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Determination of limiting electrophoretic mobilities of charged cyclodextrins
Boublík, Milan ; Riesová, Martina (advisor) ; Křížek, Tomáš (referee)
In the frame of this work, dependences of electrophoretic mobilities of four defined multiple charged cyclodextrins on ionic strength of background electrolyte were measured using capillary zone electrophoresis. Dependencies of mobility on ionic strength do not follow Onsager law in the case of large and multiple charged species. Therefore, empirical fitting function was used to determine limiting mobilities of studied cyclodextrins. Obtained values of limiting mobilities as well as the resulting regression function are essential for correct determination of complexation constants of corresponding cyclodextrins with various analytes.
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Utilization of statistical approach in development of HPLC methods
Vymyslický, Filip ; Křížek, Tomáš (advisor) ; Kozlík, Petr (referee)
The aim of this diploma thesis was to develop a systematic procedure for the development of HPLC methods using the design of experiments. The system was developed based on the development of three HPLC methods for the determination of the purity of active substances using the design of experiments approach. The HPLC method for determining the purity of esomeprazole was selected to develop the systematic process for the development of HPLC methods by statistical approach. Experimental space was explored to find more suitable separation conditions. The second method used to develop the systematic procedure was the method for determining the purity of bisoprolol. This method was converted to a column of smaller size and the composition of the aqueous part of mobile phase was modified compared with the original pharmacopoeial method. Experimental space was explored to find more suitable separation conditions using the design of experiments. Last the method for determining the purity of risperidone was chosen. The composition of the aqueous part of mobile phase was changed in contrast to the original pharmacopoeial method. Experimental space was explored to find more suitable separation conditions using the design of experiments. For all studied HPLC methods, the values of the monitored chromatographic...
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Analysis of active pharmaceutical ingredient vemurafenib by LC
Filounová, Barbora ; Kozlík, Petr (advisor) ; Křížek, Tomáš (referee)
The aim of this work was to develop and optimize liquid chromatography method with spectrophotometric detection applicable to assay and purity of vemurafenib in solid dosage form and perform its stability study. The optimized separation conditions consisted of Poroshell HPH-C18 (3 × 100 mm, 2.7 μm) column tempered at 30 žC, mobile phase composed of 10 mM ammonium phosphate, pH 3,0/acetonitrile. Flow rate was set at 0.6 mL/min and gradient elution was performed. Detection wavelength was 250 nm. The calibration curve of vemurafenib was constructed in the concentration range 0.4 - 1.2 mg/mL. Limit of detection was 5.0 µg/mL and limit of quantitation was 16.5 µg/mL. Stability and stress tests of vemurafenib were performed under several conditions: Heat (80 žC), heat combined with humidity (80 žC/75 % relative humidity), hydrochloric acid (0,1 M), sodium hydroxide (0,1 M) and hydrogen peroxide (3% and 0,3% solution). The significant degradation of vemurafenib was observed under acid condition. Vemurafenib also degradated under oxidation condition. No degradation was observed under base condition and under heat and heat combined with humidity. Degradation of vemurafenib was not effected by tested excipients. Judging based on experiments vemurafenib is stable from the point of view of chemical stability.
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Case study of physiotherapeutic care for a patient with the diagnosis of 2nd and 3rd degree burns of hands and the head
Purchartová, Dana ; Pánek, David (advisor) ; Křížek, Tomáš (referee)
Title: Case study of physiotherapeutic care for a patient with the diagnosis of 2nd and 3rd degree burns of hands and the head Summary: The aim of this work is to obtain a comprehensive overview of the problems of burns and the medical and rehabilitation process of this diagnosis. The work is divided into a general and special section. The general part includes the anatomy and physiology of skin, the definition and pathology of burns and the possible methods of treatment focusing on the use of physiotherapeutic care. The special section includes the methodology of work and uses a case study to deal with the anamnesis, the input kinesiologic analysis, the course of therapeutic units, the output kinesiologic analysis and the evaluation of the effect of the therapy on the particular patient. Key words: burn, burning, skin, rehabilitation, physiotherapy, case study
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Case study of a patient with the diagnosis of burns II.-III. grade to 40% of body
Šrámková, Šárka ; Vrbová, Martina (advisor) ; Křížek, Tomáš (referee)
Title: Case study of a patient with the diagnosis of burns II.-III. grade to 40% of body Objectives: The main goal of this bachelor thesis is to work out a detailed case study of rehabilitation care of a patient with burns and literature search of this topic. Another goal is to acquire comprehensive teoretic and practical knowledge about this diagnosis. Methods: I used assay and physiotherapeutic approaches which I learned during the bachelor studies at FTVS UK. The general part informs about anatomy and physiology of the skin, about diagnostics of degree and extent of burns, methods of treatment, physical and psychological rehabilitation. Special part includes methodology of the work, anamnesis, opening kinesiologic analysis, individual therapies, outcoming kinesiologic analysis, the effect of the therapy and end. Results: I worked out a detailed case study of a patient with this diagnosis and a literature search has been worked out. The main contribution of the work was the possibility to gain new experiences and knowledge to this diagnosis.
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Development of the electrophoretic method for determination of phosphates and borates in cooling mixtures
Listakhava, Iryna ; Křížek, Tomáš (advisor) ; Kubíčková, Anna (referee)
In this diploma thesis, a method of routine analysis of commercial coolants was developed, focused on the simultaneous determination of inorganic anions - phosphates and borates - as corrosion inhibitors in fresh mixtures and the markers of recycling quality. The method was developed for the instrumental technique of capillary zone electrophoresis with indirect detection at 254 nm. The following were optimized: background electrolyte (its composition, concentration, pH), measured samples (coolant dilution, suitable internal standard) and measurement conditions (capillary length, sample dosing). The influence of the sample matrix on the measurement results, the robustness of the calibration line (or the agreement of the response with the actual analyte concentration) and also the repeatability of the method were tested. Optimizations and tests resulted in a method based on a standard addition with the following parameters: background electrolyte of pH = 11.50 containing sodium chromate at 10 mmol l-1 concentration and CTAB at 1 mmol l-1 concentration; dilution of the coolant sample 20-50×, addition of internal standard MES at 0,1 mmol l-1 concentration, electrokinetic sample injection at -5 kV for 10 s, capillary length 50.0 cm, inner diameter 75 μm. The repeatability of the method expressed as a...
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Analysis of potasium tetrachloroaurate by capillary electrophoresis
Lebertová, Lucie ; Sobotníková, Jana (advisor) ; Křížek, Tomáš (referee)
This bachelor thesis describes the optimalization of condition for the analysis of potassium tetrachloroaurate by capillary zone electrophoresis with spectrophotometric detection. The theoretical part at first introduces the principle of capillary electrophoresis. The following are basic information about gold and its tetrachloroaurate compound. The experimental part at first describes the procedure of optimization the composition of the basic electrolyte and problems with the instability of the base line. As the most suitable conditions for the analysis of tetrachloroaurate, have been chosen the subsequent experimental conditions: fused silica capillary with a total length of 80 cm, effective length 71.6 cm and inner diameter 50 µm; applied separation voltage -20 kV; applied pressure during analysis 20 mbar; injection with 20 mbar for 20 s; background electrolyte containing 0.01 mol dm-3 HCl and 0.04 mol dm-3 NaCl; detection vawelength at 230 nm. Subsequently, the repeatability of the measurement, and the stability of the tetrachloroaurate stock solution were evaluated. Also the calibration dependence were measured and the limit of detection and the limit of quantification were determined for the optimized experimental conditions. The value of LOD was 7.49 ∙ 10-6 mol dm-3 and the value of LOQ was...
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Determination of tryptophan, serotonine and melatonin in plants by using HPLC
Pavlů, Věra ; Křížek, Tomáš (advisor) ; Kozlík, Petr (referee)
This thesis deals with the development and optimization of a method for the determination of tryptophan and its metabolites - serotonin and melatonin - in plant material, in grapevine, during one analysis. It uses a high-pressure liquid chromatography. The theoretical part is about tryptophan, its metabolism and basic properties of its metabolites - serotonin and melatonin. Their occurrence in wine is also discussed. Analytical techniques by which these analytes can be determined are also provided. Then information about modern stationary phases, that are suitable for this species, is included. The experimental part consists of optimization of the method, measurement of calibration dependences and measurement of real samples. It is measured by the method of reverse phase chromatography. As first stationary phase it is used a C18 column with core-shell packing, second is a BEH Phenyl column. The mixture of 10 mM acetate buffer (pH = 4.5) and methanol is used as the mobile phase. For detection UV at wavelength 254 nm is used, then for greater sensitivity mass detectionis is used. The basic conditions for the experiment have been set. At the beginning of the analysis, the mobile phase contains 95 % (v/v) buffer and 5 % (v/v) methanol. Then the methanol content is linearly increased to 80 % (v/v) from...
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Electrophoretic determination of saccharides in flower nectar
Hurychová, Nikola ; Křížek, Tomáš (advisor) ; Sobotníková, Jana (referee)
This work deals with the development and basic validation of a method for determination of sucrose, glucose and fructose content in floral nectar. It uses capillary zone electrophoresis with contactless conductivity detection. The theoretical part describes the functions of carbohydrates in nectar, principles of capillary zone electrophoresis and contactless conductivity detection. There is also a brief overview of applications in the determination of carbohydrates. In the experimental part, sample injection at the short and at the long end of capillary were tested. In further experiments, the background electrolyte was optimized. The tested concetrations of NaOH were from 10 to 50 mmol l-1 . Optimal conditions for the experiments were injection at the short end of the capillary, 40mmol l-1 NaOH as background electrolyte and separation voltage of 15 kV. Then, the repeatability, limit of detection and quantification and recovery of the method with a real sample of nectar were verified. Lactose was used as an internal standard. Relative standard deviation was below 2 %. Limits of detection were below 0.003 mg ml-1 and limits of quantification were below 0.009 mg ml-1 . Recovery of the method was 97-105 %. Furthermore, the calibration dependences were measured, from which the concentration of...
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