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Voltammetry and liquid chromatography of cholesterol, its precursors, and oxidation products
Kubešová, Jana ; Schwarzová, Karolina (advisor) ; Baluchová, Simona (referee)
Electrochemical detection of sterols is difficult. This thesis aims to study the voltammetric behaviour of selected oxysterols, i.e. 25-hydroxycholesterol and 7-ketocholesterol on the boron-doped diamond electrode. Further, an HPLC method with spectrophotometric and electrochemical detection was developed for separation of selected sterols. The study was performed using cyclic and differential pulse voltammetry. 0.1 mol l−1 perchloric acid in acetonitrile (water content 0.55 %) was chosen as the most suitable electrolyte. 25- hydroxycholesterol provides anodic signal at the potential of +1500 mV and 7-ketocholesterol at +1900 mV in that media. Electrochemical reduction of 7-ketocholesterol was also studied. However, the observed cathodic signal isn't reproducible. The stability of oxysterols in the presence of perchloric acid was confirmed by UV-VIS spectroscopy. Calibration dependence of oxysterols was measured using differential pulse voltammetry and resulted in the limit of detection of 0.82 µmol l−1 for 25-hydroxycholesterol and 0.66 µmol l−1 for 7-ketocholesterol. In the second part of the thesis, an HPLC method was developed for the separation of a sterol mixture on a reversed-phase C18 column using a mobile phase containing 50 mmol l−1 sodium perchlorate in acetonitrile with 0% or 6% water...
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Analyses of lignans in selected variants of linseed (Linum usitatissimum L.)
DOŠEK, Miroslav
Oilseed flax is one of the traditional agricultural crops. Flax seeds contain, among other beneficial components, lignans, which are polyphenolic substances that provide the plant's defense against biotic and abiotic stress. The main naturally occurring lignan in flax is secoisolariciresinol diglucoside (SDG). Flaxseed represents the richest natural source of lignans, which have been observed to have many positive effects on human health, including antioxidant and other biological activities. One method that can be used to determine SDG is high-performance liquid chromatography with mass spectrometry (HPLC-MS), which was used in this study for the quantitative analysis of SDG. Total polyphenol content (TPC) and antioxidant activity expressed as the ability to quench the DPPH radical were also determined. Correlation analysis was performed to determine the relationships between the studied parameters. Both variety and year had a significant influence on all three studied parameters. The highest average content of polyphenols and SDG was found in the Agram variety, while the highest antioxidant activity was determined in the Floral variety. A significant positive correlation was observed only between the total polyphenol content and the SDG content. The results of this study demonstrate the considerable influence of variety and growing conditions on the content of lignans and the antioxidant potential of flaxseed, which predetermines its health benefits.
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Determination of selected mycotoxins in tea
Pustka, Václav ; Maleček, Miroslav (referee) ; Kuchyňa, Jaroslav (advisor)
This diploma thesis deals with the development and validation of an analytical method using high performance liquid chromatography method with fluorescence detection for the simultaneous determination of aflatoxins and ochratoxin A in herbal and fruit tea. The theoretical part describes the most common groups of mycotoxins and the most important methods for their determination in food. The great attention is devoted to HPLC method and the overview of the derivatization techniques for aflatoxins B1 and G1 fluorescence response enhancement. The practical part of this study focuses on the optimization of sample extraction and purification, the settings of the instrumental analysis and the photochemical reactor assembly. The thesis also involves the determination of the basic performance characteristics for the successful method validation.
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Study of glyphosate degradation in water plasma application
Vašinková, Alena ; Vávrová, Milada (referee) ; Mravcová, Ludmila (advisor)
This work deals with the current problem of increasing concentrations of glyphosate in groundwater and wastewater due to insufficient efficiency of methods used in wastewater treatment. From this point of view effective removing of glyphosate from water have to be developed by new methods and technological processes. The methods used so far in wastewater treatment plants should be replaced or supplemented by advanced oxidation processes. The practical part of this work is devoted to glyphosate and its degradation in water by plasma. Samples were taken sequentially during plasma application and further evaluated by LC/MS selected as suitable analytical methods. The aim of this work was to determine the efficiency of plasma in water with admixture of glyphosate.
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Application of passive sampling for the analysis of hormones in drinking water
Remerová, Martina ; Mravcová, Ludmila (referee) ; Čáslavský, Josef (advisor)
The thesis focuses on the use of passive sampling during an analysis of hormones in drinkable water. In the theoretical part there are described selected passive samplers and the sample of the type of POCIS is described at fuller length. The next chapter engages with steroid hormones and an input of estrogenic hormone into the environment. The thesis contains chapters dealing with possibilities of the determination of hormones in water. It is specialized on the analysis of drinkable and surface water. In the last chapter of the theoretical part there are introduced water works where samples for an experimental assessment were collected from. The experimental part of the thesis presents the specification of the extraction of analytes and an adjustment of used device. In the thesis there are specific calibrations for individual assessment of hormones. The results of the assessment for each collection point are ordered to a well-arranged table. Increased levels of targeted estrogens were not approved in most of sampling points.
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Possibilities of elimination of sulfonamides from the aquatic ecosystem
Suková, Petra ; Mravcová, Ludmila (referee) ; Vávrová, Milada (advisor)
This diploma thesis focuses on the determination of sulfonamide antibiotics especially the possibility of elimination of these substances from the aquatic ecosystem. Nowadays, environmental contamination of the pharmaceuticals and their residues is a serious concern. Main sources of this contamination are wastewater treatment plants (WWTPs), where these compounds are not effectively removed by contemporary conventional technology. For this reason, new methods are being developed and tested that could eliminate the number of contaminants entering the environment in this way. There is a possibility to use the potential of the enzymatic system of wood-decay fungi, especially white rot fungi. Six representatives of sulfonamide antibiotics were selected and isolated from the aquatic matrix via solid phase extraction. The final identification and quantification method was high performance liquid chromatography with mass spectrometric detection. Monitoring of the concentration level of selected sulfonamide antibiotics at the inflow and effluent at the Brno-Modřice WWTP was carried out weekly. Moreover, the effectiveness of elimination of selected antibiotics from the aquatic ecosystem by the use of Trametes versicolor wood-decay fungi cultured on a suitable carrier was verified.
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Analysis of main wine saccharides
Horáková, Hana ; Šabata, Pavel (referee) ; Vespalcová, Milena (advisor)
This diploma thesis deals with determination of carbohydrates in wine. Theoretical part attends to production of wine from grape to treatment and training of wine. It refers saccharides in wine, especially glucose and fructose. The study provides an overview of the available sources concerning the possibilities of determination of carbohydrates in wine by chromatographic methods and Skalar automated chemistry analyser. The study shortly refers simple analytical methods for determination of wine saccharides. The experimental part based on this search deals with analysis of saccharides by high performance liquid chromatography with refractive index detector and UV detector on aminoalkyl column and determination of reducting sugars by Skalar automated chemistry analyser. Finally, the results of these methods were compared.
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Isolation of pure aminoacids from wheat bran
Sloupová, Klára ; Diviš, Pavel (referee) ; Pořízka, Jaromír (advisor)
Wheat bran is a promising material containing a wide range of useful components, including proteins. In addition, it is produced in significant volumes. Currently, wheat bran is used for the production of energy by combustion and for feed purposes. Gradually, new methods of valorization of this material are being sought. One of the possibilities of using wheat bran is the isolation of proteins, hydrolysis, and separation of selected amino acids. This diploma thesis deals with this issue, it is focused on the recovery of arginine and leucine from a protein isolate. Proteins were extracted from wheat bran by changing the pH. Thanks to the subsequent lyophilization a protein isolate was gained. Prior to hydrolysis of the resulting isolate, a stability test of arginine and leucine amino acid standards was first performed, to which various hydrolysis methods were applied. Acid hydrolysis using a mineralizer, which was applied to the protein isolate, was proved to be the most effective. This was followed by the derivatization of the hydrolysates with OPA and analysis of the resulting hydrolysates by high-performance liquid chromatography with UV-VIS detection. Then, suitable adsorption and desorption conditions were optimized. It was found that the time dependence does not affect the amount of adsorbed material on the sorbent. Therefore, an application time of 15 minutes was chosen. While optimizing the amount of used standard, it was found that the optimal weight was 0.25 g of sorbent. The selected conditions were applied to the protein hydrolyzate. Two fractions were obtained by the separation of selected amino acids due to the change in the pH of the citrate buffer. After the application of this procedure, 0.26 g of arginine and 0.82 g of leucine were obtained from one kilogram after evaporation. From evaporation two, 1.01 g of arginine and 0.25 g of leucine were obtained after evaporation.
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Removal efficiency of selected drugs by various sorptive materials from water
Štofko, Jakub ; Mravcová, Ludmila (referee) ; Vávrová, Milada (advisor)
This thesis deals with sorption of selected drugs from model water by various sorption materials. Contamination of water resources by the pharmaceutical industry is a major problem today. Wastewater treatment plants, whose technological processes are unable to completely remove them, have a significant share in the penetration of these substances into the environment. At present, attention is paid to alternative materials that are capable of eliminating these substances. One of the potential sorption materials is biochar as one of the main pyrolysis products. This work focused on the assessment of the sorption properties of the different types of biochar and commercially used active charcoal. The sorption properties of the individual materials were compared with respect to the non-steroidal anti-inflammatory substance ibuprofen and the sulphonamide antibiotic sulfamethoxazole. The results of vial experiments were analysed on a liquid chromatograph with mass detection.
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Study of microplastic sorption properties
Hlaváčková, Hana ; Kučerík, Jiří (referee) ; Řezáčová, Veronika (advisor)
There is currently an effort to replace conventional plastics with biodegradable products that will have the ability to replace these substances. One of the possible biodegradable felt, which is currently being studied in detail, is also poly (3-hydroxybutyrate), which is produced by bacteria. This bachelor thesis deals with the sorption of selected substances on poly(3-hydroxybutyrate) microparticles. Substances whose contamination of water sources is a significant problem today have been selected for this work. Specifically, the sorption of the nonsteroidal anti-inflammatory substance ibuprofen, the triazole fungicide tebuconazole and the most common drug caffeine on PHB particles, which fall in the size of the microplastic group, were studied. The method of liquid chromatography with mass detection was used for analyzes.
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