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Há na literatura um grande número de publicações versando sobre métodos analíticos para a determinação de razões isotópicas através das mais diversas modalidades de espectrometria. Entretanto, praticamente todos esses métodos possuem umarestrição comum em relação à gama de íons moleculares que podem ser utilizados nessas determinações: eles devem ser, ou íons elementares, ou íons cujo único átomo poli-isotópicoé o elemento de interesse. Isto é obtido, ou mediante adestruição das moléculas da amostra, ou complexos tratamentosquímicos para a obtenção de espécies poli-atômicas adequadas.Neste trabalho, foi desenvolvido um método matemático capazde deconvolver o padrão isotopomérico de um íon molecular,isto é, calcular os padrões isotópicos dos átomos que ocompõem dados a sua fórmula elementar e o seu espectro .A principal contribuição de um método desse tipo é a ampliaçãoda variedade de espécies químicas e modalidades de espectrometria aceitáveis para análises isotópicas. O algoritmo desenvolvidofoi caracterizado através da sua aplicação a um grande númerode espectros simulados visando modelar a resposta do métodoquando submetido a algumas imperfeições experimentais típicasde espectrometria e relevantes para análises isotópicas,tais como ruído, discriminação instrumental de massas, nãolinearidade de detecção, falta de resolução e má compensaçãode espectral. Os resultados obtidos permitiram concluirque, ao contrário do que o senso comum às vezes possa sugerir,determinações isotópicas realizadas através de espéciespoli-atômicas podem, muitas vezes, ser mais exatas e precisasque as efetuadas pelas abordagens convencionais. Concluiu-seque, de maneira geral, os resultados tendem a ser tantomelhores quanto maior for o número de instâncias do elementode interesse na fórmula do íon molecular escolhido. Foiestudada experimentalmente a viabilidade de métodos analíticosde equilibração para determinações de razões isotópicashidrogênio/deutério em amostras aquosas utilizando polióiscomo sondas e espectrometria com ionização electrospray.Os polióis testados foram o manitol, o ácido glucônico,a glucosamina e a N-metilglucamina (através do seu complexocom o ácido bórico). Os resultados obtidos mostraram algunsdesvios sistemáticos que sugerem que haja troca parcialde hidrogênios não lábeis dos polióis na fase gasosa, oque impossibilitaria esta aplicação. Sondas aternativasaos polióis são propostas. / Several articles can be found in the literature describing methods forthe determination of isotopic ratios through the various modalities ofmass spectrometry. However, almost all of them have a commonrestriction on the type of molecular ion that can be employed in thesedeterminations: they must be either elemental ions, or polyatomic ionswhose sole polyisotopic element is the one being analysed. This isusually achieved through the destruction of the molecules, or throughcomplex synthetic procedures. In this work, a mathematical methodcapable of deconvolving the isotopomeric pattern of a molecular ion,i.e., calculating the isotopic pattern of its constituent atoms givenits formula and its mass spectrum, has been developed. The maincontribution of such a method to the field is the broadening of therange of acceptable chemical species for isotopic analyses. Thedeveloped algorithm was characterized by applying it to a large numberof simulated spectra with the objective of modelling its response tosome experimental imperfections common to mass spectrometry andrelevant for isotopic analyses, such as noise, instrumental massdiscrimination, detection non-linearity, lack of resolution and badbaseline compensation. The results allowed us to conclude that, inspite of whatever commonsense might suggest, isotopic analysescarried out through the polyatomic approaches can, in many cases, bemore exact and precise than those performed through conventionalapproaches. It could also be concluded that, in general, the largerthe number of instances of the element of interest in the formula ofthe chosen ion, the better the results become. Also as part of theproject, the viability of employing polyols as probes for thehydrogen/deuterium ratio in aquous samples in equilibration methodsand electrospray mass spectrometry has been studied. The studiedpolyols were: manitol, gluconic acid, glucosamine and N-metilglucamine(through its complex with boric acid). The obtained results showedsome systematic errors that suggest that there might be a partialexchange of non-labile hydrogen atoms during the electrosprayphenomenon. Alternative probes are proposed.

Vários complexos intrusivos de rochas alcalinas e carbonatitos ocorrem na região centro-oeste de Moçambique e estão intimamente relacionados ao Sistema do Rifte da África Oriental. Correspondem a atividades ígneas anorogênicas e cortam o embasamento pré-Cambriano da Cadeia Moçambicana. Destes, foram estudadas algumas amostras de seis complexos carbonatíticos (Xiluvo, Muambe, Muande, Fema, Rio Mufa e Evate) e três sieníticos (Chiperone, Tumbine e Salambidua). Os carbonatitos são caracterizados por uma grande predominância de carbonatos, mais apatita, flogopita e raramente anfibólio. O de Xiluvo apresenta, além disso, minerais típicos de terras raras e pirocloro. O sienito de Chiperone tem como constituinte principal nefelina, enquanto que os dois restantes são compostos essencialmente, de K-feldspatos pertíticos. Todos têm como componentes subordinados anfibólios, piroxênio, biotita e apatita. Idades K-Ar das rochas sieníticas, obtidas em anfibólio e biotita, por volta de 118 Ma, apontam o Cretáceo Inferior como período decolocação dos sienitos de Tumbine e Salambidua, enquanto que o sienito de Chiperone resultou muito mais antigo, com aproximadamente 450 Ma. Estes valores confirmam idades radiométricas anteriores, relacionadas com a Província de Chilwa em Malawi. Dados litogeoquímicos destacam dois grupos distintos entre as amostras dos carbonatitos estudadas. Xiluvo, Muambe e Evate situam-se no campo dos carbonatitos cálcicos, enquanto que Fema, Muande e Rio Mufa situam-se no campo dos carbonatitos ferromagnesianos. Os padrões de distribuição de elementos menores e de terras raras são similares àqueles definidos para diversas ocorrências congêneres. Foi analisada também, por comparação, uma amostra carbonática do mármore de Chíduè, tirando a amostra de Chíduè a qual mostrou-se quimicamente diferente, com concentrações muito baixas em praticamente todos elementos. Por outro lado as amostras do Xiluvo exibem os mais elevados teores na maior parte dos elementos. Quanto à geoquímica isotópica, os carbonatitos exibem uma correlação negativa no diagrama 87Sr/86Sr vs. Nd(0) e indicam a existência de pelo menos dois tipos de fontes. Uma delas, correspondendo aos complexos de Xiluvo e Muambe, com 87Sr/86Sr de cerca de 0.703 e Nd com valores positivos, poderia ser astenosférica. A outra fonte, relativa aos demais complexos, apresenta valores negativos de Nd entre (-4) e (-8), e valores moderadamente elevados de 87Sr/86Sr, entre 0.705 e 0.708. A interpretação dos dados geoquímicos isotópicos levou à hipótese de misturas de fontes mantélicas diferentes, bem como possibilidades de contaminação crustal. / Several Syenitic and carbonatitic alkaline complexes occur in central-western region of Mozambique and are related to the East African Rift System. They correspond to anorogenic igneous activities and intrude the Precambrian basement of the Mozambique belt. Of these, six carbonatites (Xiluvo, Muambe, Muande, Fema, Rio Mufa and Evate) and three syenites (Chiperone, Tumbine and Salambidua) were studied. The carbonatites exhibit a great predominance of carbonates, plus apatite, phlogopite and some amphibole. Xiluvo, Muambe and Rio Mufa in addition, include typical minerals of REE and pyrochlore. The Chiperone syenite exhibits nepheline as the main constituent, while the two other are mainly composed of perthitic K-feldspar. All them present amphibole, pyroxene, biotite and apatite as subordinate constituents. K-Ar ages for the Tumbine and Salambidua syenites, obtained in amphibole and biotite, with around 118 Ma, indicate the Lower Cretaceous as the period of placement. However, the Chiperone syenite yielded a much older age around 450 Ma. These values are compatible with earlier radiometric dates, related to the Chilwa Ineous Province of Malawi. On lithogeochemistry, two groups can be envisaged within the carbonatites. One of them includes the calcium carbonatites of Xiluvo, Muambe end Evate, and the other includes the ferromagnesian carbonatites of Fema, Muande and Rio Mufa. The distribution patherns of trace and REE elements are similar to those of normal carbonatites. A sample of the Chíduè marmor was also analyzed, for comparison, and yielded much lower concentrations for most elements. On the other hand, the Xiluvo samples yielded the highest contents for practically all trace and REE elements. The carbonatites exhibit a negative correlation in the 87Sr/86Sr vs. 143Nd/144Nd diagram, and indicate the existence of at least two different sources. One of them, corresponding to the Xiluvo and Muambe complexes, yielded 87Sr/86Sr values around 0.703 and positive Nd, indicating a possible astenospheric source. The second source, for the other complexes, presents negative values of Nd between (-4) e (-8) and moderately high values of 87Sr/86Sr between 0.705 and 0.708. The interpretation of the geochemical isotopic data leads to the hypothesis of mixtures of mantles sources, as well as some possibility of crustal contamination.

Orientador: Roberto Perez Xavier / Dissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Geociencias / Made available in DSpace on 2018-07-25T00:05:32Z (GMT). No. of bitstreams: 1 Silva_GilbertodeLimaPereira_M.pdf: 4720997 bytes, checksum: 8740815167ddd2826e2cd76a34789793 (MD5) Previous issue date: 1998 / Resumo: Litotipos carbonosos comumente hospedam ou ocorrem associados a mineralizações auríferas filoneanas nos depósitos mesotermais da Fazenda Canto (FC) e Fazenda Maria Preta (FMP), na seqüência Paleoproterozóica do Greenstone Belt do Rio Itapicuru, NE Brasil. Nestes depósitos, a matéria carbonácea (MC) ocorre principalmente como: (i) bandas retas a anastomosadas (Tipo I); (ii) grãos individuais compostos por agregados de sub-grãos altamente anisotrópicos (Tipo II); ou (iii) grãos individuais com textura interna homogênea (Tipo III). Estudos de espectroscopia Raman indicaram que estes tipos de MC correspondem a alguma forma de material grafítico microcristalino desordenado e definem um trend de grafitização do depósito FMP para o depósito FC, que é interpretado como sendo o resultado de diferentes graus de maturação da MC, que foi alcançado durante o metamorfismo regional no fácies xisto-verde e o alojamento de corpos graníticos no Greenstone Belt do Rio Itapicuru. Estudos de inclusões fluidas revelaram que os veios de quartzo mineralizados são dominados por populações de inclusões ricas em CO2 (Tipo 1), contudo grupos de inclusões H2OCO2 (Tipo 2) primárias, de baixa salinidade (<5% eq. NaCl), compreendem o tipo de inclusões dominantes em apenas alguns veios. Ambos os tipos de fluidos mineralizantes podem ser interpretados como parte de um sistema hidrotermal magmático-metamórfico profundo. No depósito FC, o geotermômetro da clorita (variedade ripidolita - limite inferior) e a paragnese sulfetada (arsenopirita-pirita-pirrotita - limite superior) indicaram limites de temperatura para a deposição do ouro entre 390ºC e 491ºC, com pressões estimadas entre 2.4 a 4.6 kbars, respectivamente. A MC do depósito FMP é isotopicamente mais leve (g13C= -23.3 0/00 a -30.8 0/00) do que a MC do depósito FC (g13C= -18.5 0/00 a -21.0 0/00) Estes valores de g 13C, juntos com as evidências geológicas apontam uma origem biogênica orgânica para a MC. Os composição de g13C calculada do CO2 derivado da oxidação ou hidrólise da MC, aplicando o equilíbrio isotópico calcita-grafita, produziu valores de g13C no intervalo de -9.3 °/00 a -12.8 °/00 entre 390°C e 491°C. Estes valores de 813C calculados são menores do que aqueles obtidos Rara carbonatos do depósito FC (-4.8 °/00 a -8.9 °/00). Por outro lado, os valores da composição de g13C calculada de CO2 de paleo-fluidos responsáveis pela formação de carbonatos (calcita-ankerita), aplicando o equilíbrio calcita-CO2, produziu valores no intervalo de -2.3 °/00 a -6.6 °/00 para temperaturas entre 390°C e 491°C. Estes valores de g13C calculados são compatíveis com o intervalo obtido para inclusões fluidas do depósito FC (-2.8 °/00 a 4.9 °/00) e confirmam que os minerais de alteração de carbonato foram formados pela ação de fluidos oriundos de fonte magmática ou metamórfica profunda. O processo de maturação termal da MC contribuiu pouco para mudanças na composição química e isotópica do fluido mineralizante. Com relação à deposição do ouro, a MC provavelmente atuou como: (1) uma barreira química, reduzindo a 102 do fluido mineralizante ou promovendo a imiscibilidade do fluido pela adição de pequenas quantidades de CH4 e N2 à fase fluida; elou (2) uma barreira física, adsorvendo ouro sobre sua superfície como carvão ativado. Adicionalmente, a MC pode ser usada como um guia indireto na prospeção de mineralizações auríferas / Abstract: Carbonaceous units commonly host or occur closely related to the lode-gold mineralization in the mesothermal Fazenda Canto (FC) and Fazenda Maria Preta (FMP) deposits of the Paleoproterozoic Rio Itapicuru Greenstone Belt, northeast Brazil. In these deposits, the carbonaceous matter (CM) occurs mainly as: (i) straight to anastomosing seams (Type I); (ii) single grains composed of an agglomerate of highly anisotropic subgrains (Type 11); or (iii) single grains with an homogeneous internar texture (Type III). Raman spectral characteristics indicated that these types of CM correspond to some form of microcrystalline disordered graphitic material and define a graphitization trend from the FMP to the FC deposit, which is interpreted as being the result of different degrees of thermal maturation of the CM that was attained during the regional greenschist metarnorphisrn and granite intrusions of the Rio Itapicuru Greenstone Belt. Fluid inclusion studies revealed that the mineralized quartz veins are dominated by populations of CO2-rich inclusions (Type 1), whereas primary groups of low salinity (< 5 wt% eq. NaCl) H2O-CO2 (±CH4 ± N2) inclusions (type 2) comprise the dominant inclusion type in only a few veins. Both types of mineralizing fluids may be interpreted as part of a deep metamorphic - magmatic hydrothermal system. In the FC deposit, chlorite (ripidolite variety - lower limit) geothermometer and sulfide assemblage (arsenopyrite-pyrite-pyrrhotite - upper limit) indicated a temperature of gold deposition between 390 °C to 491°C with estimated pressures of 2.4 to 4.6 kbars, respectively. The CM of the FMP deposit is isotopically lighter (g13C= -23.3 0/00 to -30.8 0/00) than the CM of the FC (g13C= -18.5 0/00 to -21.0 0/00) These g13C values, together with the geologie evidence, point towards a primarily biogenic organic origin for the CM. The calculated g13C compositions of CO2 derived by the oxidation or hydrolysis of the CM, applying the equilibrium calcite - graphite fractionation, yield g13C values in the range -9.3 0/00 to -12.8 0/00 at 390°C 491ºC. These calculated g13C values are lower than those obtained from carbonates of the FC deposit (-4.8 0/00 to -8.9 0/00). On the other hand, the calculated g13C compositions of CO2 from paleo fluids responsable bicarbonate (calcite-ankerite) formation, applying the equilibrium calcite - CO2 fractionation, yield g13 C values in the range -2.3 0/00 to -6.6 0/00 at 390°C ¿ 491ºC. These calculated g13C values are compatible with the range obtained from fluid inclusions of the FC deposit (-2.8 0/00 to -4.9 0/00) and insure that carbonate alteration minerals were formed by action of fluids from a magmatic or deep metamorphic source. The thermal maturation process of the CM contributed little to changes in the chemistry and isotopic composition of the mineralizing fluid. Regarding gold deposition, the CM is likely to have acted as: (1) a chemical trap, reducing the fO2 of the mineralizing paleo-fluids or enhancing fluid immiscibility by adding small quantities of CH4 and N2 to the fluid phase; and/or (2) a physical barrier, adsorbing gold on its surface as activated carbon. Addictionally the CM may be used as a indirect guide in surveys for gold mineralization / Mestrado / Metalogenese / Mestre em Geociências

Nearshore marine habitats provide critical nursery grounds for juvenile fishes, but their functional role requires the consideration of the impacts of spatial connectivity. This thesis examines nursery function in seagrass habitats through a marine landscape (“seascape”) lens, focusing on the spatial interactions between habitats, and their effects on population and trophic dynamics associated with nursery function to rockfish (Sebastes spp.). In the temperate Pacific Ocean, rockfish depend on nearshore habitats after an open-ocean, pelagic larval period. I investigate the role of two important spatial attributes, habitat adjacency and complexity, on rockfish recruitment to seagrass meadows, and the provision of subsidies to rockfish food webs. To test for these effects, underwater visual surveys and collections of young-of-the-year (YOY) Copper Rockfish recruitment (summer 2015) were compared across adjacent seagrass, kelp forest, and sand habitats within a nearshore seascape on the Central Coast of British Columbia. Recruitment was positively influenced by the structural complexity of seagrass and adjacency to kelp forest sites, however a negative interaction between seagrass complexity and kelp forest adjacency suggests that predation modifies Copper Rockfish recruitment densities. In addition, using δ13C and δ15N isotopes to determine the basal contributions to seagrass food webs, kelp-derived nutrients were on average 47% ± 0.4 of YOY Copper Rockfish diets, which was 3x and 67x greater than the contribution of autochthonous seagrass production (seagrass epiphyte and seagrass blades, respectively). YOY Copper Rockfish diets in seagrass adjacent to sand habitats had the greatest amounts of kelp-derived nutrients and harpacticoid copepods, and concurrently had lower body condition compared to rockfish in the seagrass kelp edges and interior, feeding predominantly on seagrass epiphytes and calanoid copepods. This thesis provides further evidence that temperate seagrasses are nurseries for rockfish and that spatial elements of seascapes, including connectivity via habitat adjacency and variability in habitat structure, alter the recruitment and diets of rockfish in seagrass habitats. These seascape nursery effects are important considerations for marine planning, especially given the global decline of nearshore habitats. / Graduate

Feeding ecology of organisms has a critical influence on ecosystem structure, function, and stability, but how feeding ecology of a single organism varies over multiple spatial and temporal scales in nature is unknown. Here, I characterize the factors driving and the implications of variability in feeding ecology of juvenile Chinook Salmon (Oncorhynchus tshawytscha) over multiple spatial and temporal scales using stable isotopes and stomach contents. Significant variation in juvenile Chinook salmon feeding ecology at the individual-level was found to occur off of the west coast of Vancouver Island (WCVI) (British Columbia, Canada). This variation is correlated with a diet shift from feeding on invertebrates to feeding on fish, as the salmon increase in size. I developed a novel Bayesian stable isotope method to model this shift while taking into account the time-lag associated with isotopic turnover. I found that this model was able to replicate patterns seen in a simplified coastal food web, and that resource-use estimates from this stable isotope model somewhat diverged from a compilation of stomach content data. Next, I compared the feeding ecology of Chinook Salmon in one season and year along nearly their entire North American range. I found considerable spatial variation in ontogeny and feeding ecology, with individuals of the same size from different geographic regions having different δ13C, δ15N, and trophic levels. These differences likely corresponded to regional variability in sea surface temperature, ocean entry date and size, and growth rates. Subsequently, I quantified temporal shifts in the feeding ecology of Chinook Salmon from WCVI. I found that feeding ecology over winter was different from feeding ecology in the fall, and that this likely corresponds to shifts in the prey field. Finally, I found that WCVI juvenile Chinook Salmon showed significant interannual variability in feeding ecology, and that the interannual variability in the δ13C value of juvenile salmon (indicative of primary productivity or nutrient source) predicts their smolt survival. In turn, large-scale climate variability determines the δ13C values of salmon—thus mechanistically linking climate to survival through feeding ecology. These results suggest that qualities propagated upwards from the base of the food chain have a cascading influence that is detectable in salmon feeding ecology. I conclude that the feeding ecology of juvenile Chinook Salmon varies on individual, spatial, season and interannual scales, and that this variability has impacts on survival rates. These findings have implications for the understanding of ontogeny in natural systems in general, allowing for modelling of ontogeny in previously intractable ecological systems. Furthermore there may also be implications for Chinook Salmon management, considering that feeding ecology showed utility as a mechanistic leading indicator of survival rates. / Graduate

PANcreatic DERived factor (PANDER, FAM3B) is a member of a superfamily of FAM3 proteins that are uniquely structured and strongly expressed from the endocrine pancreas and co-secreted with insulin. Unique animal models available to our lab have indicated that PANDER can induce a selective hepatic insulin resistant (SHIR) phenotype whereby insulin signaling is blunted yet lipogenesis is increased. The complexity of the biological networks involved with this process warranted the logical approach of employing quantitative mass spectrometry based proteomic analysis using stable isotope labeling of amino acids in cell culture (SILAC) to identify the global proteome differences between the PANDER transgenic (TG) overexpressing murine model to matched wild-type mice under three metabolic states (fasted, fed and insulin stimulated). Additionally, this technique was used to compare the hepatic proteome of mice on a high fat diet to elucidate early and late mechanisms of disease progression. The “spike-in” process was employed by equal addition of lysate obtained from livers of heavy L-Lysine (13C6, 97%) fed mice to the mice liver protein lysate (PANTG and WT) for relative quantitative analysis. Upon acquisition of the dataset by use of liquid chromatography tandem mass spectrometry (LC-MS/MS, LTQ Orbitrap), geometric means and Uniprot Protein identification numbers were uploaded to Ingenuity Pathway Analysis (IPA) to reveal the effect of PANDER on hepatic signaling. IPA identified lipid metabolism and fatty acid synthesis as top cellular functions differentially altered in all metabolic states. Several molecules with a role in lipid metabolism were identified and include FASN, ApoA1, ApoA4, SCD1, CD36, CYP7A1 and ACC. Furthermore, central to the differentially expressed proteins was the revealed activation of the liver X receptor (LXR) pathway. In summary, our SILAC proteomic approach has elucidated numerous previously unidentified PANDER induced molecules and pathways resulting in increased hepatic lipogenesis. In addition, we have demonstrated strong utility of this approach in comprehensively phenotyping animal models of hepatic insulin resistance. PANDER may potentially propagate pro-hepatic lipogenic effects by LXR activation in contrast to increased LXRα expression. This can be evaluated through the use of LXR agonists (T0901317) antagonists (GSK 2033). LXR activity can be measured by luciferase assays using an LXRE response plasmid. Our central hypothesis is that PANDER induces activation of LXR and is measured and predicted in our line of experiments. In general, PANDER induced LXR activation will be enhanced by T0901317 and diminish effects of GSK 2033 along with direct correlation of downstream metabolic effects such as increased hepatic lipogenesis and fatty acid metabolism. Taken together, PANDER strongly impacts hepatic lipid metabolism and may induce a SHIR phenotype via the LXR pathway. Additionally, phosphoproteomic analysis uncovered large-scale differences in protein phosphorylation states as PANDER impacts insulin signaling. A notable finding was the increased phosphorylation of glycogen synthase (GSK), possibly responsible for the decreased hepatic glycogen content in the PANTG mouse. In an effort to map out critical molecules involved in non-alcoholic fatty liver disease (NAFLD) pathogenesis, the same proteomic approach was carried out, providing a unique dataset of differentially expressed hepatic proteins due to a high at diet.