A multi-proxy approach is utilized on mm- to cm-scale laminated sediment records in coastal salt ponds on St. John, U.S. Virgin Islands to characterize the sediments, identify their sources and depositional processes/events (heavy rainfall, tropical cyclones, tsunamis). Historical records are combined with high-resolution geochronology (short-lived radioisotopes, 210Pb, 137Cs, 7Be) and scanning elemental techniques (XRF and LA-ICP-MS) to link depositional events to how they are manifested in the sedimentary record. Volcanic rocks are the terrigenous sediment source and the sedimentary signature of terrigenous sediment in the geologic record consists of higher amounts of Al, Fe, Ti, Co, and Si, and is associated with terrigenous runoff due to rainfall events. A minimum threshold value of >2.0 mm per day (minimum to erode and transport terrigenous sediment downslope) of rainfall has been determined for the study area. The frequency of heavy rainfall events that exceed the threshold of >2.0 mm per day is significantly correlated to the amount of terrigenous sediment accumulation of the terrigenous indictor element Al measured by scanning LA-ICP-MS. There is a robust sedimentary record of terrigenous sediment runoff that is a function of the frequency of heavy rainfall events (exceed threshold). Variability in the sedimentary record reflects changes between periods of "wet" increased frequency of heavy rainfall events and "dry" decreased frequency of heavy rainfall events. Tropical cyclones and tsunamis can cause marine overwash into salt ponds leading to deposition of marine sediments. Elemental scans for Ca and Sr and overwash indicator elements are complicated by grain size effects of LA-ICP-MS techniques, as well the difficulty in differentiating between tropical cyclone overwash deposits and tsunami deposits. By defining the sedimentary signature for depositional events , geologic records can be interpreted to provide insight into the natural variability of these processes throughout geologic time for comparisons to the more recent anthropogenic time period. This study provides a framework that can be applied to other coastal environments on high-relief tropical islands, to compare local records, and provide information on regional processes controlling rainfall variability in tropical latitudes.

The Sardinian Bronze Age (Nuragic period) and the factors which created and maintained an island-wide identity as seen through the presence of its distinctive nuraghi have received considerable attention; however the amount of research directly related to the stone tools of the era has been relatively limited despite the wealth of knowledge it is capable of yielding. This thesis hopes to contribute to Sardinian archaeology through the study of ancient technology, specifically obsidian lithic technology, by combining typological information with source data gleaned from the use of X-ray fluorescence spectrometry (XRF). These data are integrated with statistical analyses breaking down the spatial distribution of nuraghi across the island through the use of distance-based methods, including k-means and kernel density analyses, which create a more comprehensive understanding of the island-wide political and social structure. This research will test the hypothesis that changes in the acquisition of obsidian raw materials were coupled with corresponding changes in how the obsidian was used. The results provide precedence for future work in Sardinia and create a model for integrating two types of analyses, sourcing and typological. By combining these results, it is possible to investigate how obsidian influenced the ancient economy as well as assess its cultural significance for people of the past.

Most urinary tract infections in humans and dogs are caused by uropathogenic strains of , and increasing antimicrobial resistance among these pathogens has created a need for a novel approach to therapy. Bacterial iron uptake and metabolism are potential targets for novel antimicrobial therapy, as iron is a limiting factor in . growth during infection. As a trivalent metal of similar atomic size to iron (III), gallium can interact with a wide variety of biomolecules that normally contain or interact with iron. Gallium compounds disrupt bacterial iron metabolism, are known to accumulate at sites of infection and inflammation in mammals, exert antimicrobial activity against multiple bacterial pathogens in vitro, and may be good candidates as novel antimicrobial drugs. We assessed the suitability of orally administered gallium maltolate as a potential new antimicrobial therapy for urinary tract infections by evaluating its distribution into the bladder, its activity against uropathogenic . in vitro, and its pharmacokinetics and efficacy in a mouse cystitis model. Using a novel application of synchrotron-based analytical methods, we confirmed the distribution of gallium to the bladder mucosa and characterized the relationship between iron and gallium distribution in the bladder. In vitro experiments with human and canine uropathogenic . isolates demonstrated that gallium maltolate exerts antimicrobial effects in a time-dependent, bacteriostatic manner. Minimum inhibitory concentrations ranged from 0.144 µmol/mL to >9.20 µmol/mL with a median of 1.15 µmol/mL. Isolates resistant to ampicillin, ciprofloxacin, or with decreased susceptibility to cephalothin were susceptible to the antimicrobial activity of gallium maltolate, suggesting that resistance to conventional antimicrobials does not predict resistance to gallium maltolate. Pharmacokinetic studies in healthy mice and in a mouse model of urinary tract infection confirmed that gallium is absorbed into systemic circulation after oral administration of gallium maltolate. Gallium is slowly eliminated from the body, with a trend toward longer terminal half-lives in blood and bladder for infected mice relative to healthy mice. This study did not reveal any statistically significant effect of infection status on maximum blood gallium concentrations (4.46 nmol/mL, 95% confidence interval 2.75 nmol/mL – 6.18 nmol/mL and 4.80 nmol/mL, 95% confidence interval 2.53 nmol/mL – 7.06 nmol/mL in healthy and infected mice, respectively) or total gallium exposure in blood and kidney as represented by area under the concentration vs. time curves. Gallium exposure in the bladder was significantly greater for mice with urinary tract infections than for healthy mice. The investigation of gallium distribution within tissues represented a novel application of synchrotron-based analytical techniques to antimicrobial pharmacokinetics. Prior to analysing tissue samples, a library of x-ray absorption spectra was assembled for gallium compounds in both the hard and soft x-ray ranges. The suitability of hard x-ray fluorescence imaging and scanning and transmission x-ray microscopy for localizing and speciating trace elements in tissues was subsequently assessed. Of these methods, only hard x-ray microprobe analysis was well-suited to the analysis and was successfully used for this application. This approach confirmed that gallium arrives at the bladder mucosa after oral administration of gallium maltolate. Furthermore, comparison of iron and gallium distribution within the bladder mucosa indicated that these elements are similarly but not identically distributed and that they do not significantly inhibit one another’s distribution. This finding suggests that gallium may be distributed in part via pathways that do not involve iron. Despite the favorable distribution characteristics of gallium and the persistence of gallium in target tissues following the oral administration of gallium maltolate, its efficacy in a mouse model of urinary tract infection was disappointing. In this study, no statistically significant difference was detected between gallium maltolate, ciprofloxacin and sham treatments in their ability to eliminate bacteria in the urinary tracts. The failure of ciprofloxacin treatment to render bladder tissue culture-negative for an organism that is classified as ciprofloxacin-susceptible in vitro is consistent with observations from other research groups. The similar lack of efficacy observed for gallium maltolate may be related to the large gap between minimum inhibitory concentrations observed in vitro and gallium concentrations observed in tissues from treated mice, but may also be related to the small study size if the effect size of gallium maltolate treatment is small. Given the magnitude of the difference between tissue concentrations and minimum inhibitory concentrations, it may not be possible to increase the dose sufficiently to achieve therapeutic concentrations without causing toxicity. While the results of these experiments suggest that orally administered gallium maltolate may not be a reasonable antimicrobial drug candidate for treating urinary tract infections caused by uropathogenic . , it may be useful for other applications. Other bacterial pathogens may be more susceptible to the antimicrobial effects of gallium maltolate, and local or topical administration could produce much higher concentrations than we observed following oral administration. Continued development of the synchrotron-based analytical techniques used in these experiments could provide new and important opportunities to investigate antimicrobial distribution and metabolism within cells and tissues, particularly for metal-based drugs.

Fundação Carlos Chagas Filho de Amparo a Pesquisa do Estado do Rio de Janeiro / Desde o início do século XX, a poluição do ar nos grandes centros piorou em consequência processo de industrialização e urbanização, juntamente com o rápido crescimento populacional e do transporte motorizado. Algumas espécies de plantas absorvem os poluentes atmosféricos pelas suas folhas e então, fixa-os em sua matriz, tornando-se assim um biomonitor de poluição nessa área. Assim, a análise foliar dessas espécies de vegetal pode ser usado como monitoramento ambiental. Uma das plantas que tem a habilidade de reter certos elementos químicos do ambiente e pode ser usada como biomonitor é a Nerium oleander L.. Neste estudo utilizou-se folhas de Nerium oleander L. para avaliar os níveis de poluição ambiental em uma sub-região da Região Metropolitana do Rio de Janeiro através da Fluorescência de Raios X (EDXRF). O sistema de EDXRF foi desenvolvido no próprio laboratório e consiste de um sistema portátil de XRF formado por um mini tubo raio X de baixa potência (anodo de Ag e operação em 20 kV/50 μA) e um detector de SiPIN. As amostras de Nerium oleander L. foram coletadas de plantas adultas. As amostras foram coletadas durante as quatros estações do ano (verão, outono, inverno e primavera). Todas as folhas foram coletadas a uma distância superior de 1,5 m em relação ao solo. As amostras foram acondicionadas em sacos plásticos e depois da chegada ao laboratório foram colocados sob refrigeração a 5 C. No laboratório, as amostras foram limpas com um pincel com cerdas macias para retirar a poeira. Depois disso, as amostras foram colocadas na estufa a 60 C por 48 h. Em seguida, as amostras foram pulverizadas (44 μm). Depois desse processo, alíquotas de 500 mg de massa foram prensadas a uma pressão de 2.32×108 por cerca de 15 minutos, afim de se obter pastilhas finas com diâmetro de 2,54 cm e densidade superficial de 100 mg/cm2. Foi possível detectar a concentração de 13 elementos: S, Cl, K, Ca, Mn, Fe, Cu, Zn, Br, Rb, Sr, Ba e Pb. A partir da concentração de cada elemento foram obtidos os mapas de distribuição elementar da área de estudo para cada estação. A análise da correlação de Pearson mostrou que existe uma correlação significativa entre os elementos Fe, Zn, Ba e Pb, entre os elementos Ca e Sr e entre os elementos Cl, K, Rb. A análise do PCA (Análise por Componentes Principais) mostrou que existem dois fatores principais da emissão de poluição ambiental: emissão por ressuspensão do solo (Cl, K, Ca, Mn, Rb e Sr) e emissões veiculares e industriais (Fe, Zn, Ba e Pb). O estudo da poluição ambiental através da técnica de EDXRF utilizando folhas de Nerium oleander L. como biomonitor se mostrou uma técnica de baixo custo e eficiência substancial na determinação da concentração elementar dos poluentes atmosféricos. / Since the early 20th century, the air pollution in the great urban areas has worsened as a result of the industrialization and urbanization processes, jointly with the rapid population growth and the motorized transport. Some plants species absorb the air pollutant atmosphere by the leaves and then fixed them in its matrix, thus becoming a biomonitor of pollution in that area. Thus, the foliar analysis of these vegetal species can be used to environmental monitoring. One of the plants that have the ability to retain certain chemical elements in the environmental and it can be used as a biomonitor is the Nerium oleander L.. In this study were used Nerium oleander L. leaves to measure the environmental pollution levels in a sub-region in the Rio de Janeiro Metropolitan Region-Brazil through the X-ray Fluorescence (EDXRF). The EDXRF system was developed in the own laboratory and consist of a portable XRF system formed by a mini X-ray tube of low power (anode of Ag and operated in 20 kV/50 μA) and a SiPIN detector. The samples of Nerium oleander L. were collected from adult plants. The samples were collected during the year seasons (summer, fall, winter and spring). All the leaves were collected at a distance superior of a 1.5 m relative to the soil. The samples were packed in plastic bags and after the arrival in the Laboratory were placed under refrigeration at 5 C. In the laboratory, the samples were cleaned with a brush with soft bristles to remove dust. After that, the samples were placed in the stove at 60 C for 48 h. Next, the leaves were powdered (325 mesh). After this process, aliquots of 500 mg mass were pressed at a pressure of 2.32×108 Pa for about 15 minutes, order to obtain thin pellets with a diameter of 2.54 cm and superficial density of 100 mg/cm2. It was possible to determinate 13 elements concentration: S, Cl, K, Ca, Mn, Fe, Cu, Zn, Br, Rb, Sr, Ba and Pb. From the concentrations of each element were obtained the elemental distribution maps of the studied area in each season. The Pearson's correlation analysis shows a significant correlation between the elements Fe, Zn, Ba and Pb, between the elements Ca and Sr and between the elements Cl, K and Rb. The PCA (Principal Components Analysis) analysis shows that there is two mainly factors of the environmental pollution emissions: emission through the resuspension of the soil (Cl, K, Ca, Mn, Rb and Sr), vehicular and industrial emission (Fe, Zn, Ba and Pb). The study of the environmental pollution using the Nerium oleander L. leaves as a biomonitor proved an inexpensive technique and substantial efficiency in the determination of elements concentration.

Fundação Carlos Chagas Filho de Amparo a Pesquisa do Estado do Rio de Janeiro / Desde o início do século XX, a poluição do ar nos grandes centros piorou em consequência processo de industrialização e urbanização, juntamente com o rápido crescimento populacional e do transporte motorizado. Algumas espécies de plantas absorvem os poluentes atmosféricos pelas suas folhas e então, fixa-os em sua matriz, tornando-se assim um biomonitor de poluição nessa área. Assim, a análise foliar dessas espécies de vegetal pode ser usado como monitoramento ambiental. Uma das plantas que tem a habilidade de reter certos elementos químicos do ambiente e pode ser usada como biomonitor é a Nerium oleander L.. Neste estudo utilizou-se folhas de Nerium oleander L. para avaliar os níveis de poluição ambiental em uma sub-região da Região Metropolitana do Rio de Janeiro através da Fluorescência de Raios X (EDXRF). O sistema de EDXRF foi desenvolvido no próprio laboratório e consiste de um sistema portátil de XRF formado por um mini tubo raio X de baixa potência (anodo de Ag e operação em 20 kV/50 μA) e um detector de SiPIN. As amostras de Nerium oleander L. foram coletadas de plantas adultas. As amostras foram coletadas durante as quatros estações do ano (verão, outono, inverno e primavera). Todas as folhas foram coletadas a uma distância superior de 1,5 m em relação ao solo. As amostras foram acondicionadas em sacos plásticos e depois da chegada ao laboratório foram colocados sob refrigeração a 5 C. No laboratório, as amostras foram limpas com um pincel com cerdas macias para retirar a poeira. Depois disso, as amostras foram colocadas na estufa a 60 C por 48 h. Em seguida, as amostras foram pulverizadas (44 μm). Depois desse processo, alíquotas de 500 mg de massa foram prensadas a uma pressão de 2.32×108 por cerca de 15 minutos, afim de se obter pastilhas finas com diâmetro de 2,54 cm e densidade superficial de 100 mg/cm2. Foi possível detectar a concentração de 13 elementos: S, Cl, K, Ca, Mn, Fe, Cu, Zn, Br, Rb, Sr, Ba e Pb. A partir da concentração de cada elemento foram obtidos os mapas de distribuição elementar da área de estudo para cada estação. A análise da correlação de Pearson mostrou que existe uma correlação significativa entre os elementos Fe, Zn, Ba e Pb, entre os elementos Ca e Sr e entre os elementos Cl, K, Rb. A análise do PCA (Análise por Componentes Principais) mostrou que existem dois fatores principais da emissão de poluição ambiental: emissão por ressuspensão do solo (Cl, K, Ca, Mn, Rb e Sr) e emissões veiculares e industriais (Fe, Zn, Ba e Pb). O estudo da poluição ambiental através da técnica de EDXRF utilizando folhas de Nerium oleander L. como biomonitor se mostrou uma técnica de baixo custo e eficiência substancial na determinação da concentração elementar dos poluentes atmosféricos. / Since the early 20th century, the air pollution in the great urban areas has worsened as a result of the industrialization and urbanization processes, jointly with the rapid population growth and the motorized transport. Some plants species absorb the air pollutant atmosphere by the leaves and then fixed them in its matrix, thus becoming a biomonitor of pollution in that area. Thus, the foliar analysis of these vegetal species can be used to environmental monitoring. One of the plants that have the ability to retain certain chemical elements in the environmental and it can be used as a biomonitor is the Nerium oleander L.. In this study were used Nerium oleander L. leaves to measure the environmental pollution levels in a sub-region in the Rio de Janeiro Metropolitan Region-Brazil through the X-ray Fluorescence (EDXRF). The EDXRF system was developed in the own laboratory and consist of a portable XRF system formed by a mini X-ray tube of low power (anode of Ag and operated in 20 kV/50 μA) and a SiPIN detector. The samples of Nerium oleander L. were collected from adult plants. The samples were collected during the year seasons (summer, fall, winter and spring). All the leaves were collected at a distance superior of a 1.5 m relative to the soil. The samples were packed in plastic bags and after the arrival in the Laboratory were placed under refrigeration at 5 C. In the laboratory, the samples were cleaned with a brush with soft bristles to remove dust. After that, the samples were placed in the stove at 60 C for 48 h. Next, the leaves were powdered (325 mesh). After this process, aliquots of 500 mg mass were pressed at a pressure of 2.32×108 Pa for about 15 minutes, order to obtain thin pellets with a diameter of 2.54 cm and superficial density of 100 mg/cm2. It was possible to determinate 13 elements concentration: S, Cl, K, Ca, Mn, Fe, Cu, Zn, Br, Rb, Sr, Ba and Pb. From the concentrations of each element were obtained the elemental distribution maps of the studied area in each season. The Pearson's correlation analysis shows a significant correlation between the elements Fe, Zn, Ba and Pb, between the elements Ca and Sr and between the elements Cl, K and Rb. The PCA (Principal Components Analysis) analysis shows that there is two mainly factors of the environmental pollution emissions: emission through the resuspension of the soil (Cl, K, Ca, Mn, Rb and Sr), vehicular and industrial emission (Fe, Zn, Ba and Pb). The study of the environmental pollution using the Nerium oleander L. leaves as a biomonitor proved an inexpensive technique and substantial efficiency in the determination of elements concentration.

Neste trabalho são apresentados os procedimentos de caracterização de um sistema comercial portátil de Fluorescência de Raios X por dispersão em energia, o ARTAX 200, bem com seu processo de calibração. O sistema é composto por um tubo de Raios X, com anodo de Molibdênio e um detector XFlash (Silicon Drift Detector) refrigerado por Efeito Peltier. O procedimento de caracterização do sistema foi realizado utilizando-se uma amostra de referência contendo Ferro e Cromo. Foram também usadas amostras certificadas (National Bureau of Standards) D840, D845, D846, D847 e D849 para a realização do processo de calibração do sistema para análise quantitativa. O processo de calibração foi realizado por três metodologias diferentes a fim de avaliar qual deles apresentaria melhores resultados. A caracterização do sistema ARTAX 200 foi realizada executando testes de estabilidade do tubo de Raios X, repetibilidade, reprodutibilidade, resolução em energia do sistema, levantamento da curva de limite de detecção e verificação do centro geométrico do feixe (CG). Os resultados obtidos nos testes de estabilidade apresentaram um coeficiente de variação médio menor do que 2%, o teste de repetibilidade apresentou valores médios menores que 0,5 %. A reprodutibilidade apresentou um coeficiente de variação médio menor que 1,5%. A verificação do centro geométrica mostrou que o CG encontra-se alinhada com o centro ótimo do feixe em duas das três direções do plano cartesiano. A resolução em energia do sistema para a energia de 5,9 keV foi de 150 eV. O limite de detecção apresentou valores menores que 1 % do Si ao Cu. Na avaliação das metodologias para calibração verificou-se que uma das metodologias aplicadas apresentou melhor resultado. Comparando os resultados com outros sistemas portáteis de XRF observa-se que o ARTAX 200 apresenta eficiência superior em relação aos parâmetros analisados. / This paper presents procedures for characterization of a commercial system for portable X-Ray Fluorescence energy dispersive, the ARTAX 200, along with its calibration process. The system consists of an X-ray tube with molybdenum anode and a Silicon Drift Detector XFlash cooled by Peltier effect. The procedure for the characterization of the system was conducted using a reference sample containing Iron Chromium. We also used the certified samples (National Bureau of Standards) D840, D845, D846, D847 and D849 to perform the calibration of the system. The calibration process was conducted by three different methods: Methodology 1, Methodology 2 and Methodology 3, to evaluate them which present better results. The characterization system ARTAX 200 was performed by running stability tests of the X-ray tube, repeatability, reproducibility, resolution in energy of the system, limit of detection and verification of the geometric center of the beam. The results of the stability tests showed an average coefficient of variation of less than 2% repeatability test showed average values lower than 0.5%. The reproducibility showed a coefficient of variation of less than 1.5% which. The verification of the geometric center is aligned with the center of the great beam in two of the three directions of the Cartesian plane. The energy resolution of the system presented to the energy of 5.9 keV a resolution of 150 eV. The detection limit values were less than 1% of the Cu Si. In evaluating methodology for calibrating the best result was obtained with the methodology 3. Comparing the results with other portable XRF systems shows that the ARTAX 200 presents superior efficiency with respect to the parameters analyzed.

Master of Science / Geology / Matthew W. Totten / Organic-rich shales were deposited over a large part of what is now North America during the Late Devonian. North America in the late Devonian was located in the tropics (Woodrow et al., 1973), possibly in low southerly latitudes (Heckel and Witzke, 1979; Witzke and Heckel, 1988; Streel et al., 1990). This environment creates an organic-rich environment that resulted in thick, black shales. The Devonian-Mississippian Chattanooga (Woodford) shale is known to be an important petroleum source rock in many intracratonic basins of the Midcontinent (Lambert, 1993). Geochemical analysis of the Chattanooga shale, using various techniques, provides additional information on oil-source rock potential. Handheld XRF analysis was conducted on well cuttings samples, Loss on Ignition (LOI) was performed on a subset of those samples and mapping of the organic matter results of the two methods was completed. Handheld XRF still has the prospect for providing quick analysis to infer organic matter content to be used as a determination of the quality of source rock. Although slightly reduced correlation has been found within this study compared to Willey (2015), the method has still proven viable for fracking targets to be determined on site and in a more efficient manner. Loss on Ignition results have correlated with TOC data better then XRF results, making this method the better option for evaluating source rock potential. Mapping of these results provide the first known source rock potential map across Kansas and can be used by the industry for future exploration.

Made available in DSpace on 2014-06-11T19:27:17Z (GMT). No. of bitstreams: 0 Previous issue date: 2011-02-11Bitstream added on 2014-06-13T18:31:17Z : No. of bitstreams: 1 sakamoto_ss_me_araca.pdf: 2232778 bytes, checksum: 2d567023e0bd2b444f0d70e7197d8eaf (MD5) / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) / O papel dos elementos traço em tumores mamários tem sido investigado nas últimas décadas, mas comparações de subclasses de tumores mamários malignos são ainda inéditas em medicina veterinária. Portanto, o objetivo do presente trabalho foi identificar a concentração dos elementos cálcio, ferro, cobre e zinco em neoplasias mamárias de cadelas, comparando-se um grupo controle com três tipos histológicos malignos. Cinquenta e uma biopsias mamárias foram avaliadas e divididas em quatro grupos (G1 - controle, G2 - carcinoma complexo, G3 - carcinoma tubular/tubulopapilífero e G4 – carcinoma sólido). O material foi colhido de mastectomias realizadas na rotina do Hospital Veterinário da UNESP-Araçatuba sendo classificado segundo os critérios diagnósticos propostos pela Organização Mundial de Saúde. As amostras foram analisadas, quanto aos elementos traço, pela técnica de Fluorescência de Raios X por Dispersão de Energia (EDXRF). A análise estatística revelou aumento significativo (p<0,05) dos elementos cálcio, ferro e zinco entre os grupos G1 e G2. Comparações entre o sistema TNM (Tumor/Linfonodo/Metástases) e os elementos traço não foram significativas (p˃0,05) à análise estatística, já que os mesmos demonstraram estar correlacionados ao tipo histológico e não ao sistema TNM de prognóstico de vida. O aparelho de EDXRF mostrou-se eficaz para a análise dos elementos traço, além de ser uma técnica mais acessível, multielementar e não destrutiva, permitindo que outras metodologias possam ser utilizadas para estudos complementares com as mesmas amostras / The role of trace elements in breast cancer has been investigated in recent decades, but comparisons of subclasses of malignant mammary tumors are still unpublished in veterinary medicine. So, the aim of this work was to identify the concentration of calcium, iron, cooper and zinc in canine mammary tumors, comparing them with a control group and three malignant neoplasias. 51 mammary fragments of biopsies were analyzed and divided in four groups (G1 – Control, G2 - Complex Carcinomas, G3 – Tubular/Tubulopapillary Carcinoma and G4 – Solid Carcinoma). Samples of the tumors were collected during surgical procedures, mastectomy, performed at Veterinary Hospital of Sao Paulo State University – Araçatuba and were classified according to the diagnostic criteria proposed by the World Health Organization. Samples were analyzed by Energy Dispersive X-Ray Fluorescence Equipment (EDXRF). Statistical analysis revealed a significant difference (p<0.05) only in the groups G1 and G2, concerning to the calcium, iron and zinc elements. The comparison between TNM system and trace elements revealed an absence of statistical evaluation, because trace elements were connected with histopathologycal graduation. The EDXRF was useful for trace element analyses and it is a non-destructive, multielementar technology that permits complementary studies with the same samples

Made available in DSpace on 2014-06-11T19:27:29Z (GMT). No. of bitstreams: 0 Previous issue date: 2010-06-18Bitstream added on 2014-06-13T18:31:46Z : No. of bitstreams: 1 lima_pm_me_botfmvz.pdf: 842879 bytes, checksum: 6d83f475b744d68583fa0fe06786a4aa (MD5) / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) / Universidade Estadual Paulista (UNESP) / No presente trabalho foi feito uma análise qualitativa de cálcio, ferro e zinco em spots de proteínas de amostras de tecido hepático de tilápia do Nilo (Oreochromis niloticus) por Fluorescência de Raios-X de Radiação Síncroton, após a separação das proteínas por Eletroforese Bidimensional em Gel de Poliacrilamida (2D-PAGE). Os espectros de fluorescência obtidos indicaram a presença de cálcio, ferro e zinco em doze, seis e oito spots protéicos das amostras de fígado, respectivamente. Os íons metálicos detectados nas amostras estão distribuídas principalmente em proteínas de massa molar menor que 45 kDa e com pI na faixa de 4,5 a 9,0. Além do cálcio, ferro e zinco foram detectados a presença de enxofre e fósforo, elementos não metálicos, que podem ser constituintes da estrutura das proteínas. As concentrações de cálcio, ferro e zinco ligados às proteínas foram determinadas por FAAS após a mineralização ácida dos spots protéicos, encontrando-se concentrações na faixa de 1,08 a 5,80 mg g-1, 2,02 a 8,03 mm g-1 e 1,60 a 8,55 mg g-1, respectivamente / An investigation was made into calcium, iron and zinc in protein spots in samples of Nile tilapia (Oreochromis niloticus) liver tissue obtained after protein separation by two-dimensional polyacrylamide gel electrophoresis (2D-PAGE) and subsequent qualitative and quantitative evaluation by synchrotron radiation X-ray fluorescence (SRXRF) and graphite furnace atomic absorption spectrometry (FAAS). An analysis of the fluorescence spectra indicated the presence of calcium, iron and zinc in twelve, six and eight liver protein spots, respectively. The metal ions found were distributed mainly in proteins with a molar mass of less than 40.00 kDa and more than 12.00 kDa, with pI in the range of 4.70 to 9.40. The only exception was a spot presenting protein with a molar mass of 10.10 kDa. In addition to calcium, iron and zinc, sulfur and phosphorus – which are non-metals that may be part of the protein structure, were also detected. After microwave-assisted acid mineralization of the proteins spots, a FAAS estimation of the concentration of calcium, iron and zinc bound to these proteins indicated a range of 1.08 to 5.80 mg g-1, 2.02 to 8.03 mg g-1 e 1.60 to 8.55 mg g-1, respectively

Made available in DSpace on 2014-10-09T12:38:44Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:00:08Z (GMT). No. of bitstreams: 1 06003.pdf: 11473213 bytes, checksum: 759e2030493408079cad31ae3d3dd261 (MD5) / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP