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Content of rutin in selected elderberry cultivars
Píšťková, Magdalena ; Hrstka, Miroslav (referee) ; Vespalcová, Milena (advisor)
The aim of this diploma thesis was to determine the rutin content in springs and leaves of 19 elderberry species (Sambucus nigra L.) with use of liquid chromatography. Furthermore the rutin content was determined in its significant sources – rue and buckwheat. The observed values were compared in order to answer the question whether it is useful to use the elderberry spring and leaves as a new source of rutin. Theoretical part of the thesis describes elderberry in general, its chemical composition and its usage in medicine. Following part concentrates on important substances contained in elderberry – flavonoids. Also principles of extraction techniques and HPLC are discussed. In practice the rutin was gained from plant matrix with use of pressurized hot water extraction (PHWE) which was performed in three five minutes long cycles. Conditions during the PHWE were set up to 80 °C and 150 bars. Obtained extract was purified with use of SPE columns and analyzed by HPLC with DAD detector (wave length – 360 nm). HPLC was performed with SUPELCOSILTMLC-8DB column. The mobile phase was composed of MeOH, H2O, and HCOOH in ration of 36:61,5:2,5. The set up flow of mobile phase was 1 ml/min. In the leaves the highest rutin content was determined in Pregarten – 26,34 ± 0,50 mg/g. On the other hand the lowest rutin content in leaves was determined in Körsör – 3,74 ± 0,13 mg/g. In springs the obtained results were as follow. The highest content was determined in Samyl – 4,87 ± 0,01 mg/g and the lowest content was determined in Heidegg 13 springs – 0,56 ± 0,01 mg/g. Also the HPLC detection limit – 6,3 . 10-5 mg/ml and quantitation limit – 2,1 . 10-4 mg/ml were determined for rutin.
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The selection and optimization of the method for assessment of free fatty acids
Koval, Dominik ; Vespalcová, Milena (referee) ; Vítová, Eva (advisor)
This master´s thesis deals with optimization and validation of method for determination of free fatty acids. The theoretical part is focused on possibilities of extraction, extract separation, esterification, gas chromatography determination and brief description of the most important validation parameters. All with main emphasis on applying on free fatty acids. The experimental part describes the selection and procedure of optimizing individual steps of the method. Extraction of lipids was performed by solvent mixture (diethylether/petroleumether), based on the standard ČSN EN ISO 1735, for the extraction of free fatty acid solid phase extraction was tested. The acid catalyzed esterification based on ČSN EN ISO 5509 using methanolic solution BF3 was used for derivatization of free fatty acids and a gas chromatograph with a flame ionization detector was used for their determination. Subsequently, selected validation parameters of the method were verified: repeatability, reproducibility, linearity, limits of detection and quantitation. Sunflower oil and emmental type cheese, bought in common food market, were used as model samples for selection and optimatization of the method.
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Use of biomarkers for assessing environmental pollution by platinum group metals
Nedvědická, Lucie ; Řezáčová, Veronika (referee) ; Komendová, Renata (advisor)
This diploma thesis in the theoretical part analyses the characteristic feature of individual platinum group elements, their toxicity, anthropogenic sources and the presence of platinum group elements in the environment of the Czech Republic. In addition, there are specified types of bioindicators focusing mainly on lichens, mosses and needles. There are described individual bioindication techniques and pre-treatment of samples for platinum metals determination in bioindicators. The subject of the experimental part is to verify the sorption efficiency and ability of platinum and palladium using the SPE method and to determine the actual platinum metal contamination in selected localities in the city of Brno. There was also the additionally subject to verify the sorption potential of selected bioindicators and determination of the environmental pollution by platinum metals using the bag technique. In the experimental part, the bioindicators of moss Pleurozium schreberi, lichen Xanthoria parietina, lichen Flavoparmelia caperata and needles Pinus nigra were used.
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Determination of NSAIDs in wastewater
Krůzová, Sabina ; Mravcová, Ludmila (referee) ; Vávrová, Milada (advisor)
The thesis focuses on non-steroidal anti-inflammatory drugs in wastewater. It characterizes drugs and defines specific methods of determination naproxen and ibuprofen in wastewater. Besides their characteristics there are pre-analytics and final analytic methods described here which are used for determination of drugs in wastewater. To analyse we used wastewater from Veterinary and Pharmaceutical University in Brno. Samples were filtered and concentrated by solid phase extraction (SPE) and after that they were analysed by UHPLC with diode array detector. Thanks to these practices and methods, there were found, that concentration of naproxen in wastewater from VFU Brno was below the limit of quantification and ibuprofen wasn´t detected in most of cases.
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Determination of residues of the selected pesticide effective substances in wine using the GC/MS method
Ehrenbergerová, Martina ; Benešová, Karolína (referee) ; Mikulíková, Renata (advisor)
The grape is one of the oldest cultivated plants. It can be consumed as a fruit or it can be used as a raw material for making stews, juices or the cultivated drink – wine. Generations of wine-makers have been striving to improve both the cultivating conditions of vineyards and the quality of wine. Many harmful elements, such as herbivorous pests, diseases and storms are important factors that can have a negative impact on crop quality. To regulate the effects of these factors, an integrated protection system is used, incorporating agronomical measures, resistant varieties and a wide spectrum of pesticides. However, increasing the usage of pesticides brings certain dangers to both the production quality and the environment. This necessitates the monitoring of the negative effects, including the content of pesticide residues in the grapes. My thesis studies and experimentally assesses selected pesticide residues in certain wine samples.
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Analysis of fluoroquinolone antibiotics in the soil
Vdolečková, Monika ; Řezáčová, Veronika (referee) ; Mravcová, Ludmila (advisor)
The thesis dealt with the global problem of the occurrence of pharmaceuticals in the environment, specifically fluoroquinol antibiotics (ciprofloxacin and enrofloxacin), which are among other critically important antibiotics. These drugs enter the soil environment through the application of already contaminated animal waste (e.g. manure) or through wastewater used in irrigation or through the application of treated sewage sludge, which may contain drug residues. Increasing concentrations of these antimicrobial drugs in the environment provide an environment for the emergence and spread of microbial resistance. The accumulation of these drugs then leads to the emergence of resistance to these antibiotics. The experimental part of the thesis focused on the optimization of a method for the extraction and subsequent determination of fluoroquinolones in soil and litter. For this purpose, parameters related to the extraction yield of fluoroquinolones from the soil matrix were optimized, such as sample weighting, selection of a suitable extraction medium, SPE performance, elution method from the SPE, etc. Extraction recoveries of 70 to 140 % were achieved as part of the optimization. Finally, the optimised method for extraction of fluoroquinolones from poultry litter and soil samples provided by the ÚKZÚZ was used. The experimental results confirm the long-term persistence of these drugs in the environment.
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The use of GC/MS for the analysis of drugs
Sýkora, Richard ; Opatřilová, Radka (referee) ; Vávrová, Milada (advisor)
This diploma thesis is based on the current issue of the presence of pharmaceuticals in various components of the environment. Concerning the contamination by residues of pharmaceuticals the most affected environment is the aquatic environment where these substances leaks especially from wastewater treatment plants, which eliminate them during the cleaning process only partially. This work is focused on the selected group of pharmaceuticals, non-steroidal anti-inflammatory drugs (salicylic acid, ibuprofen, caffeine, naproxen, ketoprofen, diclofenac) in waste water. For analysis purposes two types of sampling were used and compared: the conventional spot sampling of wastewater and the sampling using passive samplers POCIS. The sampling took place at the inflow and outflow of the wastewater treatment plant in Brno Modřice. The solid phase extraction (SPE) using Oasis HLB columns was used as the extraction method. Extracted sample was derivatized then. Derivatization agents were: MSTFA (N-methyl-N-(trimethylsilyl)trifluoroacetamid) and BSTFA (N, O-bis(trimethylsilyl) trifluoroacetamid). The final analysis was performed using gas chromatography with mass spectrometric detection Time-of-Flight (GC/TOF-MS).
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The use of SPE methods for determination of ultratrace concentrations of platinum metals in environmental matrices
Ježek, Stanislav ; Zlámalová Gargošová, Helena (referee) ; Gregor, Tomáš (referee) ; Komendová, Renata (advisor)
This dissertation is focused on the study of sorption techniques for the determination of platinum and palladium on modified solid sorbents and ion exchangers. The final determination was made using atomic absorption spectrometry with electrothermal atomization (ET-AAS). Six modified sorbents were selected for the sorption study. Four modified non-polar silica gels were studied and two sorbents were based on styrene divinylbenzene copolymer. Furthermore, three cation exchange resins and three anion exchange resins were studied. The sorption efficiency of platinum and palladium was studied with modified sorbents and anion exchange resins. Furthermore, the influence of interfering elements (Fe, Cu, Zn, Pb, K, Na, Ca and Mg). Another parameter for evaluating the effectiveness of sorbents is the volume of the elution mixture required for effective elution of platinum and palladium from the sorbents. Based on the results, a sorbent was selected for the preconcentration of platinum and palladium from real environmental samples from the environment. The study of the concentration of platinum and palladium in environmental components is divided into two parts. The first part compares two cities with different sizes and vehicle concentrations. It is a regional capital in the Czech Republic – Jihlava and the capital of Austria – Vienna. For soil matrix sampling, locations near frequent traffic junctions were selected. In Jihlava, the concentration of platinum ranged from 16.93 to 38.72 ng.g-1 and for palladium from 2.705 to 8.452 ng.g-1. In Vienna, the detected concentrations were higher. Platinum concentrations ranged from 39.22 ng.g-1 to 159.2 ng.g-1 and for palladium from 18.45 ng.g-1 to 98.21 ng.g-1. The second part was focused on the busiest traffic junction in the Czech Republic - the D1 highway, focusing on the section near the Švihov water reservoir, which serves as one of the main sources of drinking water for the capital of the Czech Republic - Prague. Rain retention tanks - "lapolas" - are installed in this section. A soil sample was always taken in the vicinity of these lapolas, and from the lapolas the sediment in the reservoir and settled water at the outlet from the reservoir. These rain retention tanks proved to be suitable places for monitoring pollutants from automobile traffic.
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The use of solid phase extraction for fractionation of lipids in cheese matrix
Scholzová, Kristýna ; Vespalcová, Milena (referee) ; Vítová, Eva (advisor)
This bachelor thesis deals with Solid Phase Extraction, as a method for isolation of free fatty acids from cheese matrix to be subsequently determined using gas chromatography with FID detection. The theoretical part provides information about milk fat composition and related reactions being a source of flavour compounds, free fatty acids including. The main objective of the theoretical research is to summarize alternatives to determining fatty acids in cheese, focusing on current advancement and use of Solid Phase Extraction for this purpose. The practical part discovers proper technique and conditions for fractionation of lipids by Solid Phase Extraction, using aminopropyl bonded phase columns. Agilent SampliQ Amino columns were utilized to separate lipid mixture and different lipid classes were eluted using suitable organic solvents. Composition and purity of lipid extracts were verified combining thin layer chromatography and gas chromatography. Before being determined by gas chromatography, free fatty acids were converted into methylesters, based on ČSN EN ISO 12966-2. Besides discussing proper experimental conditions, the assesment also comes with solving optimal volumes of sample and eluting solvents to apply. The results of this thesis are considered to be useful base for subsequent experimental optimization and following integration of validated method into process of determining free fatty acids.
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The assesment of chloramphenicol residues in biological material, water and feed by GC/MS
Lukačková, Dagmar ; Šalplachta, Jan (referee) ; Rejtharová, Martina (advisor)
This diploma thesis addresses the presence and determination of chloramphenicol residues in biological materials. The theoretical part presents the literature retrieval containing information about veterinary medicaments with the banned use in food producing animals and also the sum of the legislative requirements concerning the presence of these substances in foodproducts and raw food materials of animal origin. The comparison was carried out between the existing analytical methods used for the determination of chloramphenicol residues in different biological materials, which are altogether based on the solid phase extraction for the extract cleaning and the new procedures for sample preparations using columns where the sorbent performs on the molecularly imprinted polymers principle.
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