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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
11

Stanovení oxinů v biologických materiálech metodou HPLC / HPLC determination of oximes in biological samples

PROCHÁZKA, Petr January 2008 (has links)
Reactivators of acetylcholinesterase inhibited by organophosphate inhibitors play an important role in organophosphate poisoning therapy. There are a large number of reactivators being tested for their ability of penetration through blood-brain barrier (BBB) nowadays. The main aim of this thesis is to test this ability in four well know reactivators {--} HI-6, K-027, K-074 and TO-032. The 5% lethal dose (LD50) {--} therapeutic dose - of each reactivator was i.m. (intramuscularly) applied to experimental animals (Wistar rats) into right posterior thighs. Then the animals were sacrificed and the blood (plasma) and brain were collected for HPLC analysis. Subsequently, brain and plasma were frozen at -80 °C and stored until the assay. The reactivator concentrations were measured in plasma and four parts of the brain {--} frontal cortex (FC), basal ganglia (BG), ponto-medullar part (PM) and cerebellum (Ce). There were five animals for each group used for the purpose of the experiment. The concentrations of reactivators in plasma and blood samples were measured using HPLC-UV/VIS methodology. HI-6 concentrations CFC were on the average 4.29% of Caverage in plasma, CBG were on the average 1.9% of Caverage in plasma, CPM were on the average 2.3% of Caverage in plasma, and CCe were on the average 1.85% of Caverage in plasma. These rates were counted from all concentrations within the scope of particular observed parts of the brain. All the other tested reactivators were not quantified in brain at all.
12

Desenvolvimento de método para determinação de agrotóxicos (perturbadores endócrinos) em água / Development of method for determination of pesticides (endocrine disruptive) in water

Santos, Ruyanne Andreza Camilo 26 February 2016 (has links)
Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES / The water pollution causes changes in physical, chemical and biological water, which interfere with their quality, preventing its use for human consumption. Most chemical contaminants in surface water are related to industrial and agricultural sources. Since, with farming the Brazil pollute existing water resources making use of pesticides and fertilizers. This study aims to develop a fast and efficient method based on extraction techniques in solid phase (SPE) and high-performance liquid chromatography with UV detection in the ultraviolet and visible with diode array (HPLC UV-Vis / DAD) for the determination of pesticides, endocrine disruptors, epoxiconazole, fenarimol, fenbuconazole, flusilazole, flutriafol, and vinclozolin in water using biocarvões produced from agro-industry waste as an alternative sorbent for SPE. Tests with the analytes allowed the adjustment of the chromatographic conditions for simultaneous analysis of five selected pesticides. The optimal condition for the extraction of analytes was performed using 0.5 g of adsorbent to 50 mL of ultrapure water and eluted with 5 mL of acetonitrile. The biochar produced from coconut waste was tested as an adsorbent for the extraction by SPE and showed good recovery results between 75% ± 9 - 119 ± 12% for the concentration levels of 0.5 to 1 ug mL-1. The parameters studied to validate the method were: linearity and sensitivity, obtaining a good sensitivity and linear response with 0.9998 coefficients in the range of 0.01 to 10 ug mL-1; precision based on the precision of measurements (Intra) and intermediate precision (interday), obtaining results of 0.1-1%, 0.6-1%, respectively; accuracy with recovery values of 60 ± 37% - 117 ± 3% to the concentration levels of from 0.025 to 0.1 mg L-1 and 75 ± 9% - 119 ± 12% for levels 0.5 to 1 ug mL- 1 related to the biochar and C18, respectively. The LD 0.01 to 0.025 in range and LQ from 0.025 to 0.5 ug mL-1. The method developed was adequate for the determination of pesticides in water samples. / A poluição aquática provoca mudanças nas características físicas, químicas e biológicas das águas, as quais interferem na sua qualidade, impossibilitando o seu uso para o consumo humano. A maioria dos contaminantes químicos presentes em águas superficiais estão relacionados às fontes industriais e agrícolas. Uma vez que, com a atividade agrícola o Brasil polui os recursos hídricos existentes fazendo uso de agrotóxicos e fertilizantes. O presente trabalho tem como objetivo desenvolver um método rápido e eficiente baseado nas técnicas de extração em fase sólida (SPE) e cromatografia líquida de alta eficiência com detector espectrofotométrico na região do ultravioleta e visível com arranjo de diodos (HPLC UV-Vis/DAD) para a determinação dos agrotóxicos, perturbadores endócrinos, epoxiconazol, fenarimol, fenbuconazol, flusilazol, flutriafol, e vinclozolina, em água, utilizando biocarvões produzidos a partir de rejeitos de agroindústria, como adsorvente alternativo para a SPE. Testes realizados com os analitos permitiram o ajuste das condições cromatográficas para análise simultânea de cinco agrotóxicos selecionados. A condição ótima de extração dos analítos consistiu em utilizar 0,5 g do adsorvente para 50 mL de água ultrapurificada e eluição com 5 mL de acetonitrila. O biocarvão produzido a partir de rejeitos de coco foi testado como adsorvente para a extração por SPE e apresentou resultados satisfatórios de recuperação entre 75 ± 9% – 119 ± 12% para os níveis de concentração 0,5 a 1 μg mL-1. Os parâmetros estudados para a validação do método foram: linearidade e sensibilidade, obtendo-se uma boa sensibilidade e resposta linear com coeficientes de 0,9998 no intervalo de 0,01 a 10 μg mL-1; precisão com base nos estudos de repetibilidade (intradia) e precisão intermediária (interdia), obtendo-se resultados de 0,1–1%, 0,6–1%, respectivamente; exatidão com valores de recuperação entre 60 ± 37% – 117 ± 3%, para os níveis de concentração 0,025 a 0,1 μg mL-1 e 75 ± 9% – 119 ± 12% para os níveis 0,5 a 1 μg mL-1, com relação ao C18 e o biocarvão, respectivamente. O LD no intervalo de 0,01–0,025 e LQ 0,025-0,5 μg mL-1. O método desenvolvido se mostrou adequado para determinação de agrotóxicos em amostras de água.
13

Zkoumání účinku kreatinu v kombinaci s hořčíkem a vitamínem C na výkonost jedince / Investigation of the effect of creatine in combination with magnesium and vitamin C on the performance of the individual person

Vlasák, Jan January 2017 (has links)
Creatine is nitrogen-containing organic acid which naturally occurs in the human body. The aim of this work was to determine the optimal dose of creatine in combination with vitamin C and magnesium for male respondents aged 18-26 years. They were divided into two groups differing in the creatine dosage. Group 1 took smaller dose of creatine (3 g per day) and group 2 higher dose of creatine (10 g per day). Both groups took both magnesium and vitamin C at constant doses throughout the study. The effects of significantly different dose of creatine in the individual groups were compared with each other in terms of the performance of individuals in the powerlifting, the anthropological changes and the overal metabolism of the intakes. In all disciplines of powerlifting, group 1 recorded higher average weight gains, which were not found to be statistically significant at a significance level of alpha 0,05. Anthropological changes were measured using the InBody 160 and a diagnostic measuring tape. In both cases, group 1 recorded better results than group 2, but these results were not statistically significant at a significance level of alpha 0,05. The total metabolism of the accepted dietary supplements was investigated through analytical methods. The urine of each respondent was regularly collected and subsequently analyzed during the research. Determination of creatinine, a creatine waste product, was performed by UV-VIS spectrophotometry using the Jaffe reaction. Vitamin C was analyzed by RP-HPLC. Magnesium was determined by the ICP-OES method. After creatine suplemantion of 3 per day, group 1 showed a slight increase in creatinine in the urine, but still in the physiological range. At the significance level alpha 0,05 there was no statistically significant difference. Group 2 showed an increase above the physiological limit which was already a statistically significant difference. Overall, creatine supplementation of 3 g per day has been found as a sufficient intake of creatine needed to build up muscle mass, increase energy metabolism and overall physical performance. The metabolization itself works very well and within the physiological values.
14

Analyse chimique des matières résineuses employées dans le domaine artistique pré-hispanique au Mexique : application aux échantillons archéologiques aztèque et maya / Chemical analysis of resinous materials employed in artistic pre-hispanic Mexico : application to aztec and maya archaeological samples

Lucero, Paola 14 September 2012 (has links)
Dans le present travail de recherche notre équipe s'est interessé à l'étude de la composition chimique -au niveau moléculaire- d'un groupe d'échantillons résineuses provenant d'objects Aztecs et Mayas. Le but ultime de cette étude a été d'établir l'origin botanique de ces résines et d'avoir une vue d'ensemble des formulations utilisées dans les adhésifs ou les figurines, afin de mieux comprendre leurs propriétes physiques.Pour aboutir à cet objectif une stratégie analytique très spécifique a été créeé et mise en oeuvre. Cette stratégie a inclus l'analyse d'échantillons des résines archéologiques mais aussi de résines d'origine botanique certifiée et de résines commerciales, achetées dans des marchés traditionels au Mexique dans une région qui correspond a la one géographique occupée autre fois par l'empire aztèque.L'étude des matériaux a fait appel à des techniques tels que l'observation a l'échelle microscopique, la spectroscopie infrarouge (IRTF), la chromatographie liquide-DAD (HPLC-UV/Vis) et la chromatographie en phase gazeuse couplée à la spéctroscopie de masse (CPG-SM).L'étude moléculaire de ces échantillons, et plus précisement, l'étude leur fraction tritérpenique a permis de : Établir un profil moléculaire des résines pour chaque origine botanique étudiée Idéntifier précisement certain composées tritérpeniques présents dans toutes les échantillons Réperer les molécules tritérpeniques susceptibles d'être utilisées dans l'avenir comme des marqueurs moléculaires d'origine botanique pour les résines frais des espèces étudiées Suggèrer une origine botanique pour les échantillons archéologiques Aztèques Écarter des origines botaniques possibles pour l'échantillon Maya Avoir une vue d'ensemble de l'origine botanique des résines commercialisées au territoire mexicain sous le nom de «copal» Créer un protocole d'analyse simple pour permettre aux professionnels de la conservation et des biomatériaux d'établir l'origine botanique et un profil moléculaire des résines utilisées dans des expériences diverses Caractériser le comportement du copal lors du vieillisement naturel et artificiel Établir des molécules susceptibles de devenir marqueurs moléculairs pour les deux types de vieillisement Établir que l'origine botanique d'un échantillon résineux peut être retrouvée malgré son âge (archéologique) / In the present work, the molecular composition of series of resinous aztec and maya archaeological samples were investigated to determinate their nature.Thus an analytical strategy was specifically designed. This analytical strategy included the analysis of botanically certified resins, freshly collected. It included as well the analysis of commercial samples bought in Mexican traditional markets.The study of all the samples included microscopical techniques, Fourier Inverse Infrared Spectrometry (FTIR) , High Performance Liquid Chromatography coupled to Ultraviolet-visible spectrometry (HPLC-UV/Vis) and Gas Chromatography coupled to Mass Spectrometry (GC-MS).The molecular study of these samples, in particular of their trterpenic composition allowed to : establish the molecular profile of resins from certified botanical origin. Identifiy some of the triterpenic compounds present in samples; Identify triterpenic molecules that could be uses as molecular markers for each botanical origin. Find the botanical origin of archeological astec samples. Discard possible botanic origins for maya archaeological sample. Have an overview of the origin of commercial samples of mexican copal. Create a simple protocol that allows conservation and biomaterials professionals to establish the botanical origin of archaeological and commercial resins, used in conservation interventions. Observe the behavior of copal materials upon ageing, establishing potential markers for natural ageing in copal, under darkness. Asses the botanical origin of a sample can be found regardless the age of the resin

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