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Impact of soil samples treatment and used measurement methods on heavy metals concentrations.
Kejík, Marek ; Marko, Michal (referee) ; Hajzler, Jan (advisor)
This bachelor thesis aims to explore the possibilities of treatment of soil samples and compare the suitability of selected analytical methods of analysis for determining the concentration of heavy metals. 7 reference certified materials of various soil types and one soil sample from the recreational area located in Brno were selected. Each soil sample was subjected to three different treatments. It is a method of melting into a solution, decomposition in aqua regia and aqueous extract. All thus treated samples were subsequently subjected to analytical methods for determining the concentration, specifically the ICP-OES and GF-AAS methods were used. To assess the suitability of selected methods of treatment of soil samples and analytical methods of determination, the 4 most risky elements were selected, namely arsenic, cadmium, copper and lead. The measured concentrations were compared with reference values of soil samples. Finally, the suitability of combinations of different sample preparation procedures and selected methods of analytical determination of the content of determined elements from soil samples was assessed.
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Production technology of wine sausage with reduced salt content
Martonová, Rebeka ; Punčochářová, Lenka (referee) ; Mikulíková, Renata (advisor)
The aim of this bachelor thesis was preparation of wine sausages with reduced salt content, followed- up by sensory analysis. The theoretical part generally characterizes meat and meat products, sodium chloride and its importance in food. In the next chapters, the paper deals with sensory analysis of samples and analytical method for determining the concentration of elements in biogenic samples, in particular inductively coupled plasma - optical emission spectrometry. The experimental past focuses on the evaluation of data from sensory analysis using the Kruskal- Wallis and Spearman test. The samples were analyzes using ICP-OES method. The analysis determined the concentration of sodium and potassium in the samples before and after roasting.
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Physical hydrogels based on biopolymers and surfactants
Velcer, Tomáš ; Lehocký, Marián (referee) ; Kráčalík, Milan (referee) ; Pekař, Miloslav (advisor)
This doctoral thesis studies the properties and behaviour of phase-separated hydrogels. These can be prepared by interaction of polyelectrolytes with oppositely charged surfactants. Negatively charged polysaccharide hyaluronan and cationic surfactant carbethopendecinium bromide (Septonex), whose properties, behaviour and utilization are described in the first two chapters of theoretical part, were selected for this role. Hyaluronan is naturally-occuring in living organisms and is known for his specific targeting to the tumour cells. Septonex is used as antiseptic and disinfectant. Experimental part of this work is focused on examination of the structure and behaviour of these types of hydrogels especially from rheological point of view. The crucial part of this study was to establish mechanical properties and their dependence on environment. This led to design further studies. Structural analysis was held using the methods of ATR-FTIR, ionic chromatography and ICP-OES helping to measure the inner content of entry materials in the gels and supernatants respectively. The last chapter deals with antimicrobial activity. The results of this study indicate a potential usage of these substances in the field of medical applications.
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Study of the authenticity of spices and condiments
Štursa, Václav ; Golian, Jozef (referee) ; Urík, Martin (referee) ; Diviš, Pavel (advisor)
This disertation deals with geographical authentification of different types of spices and spice preparations. Investigated spice species were garlic (Allium sativum), ground pepper (Capsicum anuum), and dried carrot (Daucus carota). Theoretical part of the disertation describes main qualitative parameters of the examined species and production technology, means of food adulteration and statistic methods used in chemometrics. The aim of this dissertation was to verify the hypothesis whether it is possible to use targeted analytical techniques commonly used in quality control of spices and condiments, and statistical processing of measured data to distinguish samples of spices and condiments of different geographical origin. The use of non-targeted analysis was also investigated. Samples of garlic and ground pepper were used for targeted analysis. The examined parameters were dry matter and moisture of the sample, ash content, total phenolic content according to Folin-Ciocaulteu, carbohydrate content, alliin concentration, total nitrogen content, total color pigment (ASTA), pH of aqueous extract, total fat content, and concentration of selected elements (Ca, Cu, Fe, K, Mn, Mg, Na, P, Zn). The instrumental techniques used were molecular absorption spectrometry, inductively coupled plasma optical emission spectrometry and high performance liquid chromatography. The obtained data were statistically processed by analysis of variance (ANOVA) and principal component analysis (PCA). Using statistical analysis significant differences between samples that came from more distant areas were found. However, samples from closer areas could not be distinguished. The researched hypothesis could not be unequivocally confirmed or refuted. Metabolic fingerprint of carrot samples was determined using non-targeted analysis. Metabolic analysis was performed using the tandem LC-TOF-MS technique. The data were processed by recursive peak extraction (BRE) and subsequently uvaluated with PCA. The samples were divided into clusters according to their origin. Targeted and non-targeted techniques have great potential in verifying the geographical authenticity of different types of spices. However, the main condition is consistent and sufficient sampling, guaranteed information on the origin of the sample and obtaining a sufficient amount of input data for statistical analysis.
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Analysis of onion and garlic samples of different geographical origin
Korček, Jakub ; Mikulíková, Renata (referee) ; Diviš, Pavel (advisor)
Presented master thesis dealt with the analysis of garlic and onion samples and tried to find correlations between chemical composition and country of origin. The parameters examined were dry content, crude protein content, concentration of phenolic compunds, carbohydrate content (fructose, glucose), alliin content and concentration of selected elements (P, Mg, Ca, Na, K, Fe, Zn). Average content of dry matter of fresh samples was 35,84 ±2,12 g/100 g and of dehydrated samples was 90,61 ±2,90 g/100 g. Concentration of phenolic compounds was measured spectrophotometrically with Folin-Ciocault reagent. Average phenolic compounds content of samples was 0,1840 ±0,1286 GAE g/100 g. Crude protein content was measured by Kjeldahl method, and calculated from total nitrogen content. Carbohydrates were measured by HPLC-ELSD after hydrolysis of fructans. Average content of fructose of garlic samples was 57,014 ±0,863 g/100 g, of onion samples was 33,718 ±1,168 g/100 g. Average content of glucose of onion samples was 22,633 ±0,405 g/100 g. Alliin content was measured by HPLC-DAD method. Average alliin content of fresh samples was 4,644 ±0,446 g/100 g and of dehydrated samples was 1,962 ±0,180 g/100 g. Elemental analysis was conducted by ICP-OES method. Average concentration of selected elements was: P 2,15 ±0,11 mg/g, Mg 0,638 ±0,03 mg/g, Ca 1,246 ±0,05 mg/g, Na 0,550 ±0,08 mg/g, K 7,49 ±0,41 mg/g, Fe 79,3 ±6,16 mg/kg, Zn 11,4 ±3,33 mg/kg. Obtained data were statistically processed on significance level 0,05. Based on the principal components analysis, it was found, that the best parameters to differentiate samples from Czechia, Poland and Ukraine from other countries were content of nitrogen, phosphorus, magnesium, sodium and calcium. It was also discovered, that genus differences between onion and garlic have greater significance than geographical differences.
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Determination of microelements by ICP-OES after extraction by DGT technique
Habartová, Aneta ; Pořízka, Jaromír (referee) ; Diviš, Pavel (advisor)
This thesis is focused on determination of microelements (Cd, Co, Cu, Fe, Mn, Ni, Pb a Zn) in milk by optical emission spectrometry with inductively coupled plasma (ICP-OES) after extraction by Diffusion Gradients in Thin films technique (DGT) containing Chelex 100 resin gel and agarose diffusion gel. The optimalization of DGT in model metal solutions was verified by recommended basic tests. The performance of the DGT technique in the diluted milk matrix was verified. By DGT technique was determined only Zn in real milk matrix with concentration 3,74 ± 0,02 mg/l. The other microelements in the prepared eluate were at or below the limit of detection of the instrumental method. The obtained results were compared with the analysis of milk after microwave digestion by ICP-OES. However, these results were below the detection limit of the device too, only Zn with concentration 3,91 ± 0,16 mg/l was measured. For the future analysis of the selected microelements in milk by DGT technique, further optimization of the preconcentration technique is required, or use of a more sensitive instrumental method.
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Analysis of sweet peppers of different geographical origin
Fiala, Petr ; Mikulíková, Renata (referee) ; Diviš, Pavel (advisor)
The diploma thesis is focused on the determination of basic nutritional properties of 26 samples of ground pepper from different countries and evaluates, whether the chemical composition of ground pepper is affected by the geographical origin. The amount of 19 nutritional properties were determined by advanced analytical methodes (ICP-OES, HPLC DAD, HPLC ELSD) together with other laboratory techniques. Final results were statistically processed by the methods of analysis of variance (ANOVA), cluster analysis, principal component analysis (PCA) and discriminant analysis (DA). Statistical evaluation confirmed, that the chemical composition is affected by the geographical origin. Analysis of variance (ANOVA) determined 14 parameters to statistically differ (p
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Study of geographical authenticity of Moravian white wines
Horáková, Kristýna ; Křikala, Jakub (referee) ; Diviš, Pavel (advisor)
The aim of this bachelor thesis was to verify geographical autenticity of Moravian white wines based on elemental analysis. This data were completed with the analysis of organic acids, fenolic compounds and atioxidants in wines. There were used two spektrometric methods for the elemental analysis (ICP-MS and ICP-OES). The concentration of organic acids was mesured by Ion chromatography. To determine the concentration of phenolic compounds in wines there was used the high performance liquid chromatography (HPLC-DAD), the content of antioxidants and the total content of phenols was measured on spectrophotometer. In total there were 33 samples of wine from 4 Moravian subregions. For the purpose of determination the samples in groups the dataset was firstly corrected by Grubbs test for remote results. From those data the box plots were created which represents the minimal, maximal and mean concentrations of each measured component. Furthermore the analysis of variance was applied, which picked up 12 statisticly valuable parameters from the whole 47. By appliyng the multidimensional statistical methods (Pearson correlation analysis (PCA) and discriminant analysis (DA)) were compiled mathematical models for the division of Moravian wines according to geographical origin. The success rate of the discrimination test was 96,97%. The cross-validation test showed an 81,82% success rate for classifying unknown samples.
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Monitoring of chemical composition changes in wine during the wine making process
Orságová, Marie ; Punčochářová, Lenka (referee) ; Diviš, Pavel (advisor)
The Chardonnay wine variety was harvested in the region of Znojmo on the wine rout Načeratický kopec. In connection with the entire winemaking process of this particular variety, research was focused on mineral concentration changes during the maturation process. The theoretical part characterizes the technology of wine production, as well as the classification and chemical composition of wine. In the experimental part, the analytical technique of inductively coupled plasma optical emission spectrometry (ICP-OES) was used for the determination of minerals (K, Ca, P, Mg, Na, Zn, Cu, Fe and Mn) in wine. The data show the differences in the concentrations of all macroelements and microelements during the whole wine production technology.
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Nutritional composition of different type of milk
Viznerová, Veronika ; Punčochářová, Lenka (referee) ; Diviš, Pavel (advisor)
The aim of this bachelor’s thesis was to compare selected methods of milk treatment for elementary analysis using the ICP-OES technique. Certified reference material ERM®-BD150 was used to validate the method, which was treated by mineralization, the addition of reagents and dispersion. The highest calcium yield during validation was determined to be 90,6 ± 8,6 % with the addition of Triton X-100 reagent. In the potassium analysis, the highest yield was determined to be 89,5 ± 5,2 % by wet decomposition. The highest yield of magnesium was determined to be 120,1 ± 1,1 % after microwave decomposition. Furthermore, the highest yield of sodium was determined to be 104,4 ± 4,8 % by wet decomposition and the highest yield of phosphorus was determined to be 98,6 ± 4,5 %. Based on the validation results, suitable methods were selected for the analysis of real milk samples (wet decomposition, acid dispersion, addition of Triton X-100 reagent). Samples of fresh cow's, goat's and sheep's milk from domestic breeding were used for the analysis. The highest concentrations of most elements were determined in goat 's milk, namely calcium to 1 733 ± 126 mg.kg-1, potassium to 1 840 ± 39 mg.kg-1, magnesium to 252 ± 77 mg.kg-1, copper to 1,41 ± 0,56 mg.kg-1, manganese to 0,54 ± 0,26 mg.kg-1 and zinc to 7,98 ± 1,33 mg.kg-1. The highest concentrations of sodium in sheep's milk were set at 515 ± 90 mg.kg-1, phosphorus at 1 440 ± 100 mg.kg-1 and zinc at 7,98 ± 1,33 mg.kg-1. The most iron was found in cow's milk, namely 5,27 ± 1,59 mg.kg-1. For ICP-OES analysis, the use of an acid dispersion appears to be the best method of sample preparation, as the concentrations of the measured elements were the highest. However, only macroelements and zinc were measured reliably. For the determination of other biogenic elements, it would be more appropriate to choose a more sensitive technique or preconcentration of the analyte in the sample.
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