIV
Fišerová, Veronika ; Pilařová, Pavla (advisor) ; Kastner, Petr (referee)
The Determination of the Biologically Active Substances using Liquid Chromatography XIV Thesis Veronika Fišerová Charles University Prague Faculty of Pharmacy Hradec Králové Department of Pharmaceutical Chemistry and Drug Control A method has been developed for the determination of the aciclovir by UHPLC in a pharmaceutical preparation containing 5 % of aciclovir with regard to the separation of a related substance, guanine. By using the UHPLC method the time of analysis was shortened. A Thermo Scientific 1,7 µm C18 100A, 100 × 3 mm column was used. A mixture of 90% acetonitrile and a buffer with a pH of 5,5 was chosen as the mobile phase and the analysis was performed by gradient elution. The flow rate of the mobile phase was set at 0,5 ml/min and the column temperature was 40 řC. Detection was carried out at a wavelength of 245 nm. Keywords: UHPLC, aciclovir
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Metody frakcionace a obohacování rostlinného proteomu
Breineková, Alžběta
The proteome is a complex and dynamic mixture of proteins produced by an organism. It represents tens of thousands different protein species and its characterization is a difficult task even with state-of-the-art techniques. This thesis entitled "Methods for plant proteome fractionation and enrichment" is focused on plant proteomics and approaches that can improve detection limits and increase proteome coverage. In the experimental part, model plant Arabidopsis thaliana proteome was analysed. The tested techniques include crude fractionations on the tissue level, a subcellular fractionation, and separations on the protein level. Finally, sets of samples were analysed via LC-MS and the method for peptide analysis was optimized. Combining the LC-MS datasets revealed more than 4900 identified Arabidopsis proteins (FDR<1%). Of these, 248 were detected only in equalized proteome. The results of this work helped to establish a robust proteome analysis workflow that will be implemented in plant proteome research at MENDELU.
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Detekční systémy pro měření vyzařování vysokoteplotního plazmatu tokamaku COMPASS na bázi rychlých bolometrů a měkkých rentgenových detektorů
Vácha, Miroslav ; Weinzettl, Vladimír (advisor) ; Piffl, Vojtěch (referee)
Title: Detection systems for measurements of high-temperature plasma radiation on the COMPASS tokamak by fast bolometers and soft X-ray detectors Author: Miroslav Vácha Department: Institute of Particle and Nuclear Physics Supervisor: Mgr. Vladimír Weinzettl, Ph.D., Institute of Plasma Physics AS CR, v.v.i. Supervisor's e-mail address: vwei@ipp.cas.cz Abstract: Multi-channel spectroscopic diagnostics on the COMPASS tokamak com- prising AXUV-based bolometers, soft X-ray (SXR) and visible light detectors will cover a wide spectral range of the core and edge plasma emission, aiming to realize a fast tomography at microsecond time scales. This thesis reports on a development of the bolometric and SXR diagnostics. First, procedures of the detector selection and their tests are described. There the design and tests of the special complex port plug, com- bining both detection systems, taken into account a strongly limited available space, a heat protection and a shielding during a cleaning glow discharge, is also summarized. Development of new electronic amplifiers and their connection with the data acquisition system is documented. In the last chapters, basic methods for analysis of data collected using these diagnostic systems are introduced. Keywords: tokamak, plasma radiation, photodiode, tomography
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Modification of dietary habits and physical activity and its effect on the density of bone tissue of a middle-aged female
JAROŠOVÁ, Veronika
The aim of this thesis is to find out about the effect which have modification of dietary habits and physical activity on the density of bone tissue of a middle-aged female. Intervention programme was prepared for middle-aged female in the length od six months. Intervention programme included modification of dietary habits which meant that the amount of calcium was increased. Programme also included modification of physical aktivity. Training programme was dividend into two parts. There were aerobic physical activities and special work out. Study started in August 2011 and it was finished in February 2012. DXA examination was done to detect bone density. There were two areas to examine - L1-L4 and proximal femur (Neck, Troch, Inter, Ward´s). Apart from bone density, there was also body composition examination. Fat mass, lean mass and total body fat were detected. DXA results from medical examinations for the areas are evaluated in the practical part.
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Development and validation of HPLC method for determination of retinyl esters in human serum using monolithic columns.
Krčmová, Lenka ; Solich, Petr (advisor) ; Šatínský, Dalibor (referee)
DEVELOPMENT AND VALIDATION OF HPLC METHOD FOR DETERMINATION OF RETINYL ESTERS IN HUMAN SERUM USING MONOLITHIC COLUMN Absorption test of vitamin A is used for monitoring of intestinal permeability and may represent a sensitive indicator of intestinal damage. In this study, a simple and rapid reversed- phase high-performance liquid chromatography (RP-HPLC) procedure for selective and sensitive determination of retinol, -tocopherol, retinyl-palmitate and retinyl-stearate in blood serum has been developed and used for the monitoring of intestinal mucosal damage in cancer patients treated with cytotoxic drugs after absorption test of vitamin A. The HPLC instrumentation Series 200 LC from Perkin Elmer (Norwalk, USA) with diode- array detector (DAD) was used for the analysis. Separation of retinol, -tocopherol, retinyl- palmitate and retinyl-stearate were performed using the monolithic column Chromolith Performance RP-18e, 100 x 4.6 mm (Merck, Darmstadt, Germany). The gradient elution was used at the flow rate 3 ml min-1 ; mobile phase methanol:water (95:5) in 0-2.1 min and methanol:2-propanol (60:40) in 2.1-4.9 min. The total time of analysis was 6 min. The injection volume of sample was 20 μl and analysis was done at ambient temperature. The detection of retinol, -tocopherol and retinyl esters was carried out...
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Formation of RONS in cold air plasma activazed water and their effects on cell membranes of Escherichia coli
Tarabová, B. ; Machala, Z. ; Doležalová, Eva ; Lukeš, Petr
In this work, we focused on the detection of secondary reactive oxygen and nitrogen species (RONS) formed by cold plasma induced gas-liquid chemistry in air discharge activated water and liquids. Plasma induced chemical changes in plasma activated water (PAW) were correlated with the antibacterial effect, sublethal injury of bacterial cells and peroxidation of membrane lipids. The contribution of the electric field induced by the plasma treatment was evaluated by the detection of membrane permeabilization. The bactericidal effects of direct (plasma and PAW) and indirect (only PAW) treatments were compared with long-term preservation of the PAW with its antibacterial properties
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