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Study of the Selected Types of Sulphur Compounds in Beer and Brewing Materials
Mikulíková, Renata ; Ventura, Karel (referee) ; Ventura, Karel (referee) ; Čáslavský, Josef (referee) ; Márová, Ivana (advisor)
Much attention has been recently devoted to sensorially active substances affecting beer quality in the Czech Republic and worldwide. Among them, the heterocyclic and sulphur containing compounds play an important role, some of them with high sensorial activity even in extremely low concentrations. Trace amounts of these compounds, which can be frequently found in foods, participate in formation of their aroma and this effect can be generally evaluated as favorable However, in malt or beer it is true only to a limited extent and the presence of heterocyclic and sulphur containing compounds are in this respect assessed rather unfavorably. The aim of the present study was to provide a survey about of problems in the field of sulphur containing compounds in barley, malt and beer, to describe metabolic paths leading to their formation and to verify experimentally possibilities of their determination using modern analytical methods. Sulphur-containing amino acids are a natural part of barley, malt and beer and are precursors of the origin of volatile sulphur substances. The most frequently occurring sulphur amino acids, metionine, cysteine and homocysteine, were selected for analytical monitoring. The method of gas chromatography was used to determine sulphur-containing amino acids in barley, malt and beer. Prior to the analysis, sulphur-containing amino acids were derived and volatile N(O,S)-ethoxycarbonyl propyl esters were formed; they were subsequently analyzed using the gas chromatography with mass detector (GC/ MSD) and the gas chromatography with flame photo detector (GC/ FPD). Direct analysis of sulphur volatile substances is possible only rarely as they are found in the analyzed matrices (malt, beer) only in very low concentrations ( g/kg,l - ng/kg,l). Before the analysis, the analytes must be extracted from the matrix and concentrated. The modern analytical methods SPME (Solid Phase Micro Extraction), SPDE (Solid Phase Dynamic Extraction) and TDAS (Thermal Desorption Autosampler) were experimentally compared for the extraction and subsequent concentration of sulphur volatile substances. The method of gas chromatography with flame photo detector was used to determine sulphur volatile substances. Following volatile sulphur substances were monitored: dimethyl sulphide, dimethyl disulphide, dimethyl trisulphide, carbon disulphide, ethyl sulphide, diethyl disulphide, methionol, 3-methylthiophen, ethyl thioacetate, 2-methyl-1-buthanthiol. Only metionine was detected in significant amounts in the barley samples analyzed. Not only content but also dependence on a variety and locality were studied. Further, changes in methionine, cysteine and PDMS content during malting were followed. Results proved a significant decline in these substances content depending on the kilning temperature. Three types of fibers were tested for the analyses of the selected volatile sulphur substances in beer in the SPME method. PEG - a fiber with stationary phase Carbowax, PDMS - a fiber with stationary phase polydimethylsiloxan and a combined fiber CAR/PDMS - Carboxen and polydimethylsiloxan. Carbon disulphide, methionol, dimethyl sulphide, 3-methylthiophen and diethyl disulphide were detected with this method. Content of the other analyzed volatile sulphur substances was below the limit of detection. Further was tested usage the SPDE and TDAS methods. Both methods appear to be the suitable for the determination of volatile sulphur substances in beer.
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Determination of content of organic compounds in biochar
Novotná, Martina ; Řezáčová, Veronika (referee) ; Mravcová, Ludmila (advisor)
Biochar is created during the pyrolysis of organic biomass. Once added into the soil, it can improve its features. Biochars made from sewage sludge have various compositions. It is because of the vast difference between entrance materials. Organic pollutants can be absorbed into its surface during the cooling proces sof pyrolysis. If released into the enviroment, these compounds can cause inhibition of plant growth, get into food chains and adversely affect living organisms. Organic pollutans are determined most often by GC/MS after organic solvent extraction.
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Determination of selected musk compounds in biotic samples
Blahová, Eliška ; Čáslavský, Josef (referee) ; Vávrová, Milada (advisor)
Musk compounds (MUSK) or synthetic fragrances are organic substances commonly used as fragrant constituents of detergents, soaps, cosmetics, personal care products, industrial and in-house cleaning agents, industrial plasticizers, chewing tobacco and fresheners. The big attention is pushed ahead studying these compounds, their fate in different parts of ecosystems and studying their characteristics at present, because musks infiltrate many environmental components, particularly aquatic and marine ecosystems, through their large application and their ability to be perzistant. This diploma thesis was focused on four synthetic “classical” fragrances used over the world. The aim of this study was to perform a method optimisation for the determination of selected fragrances in biotic matrix. There was made an evalution of ability of selected water treatment plant to clear away musks from water, these results were used for evaluating contamination measurement of aquatic ecosystem. The identification and quantification of analytes was carried out by high resolution gas chromatography - mass spectrometry (HRGC/MS).
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Application of Separation Techniques Connected with Mass Spectrometry for the Analysis of Environmentally Important Compounds
Mácová, Daniela ; Čelechovská, Olga (referee) ; Márová, Ivana (referee) ; Demnerová, Kateřina (referee) ; Čáslavský, Josef (advisor)
The identification of the hydrolysis and photodegradation products of flexible polyurethane foams (PUFs) with addition of biooriginated and biodegradable additive was the first topic of this dissertation work. Separation of polyurethane foam hydrolysis degradation products, designed for ecotoxicological tests, was managed by high-performance liquid chromatography coupled with mass spectrometry (HPLC/MS). The degradations product structure was elucidated by tandem mass spectrometry (MSn). PUF photodegradation products were obtained by exposure of materials by irradiation at 254 nm. Semi-volatile degradation products were isolated from the exposed polyurethane by n-hexane extraction; volatile compounds were collected by solid phase microextraction (SPME). Gas chromatography with mass spectrometry (GC/MS) and complete orthogonal tandem gas chromatography with mass spectrometry (GCxGC/TOF MS) was used for separation and identification of photodegradation products. The influence of the bio-filler on the character of degradation products and the possible effect of PUF degradation products on the environment was discussed at the end of this section. The determination of isoprostanes – markers of oxidative stress in tissues of beadlet anemone (Actinia equina) was the subject of the second topic. F2-isoprostanes were synthesized from the arachidonic acid. With thereby prepared isoprostanes the method of determination by liquid chromatography with tandem mass spectrometry (HPLC/MS/MS) was developed and optimized. The isoprostane isolation process from the Actinia equina tissues was optimized with solid phase extraction (SPE). The resulting methodology was used to quantify isoprostanes in tissues of anemones, which were exposed to both moderate and high temperature changes. The temperature changes were used to initiate the oxidative stress in organisms. In addition, concentration levels of unknown compounds were also monitored. These unknown compounds were extracted from tissues together with F2-isoprostanes and their identity is discussed in this dissertation work too. The possibility of using isoprostane levels in the Anthozoa tissues for the oxidative stress monitoring is discussed in the conclusion of this work.
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Determination of organic compounds in biochar produced by microwave torrefaction of biomass
Meindl, Jiří ; Vávrová, Milada (referee) ; Mravcová, Ludmila (advisor)
The thesis is focused on a determination of polycyclic aromatic hydrocarbons (PAHs) contained in dried pelletized sewage sludge and pelletized biochar. Biochars were made in mild conditions by microwave torrefaction of prepared sewage sludge. There were analyzed and quantified the 34 of standardized PAHs compounds in two series. The first serie, also called “Sada 1”, has been aimed at comparison of extraction methods for the chosen sample of sewage sludge and the sample of biochar. In serie “Sada 1”, there were compared efficiencies of chosen type of solvent or solvent mixture by comparison of yields for 34 standardized analytes in a sample of biochar and a sample of sewage sludge. There were compared also to total yields of PAHs and to number of quantified compounds in analyzed samples. The most reliable extraction method has been used for the next analyses of samples in the second serie called “Sada 2”. In Sada 2, there were compared different samples of the same type (e.g. biochar, sludge). The origin of sewage sludge (small or big sewage treatment plant expressed as PE) and used additives (cellulose, chaff, hay) as modificators for torrefaction process were variables for different type of sample. The results of analysis were identification of the most suitable sewage sludge and additive to be used as modificator for microwave torrefaction process. The main goal of correctly chosen sludge and additive was to minimize production of PAH’s during torrefaction and in samples of biochar.
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Study of selected vegetable oils from nuts
Lovásová, Kristína ; Kovalčík, Adriána (referee) ; Zemanová, Jana (advisor)
The bachelor´s thesis deals with the characterization of the selected nut oils. The theoretical part concentrates on the topic of vegetable oils, their composition and properties. It also focuses on the nuts, the specification of the selected nut oils and their use in different industries. It includes an overview of analytical methods suitable for assessing the quality of oils. The experimental part compares the results of the oil characterization using the selected methods. Based on the results, the differences between the samples were evaluated. The properties of the oils were determined on the basis of fat characteristics. These were subsequently specified by the determination of fatty acid composition. Fatty acids were determined using gas chromatography with a flame-ionization detector after conversion to methyl esters by acid esterification with boron trifluoride. The determination of volatile compounds was performed through solid-phase microextraction with gas chromatography separation and mass spectrometry detection. According to the fat characteristics, in particular the peroxide value, it was found that both oils were partially oxidatively degraded, even though they were stored in the refrigerator (4 °C). A total of 13 saturated, 7 monounsaturated and 4 polyunsaturated fatty acids were detected. The total content of fatty acids varied, the higher content was detected in the walnut oil. Significant differences occurred in the composition of unsaturated fatty acids; the hazelnut oil had a higher content of monounsaturated oleic acid, the walnut oil had a high content of polyunsaturated linoleic and -linolenic acids. A total of 29 volatile compounds were identified, the number and content of volatile compounds in samples differed. 20 volatile compounds were identified in the walnut oil, and 19 compounds in the hazelnut oil. The higher content was in the hazelnut oil, the quantitatively most important group were aldehydes in both oils.
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Personal care products as environmental contaminants
Babuš, Ondřej ; Stoupalová, Michaela (referee) ; Vávrová, Milada (advisor)
Synthetic musk compounds were first prepared artificially in the late 19th century. They have been used to perfume cosmetics, detergents and personal care products. The attention of many researchers has been focused on it recently, due to its high penetration into the nature which is a logical consequence of its great use. The main goal of this thesis is to determine the effect of the ultrafiltration on the concentration reduction of substances mentioned above in the industrial waste waters produced by the cosmetic company. Analytes from the sample were extracted using solid phase microextraction (SPME) and on gas chromatography analysis with mass spectroscopy (GC / MS) has been performed. The whole method was optimized and evaluated. Determination of the average efficiency of the ultrafiltration was made based on data obtained before and after ultrafiltration. Such efficiency determines the suitability of use of this method for removal of synthetic musk compounds from waste waters.
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Assessment of synthetic musk compounds in waste waters
Štefka, Michal ; Čáslavský, Josef (referee) ; Vávrová, Milada (advisor)
The synthetic aromatic substances are present in the products of personal hygiene, detergents and cosmetics. After the application these compounds are drained away into the waste water. But the technological process used in sewage works is not able to eliminate these substances and these ones influence the particular items of the environment. The aim of the degree work is the determination of four selected items of the linear musk compounds (2-cyclohexylethanole, Fresco Menthe, Citronellol and Isobornyl acetate) in the wastewater. The real patterns were taken on the place of affluent of the sewage discharge and on the place of the draining off in the sewage plant in VFU Brno. On the basis of measurements and subsequent evaluation on of obtaining data it was possible to express the measurement of efficiency of the elimination of the present musk compounds. Firstly it was necessary to adapt the selected analytical method to the physical and chemical qualities of the prescribed analytes. The analytes were extracted from the patterns by the method of the micro extraction for the consistent phase so called solid phase microextraction (SPME). The gas chromatography in the tandem connection with the mass spectrometry makes the identification and quantification possible.
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