Nesse trabalho foi realizado um estudo da atividade anti-radicalar de flavonóides frente ao ensaio com o sistema luminol/hemina/H2O2 desenvolvido por nosso Grupo de Pesquisa. Na tentativa de esclarecer a relação estrutura-atividade de flavonóides, foi realizada também uma investigação das propriedades de derivados fenólicos como compostos-modelo utilizando-se a reação quimiluminescente do luminol. Os resultados obtidos com os compostos-modelo com o ensaio luminol foram comparados com aqueles obtidos para estes aditivos em um ensaio que utiliza o radical estável DPPH como sonda. Além disso, foi realizado um estudo fitoquímico monitorado através da atividade anti-radicalar de extratos de Baccharis. Foram identificados dois componentes ativos da fase em acetato de etila obtida das folhas de Baccharis regnellii e a sua atividade anti-radicalar determinada. / In this work a systematic study on the antiradical activity of flavonoids was performed, using the assay luminol/hemin/H2O2 developed by our research group. With the objective to establish a structure activity relationship for flavonoids, a study on the antioxidant properties of several phenolic derivatives as model compounds was also performed, using luminol chemiluminescence. The results obtained with the model compounds from the luminol assay are compared to those obtained by an assay which utilizes the stable DPPH radical as probe. Furthermore, a phytochemical study, monitored by the antiradical activity, was performed on extracts of Baccharis. This study led to the identification of two active components in the ethyl acetate phase of Baccharis regnellii leafs and the determination of its antiradical activity.

A exposição excessiva às radiações UV é capaz de limitar a capacidade dos sistemas de defesa antioxidante em nosso organismo, provocando o estresse oxidativo. Assim, extratos vegetais ricos em compostos antioxidantes são fortes candidatos a serem veiculados em formulações tópicas para a prevenção ou tratamento dos danos causados pela RUV na pele. Dentre a gama de extratos vegetais com atividade biológica, o extrato de açaí, fruto da espécie Euterpe olerecea Mart., tem se destacado por apresentar grande quantidade de antioxidantes na sua composição. Geralmente, a quantidade de ativos que consegue penetrar na pele é pequena, exigindo métodos analíticos muito sensíveis. Assim, o presente trabalho teve como objetivo avaliar o emprego do método de quimioluminescência para a quantificação da penetração dos componentes do extrato de açaí na pele por medida da atividade antioxidante. Os resultados mostraram que o IC50 do extrato de açaí para o ensaio de inibição da quimioluminescência gerada no sistema xantina/luminol/xantina oxidase foi de 0,63 ?g/mL. Além disso, a quantificação do extrato de açaí utilizando esse método foi possível para porcentagens de inibição obtidas até o valor de 60%. Ainda, esse método mostrou-se preciso e exato na determinação da porcentagem de inibição da quimioluminescência do extrato de açaí na concentração próxima a IC50, sendo essa inibição não influenciada pelos componentes das diferentes formulações estudadas. No entanto, o uso da quimioluminescência como um método de quantificação da penetração de componentes antioxidantes de extratos hidrossolúveis torna o processo de extração desses componentes da pele um fator importante, no qual a escolha do solvente extrator é um ponto crítico. Assim, o solvente extrator escolhido para a realização dos estudos de penetração/retenção cutânea foi metanol:água (80:20), visto que esse solvente foi capaz de extrair os componentes antioxidantes do extrato de açaí sem retirar grande quantidade dos compostos inerentes da pele com atividade antioxidante. Por fim, a determinação da inibição da quimioluminescência gerada no sistema xantina/luminol/xantina oxidase mostrou-se um método importante na medida da atividade antioxidante de extratos na pele. Ainda, esse método foi eficaz na quantificação do extrato de açaí nos estudos de penetração/retenção com célula de difusão vertical, apesar de todos os erros inerentes desse método. / The excessive exposure to UV radiation is able to decrease the antioxidant defense systems in the skin leading to the oxidative stress. Thus, plant extracts, rich in antioxidant compounds, are strong candidates to be added in topical formulations for the prevention or treatment of UV radiation induced damages. Among the range of plant extracts with biological activity, the extract of açai, fruit of the Euterpe olerecea Mart. species has become known due to the considerable amount of antioxidants in its composition. Generally, the amount of active compounds that can penetrate in the skin is low requiring sensitive analytical methods. Thus, the present study aimed to evaluate the use of chemiluminescence assay for the quantification of the penetration of açai extract components in the skin by measuring the antioxidant activity. The results showed an IC50 value of 0.63 ?g/mL for the antioxidant activity determined by chemiluminescence assay using the xanthine/luminol/xanthine oxidase system. Moreover, the quantification of acai extract using this method was possible for percentages of inhibition obtained until the 60% of inhibition value. Additionally, this method proved to be precise and accurate in determining the percentage of chemiluminescence inhibition of acai extract at concentrations values close to the IC50 value. Additionally, it was observed that the inhibition was not influenced by the different components of the formulations studied. However, the use of chemiluminescence assay to quantify the penetration of water-soluble extract antioxidant components makes the extraction process of these components from the skin an important step in which the selection of the extractor solvent is a critical point. In the present study it was selected methanol:water (80%) as an organic extractor solvent which was able to extract the antioxidant components of the acai extract without removing large amounts of inherent compounds of the skin with antioxidant activity. Finally, the determination of the chemiluminescence generated in the xanthine/luminol/xanthine oxidase system inhibition showed to be an important method for the measurement of the antioxidant activity of plant extracts in the skin. Still, this method was effective in quantifying the acai extract in cutaneous penetration/retention studies using vertical diffusion cells despite all the intrinsic errors of this used method.

A exposição excessiva às radiações UV é capaz de limitar a capacidade dos sistemas de defesa antioxidante em nosso organismo, provocando o estresse oxidativo. Assim, extratos vegetais ricos em compostos antioxidantes são fortes candidatos a serem veiculados em formulações tópicas para a prevenção ou tratamento dos danos causados pela RUV na pele. Dentre a gama de extratos vegetais com atividade biológica, o extrato de açaí, fruto da espécie Euterpe olerecea Mart., tem se destacado por apresentar grande quantidade de antioxidantes na sua composição. Geralmente, a quantidade de ativos que consegue penetrar na pele é pequena, exigindo métodos analíticos muito sensíveis. Assim, o presente trabalho teve como objetivo avaliar o emprego do método de quimioluminescência para a quantificação da penetração dos componentes do extrato de açaí na pele por medida da atividade antioxidante. Os resultados mostraram que o IC50 do extrato de açaí para o ensaio de inibição da quimioluminescência gerada no sistema xantina/luminol/xantina oxidase foi de 0,63 ?g/mL. Além disso, a quantificação do extrato de açaí utilizando esse método foi possível para porcentagens de inibição obtidas até o valor de 60%. Ainda, esse método mostrou-se preciso e exato na determinação da porcentagem de inibição da quimioluminescência do extrato de açaí na concentração próxima a IC50, sendo essa inibição não influenciada pelos componentes das diferentes formulações estudadas. No entanto, o uso da quimioluminescência como um método de quantificação da penetração de componentes antioxidantes de extratos hidrossolúveis torna o processo de extração desses componentes da pele um fator importante, no qual a escolha do solvente extrator é um ponto crítico. Assim, o solvente extrator escolhido para a realização dos estudos de penetração/retenção cutânea foi metanol:água (80:20), visto que esse solvente foi capaz de extrair os componentes antioxidantes do extrato de açaí sem retirar grande quantidade dos compostos inerentes da pele com atividade antioxidante. Por fim, a determinação da inibição da quimioluminescência gerada no sistema xantina/luminol/xantina oxidase mostrou-se um método importante na medida da atividade antioxidante de extratos na pele. Ainda, esse método foi eficaz na quantificação do extrato de açaí nos estudos de penetração/retenção com célula de difusão vertical, apesar de todos os erros inerentes desse método. / The excessive exposure to UV radiation is able to decrease the antioxidant defense systems in the skin leading to the oxidative stress. Thus, plant extracts, rich in antioxidant compounds, are strong candidates to be added in topical formulations for the prevention or treatment of UV radiation induced damages. Among the range of plant extracts with biological activity, the extract of açai, fruit of the Euterpe olerecea Mart. species has become known due to the considerable amount of antioxidants in its composition. Generally, the amount of active compounds that can penetrate in the skin is low requiring sensitive analytical methods. Thus, the present study aimed to evaluate the use of chemiluminescence assay for the quantification of the penetration of açai extract components in the skin by measuring the antioxidant activity. The results showed an IC50 value of 0.63 ?g/mL for the antioxidant activity determined by chemiluminescence assay using the xanthine/luminol/xanthine oxidase system. Moreover, the quantification of acai extract using this method was possible for percentages of inhibition obtained until the 60% of inhibition value. Additionally, this method proved to be precise and accurate in determining the percentage of chemiluminescence inhibition of acai extract at concentrations values close to the IC50 value. Additionally, it was observed that the inhibition was not influenced by the different components of the formulations studied. However, the use of chemiluminescence assay to quantify the penetration of water-soluble extract antioxidant components makes the extraction process of these components from the skin an important step in which the selection of the extractor solvent is a critical point. In the present study it was selected methanol:water (80%) as an organic extractor solvent which was able to extract the antioxidant components of the acai extract without removing large amounts of inherent compounds of the skin with antioxidant activity. Finally, the determination of the chemiluminescence generated in the xanthine/luminol/xanthine oxidase system inhibition showed to be an important method for the measurement of the antioxidant activity of plant extracts in the skin. Still, this method was effective in quantifying the acai extract in cutaneous penetration/retention studies using vertical diffusion cells despite all the intrinsic errors of this used method.

Nesse trabalho foi realizado um estudo da atividade anti-radicalar de flavonóides frente ao ensaio com o sistema luminol/hemina/H2O2 desenvolvido por nosso Grupo de Pesquisa. Na tentativa de esclarecer a relação estrutura-atividade de flavonóides, foi realizada também uma investigação das propriedades de derivados fenólicos como compostos-modelo utilizando-se a reação quimiluminescente do luminol. Os resultados obtidos com os compostos-modelo com o ensaio luminol foram comparados com aqueles obtidos para estes aditivos em um ensaio que utiliza o radical estável DPPH como sonda. Além disso, foi realizado um estudo fitoquímico monitorado através da atividade anti-radicalar de extratos de Baccharis. Foram identificados dois componentes ativos da fase em acetato de etila obtida das folhas de Baccharis regnellii e a sua atividade anti-radicalar determinada. / In this work a systematic study on the antiradical activity of flavonoids was performed, using the assay luminol/hemin/H2O2 developed by our research group. With the objective to establish a structure activity relationship for flavonoids, a study on the antioxidant properties of several phenolic derivatives as model compounds was also performed, using luminol chemiluminescence. The results obtained with the model compounds from the luminol assay are compared to those obtained by an assay which utilizes the stable DPPH radical as probe. Furthermore, a phytochemical study, monitored by the antiradical activity, was performed on extracts of Baccharis. This study led to the identification of two active components in the ethyl acetate phase of Baccharis regnellii leafs and the determination of its antiradical activity.

O peroxinitrito é um oxidante versátil, sendo responsável por oxidações uni e bieletrônicas, adições nucleofílicas, nitrações, nitrosações, hidroxilações e geração de oxigênio singlete, possuindo papéis fisiológicos e deletérios. Estudos de EPR captação de spin mostraram que compostos carbonílicos podem sofrer abstração de um elétron por peroxinitrito, seguida de consumo de oxigênio e quimiluminescência; p.ex., isobutiraldeído (IBAL), acetoacetona (AA), 3-metilacetoacetpna (MAA), etil acetoacetato (EAA), etil 2-metilacetoacetato (EMAA) e succinilacetona (SA). A emissão de luz é provavelmente devida à espécies excitadas tripletes, formadas a partir da termólise de intermediários dioxetânicos. Os perfis de pH obtidos por consumo total de oxigênio e quimiluminescência em tampão fosfato, apontam o ânion peroxinitrito como oxidante e a forma enólica dos compostos carbonílicos como substratos. A análise de produtos sugere a ocorrência de uma reação em cadeia na presença de oxigênio. Estas reações podem ter importante papel biológico, considerando-se que (i) compostos carbonílicos são ubíquos em sistemas biológicos em condições fisiológicas e patológicas, (ii) peroxinitrito está relacionado a respostas fisiológicas e patológicas, (iii) carbonilas tripletes podem ser vistas como radicais alcoxil e, dessa forma, possuir papel deletério a biomoléculas. / Peroxynitrite displays an ample repertoire of chemical reactions -one- and two-electron oxidations, nucleophilic addition, nitration, nitrosation, hydroxylation, and singlet oxygen generation conferring it cell toxicity and signalling properties. Carbonyl compounds were shown by EPR spin-trapping to suffer one-electron abstraction by peroxynitrite, which is followed by oxygen consumption and chemiluminescence; e.g., isobutyraldehyde (IBAL), acetoacetone (AA), 3-methylacetoacetone (MAA), ethyl acetoacetate (EAA), ethyl 2-methylacetoacetate (EMAA) and succinylacetone (SA). Light emission probably arises from triplet species formed by the thermolysis of dioxetane intermediates. The pH profiles traced for oxygen uptake ·and chemiluminescence in phosphate buffer point to peroxynitrite anion as the oxidant and enolized carbonyls as the actual substrates. Product analysis suggests that a chain reaction occurs in the presence of oxygen. These reactions may play important biological roles considering that (i) carbonyl compounds are ubiquitous in biological systems under physiological and pathological conditions; (ii) peroxynitrite has been implicated in cell toxicity and signalling; (iii) triplet carbonyls may be viewed as alkoxyl radicals and, therefore, play a deleterious role in biomolecules.

There is a growing awareness of the risks of pollution in biological systems and one potential problem is the synthetic antioxidants, used for e.g. the stabilisation of polymeric materials. Natural antioxidants are an interesting alternative, if the high efficiency and thermal stability of the synthetic compounds can be reached. In the work described in this thesis, vitamin E (alfa-tocopherol) was studied as a natural antioxidant for the stabilisation of one of the major plastics, polyethylene (PE). The dependence of the surrounding environment for the efficiency of alfa-tocopherol in polyethylene (PE), throughout thermal aging, was characterised by sensitive techniques. Two techniques which have shown a high sensitivity in oxidation detection of polymers; chemiluminescence (CL) and gas chromatographic analysis, were compared with the commonly used methods, infrared spectroscopy (FT-IR) and thermal analysis. Three different additive systems were selected as active domains for -tocopherol in PE. Two of these contained carboxylic acid groups, poly (ethylene-co-acrylic acid) (EAA) and polyTRIM/PAA core-shell particles (Core), and the third, oat starch, had no such groups. The additives containing carboxylic groups improved the long-term efficiency of alfa-tocopherol in PE, according to carbonyl index measurements made by FT-IR, while the additive without carboxylic acid groups gave no improvement. The amount of carboxylic acids emitted from the materials after thermal aging, assessed by head-space solid-phase microextraction (HS-SPME) and gas chromatography-mass spectroscopy (GC-MS), also showed that EAA increased the antioxidant efficiency of alfa-tocopherol, whereas the Core system showed lower antioxidant efficiency. Reference systems containing the synthetic antioxidant Irganox 1076 and EAA or oat starch had the same performance as the materials stabilised with only the antioxidants. CL measurements in an inert atmosphere (TLI) have earlier been shown to give earlier oxidation detection than carbonyl index measurements in unstabilised PE. In this work, the TLI analysis and the carbonyl index measurements had the same sensitivity in the detection of oxidation in the stabilised materials. Assessment of low-molecular weight carboxylic acids in PE during the aging was made by gas chromatographic analysis together with solid-phase extraction. Propanoic acid showed the best correlation with the carbonyl index measurements, even if the carbonyl index showed earlier detection of oxidation. It was also found that TLI and CL in an oxidative atmosphere (CL-OIT) had the same sensitivity and were in accordance for all of the materials, with exception of the materials containing EAA and alfa-tocopherol or Irganox 1076. CL-OIT was also compared to the oxygen induction time determined by thermal analysis. / QC 20100921

Esta Tesis Doctoral evalúa la norma UNE EN 14211:2006 -Método normalizado de medida de la concentración de dióxido de nitrógeno y monóxido de nitrógeno por quimiluminiscencia-, citada como referencia técnica en la Directiva 2008/50/CE sobre calidad del aire y una atmósfera más limpia en Europa.La citada norma establece ensayos y criterios que deben superar los analizadores de los contaminantes citados antes de su comercialización en la Unión Europea, lo que se conoce como ensayo de aprobación de tipo. La Tesis Doctoral elaborada estudia en profundidad esta nueva norma, llevando a cabo un estudio crítico que analiza los aspectos operativos y los criterios exigidos. En algunos casos se proponen modificaciones que pueden ayudar a mejorarla. Así mismo se sugiere aplicar procedimientos correctivos de los datos obtenidos en campo, que resultan afectados por determinados parámetros físicos (presión, temperatura y humedad), modelizables mediante el empleo de leyes físicas o ajustes empíricos. / This Doctoral Thesis aims at evaluating the norm EN 14211: Standard method for the measurement of the concentration of nitrogen dioxide and nitrogen monoxide by chemiluminescence, mentioned in the Directive 2008/50/EC as technical reference document.The above standard specifies performance parameters that the analyzers must comply with prior to being sold, what is known as "Type Approval Test", and field calibration and verification guidelines, neither of which was considered in the previous standards.The study of the new Standard has revealed that some points could be improved in order to achieve a higher degree of accuracy and precision in the concentration data of nitrogen oxides. The improvement proposals cover certain aspects of the tests related to the Type Approval Test and data corrective procedures empirically obtained or by means of physical laws which are affected by physical parameters such as pressure, temperature or humidity.

Combustion systems utilizing bluff bodies to stabilize the combustion processes can experience oscillatory heat release due to the alternate shedding of coherent, von Kármán vortices under certain operating conditions. This phenomenon needs to be understood in greater detail, since unsteady burning due to vortex shedding can lead to combustion instabilities and flame extinction in practical combustion systems. The primary objective of this study was to elucidate the influence of combustion process heat release upon the Bénard-von Kármán (BVK) instability in reacting bluff body wakes. For this purpose, spatial and temporal heat release distributions in bluff body-stabilized combustion of liquid Jet-A fuel with high-temperature, vitiated air were characterized over a wide range of operating conditions. Upon comparing the spatial and temporal heat release distributions, the fuel entrainment and subsequent heat release in the near-wake were found to strongly influence the onset and amplitude of the BVK instability. As the amount of heat release in the near-wake decreased, the BVK instability increased in amplitude. This was attributed to the corresponding decrease in the local density gradient across the reacting shear layers, which resulted in less damping of vorticity due to gas expansion. The experimental results were compared to the results of a parallel, linear stability analysis in order to further understand the influence of the combustion processes in the near-wake upon the wake instability characteristics. The results of this analysis support the postulate that oscillatory heat release due to BVK vortex shedding is the result of local absolute instability in the near-wake, which is eliminated only if the temperature rise across the reacting shear layers is sufficiently high. Furthermore, the results of this thesis demonstrate that non-uniform fuelling of the near-wake reaction zone increases the likelihood of absolutely unstable, BVK flame dynamics due to the possibility of near-unity products-to-reactants density ratios locally, especially when the reactants temperature is high.

The ignition process is a critical consideration for combustion devices. External energy transfer to the combustor is required for ignition in common combustion systems. There are many ways to deposit energy into the flow but a standard method is a spark discharge because it is simple, compact, and reliable. Sparks can be categorized as either inductive or capacitive sparks that use a coil or an electrical resonance circuit with capacitor, respectively, to amplify the voltage. The creation of a successful ignition event depends on the spark energy deposited into the flow, the initial composition, pressure, temperature, turbulence level of flow etc. The deposited energy by the spark into the flow is critical for estimation of initial energy available for ignition of the mixture. Therefore, the electrical characteristics of the sparks were investigated under various flow conditions. Then measurements of deposited energy into the flow were conducted using a very accurate experimental procedure that was developed in this research. The results showed considerable electric energy losses to the electrodes for the relatively long, inductive sparks. However, the short, capacitive spark deposits electric energy into the flow with minimal loss (above 90% deposition efficiency). In addition, the characteristics of inductive spark are affected by flow velocity and by the existence of a flame. However, variations in the flow conditions do not affect the characteristics of the capacitive spark such as voltage-current time trace and energy deposition efficiency. Two ignition systems using above mentioned two spark types were developed. First, the capacitive spark energy was directly deposited into the premixed flow. Most researchers have not concentrated on the early initiation process but on the flame growth. Therefore, the generated kernel formed by the energy deposition was observed and characterized using optical methods, immediately following the spark. In addition, the mixing effect for this ignition kernel with surrounding gas was simulated using a numerical method. Based on the time trace of the OH* chemiluminescence, the reaction starts with the discharge and it is continuous until combustion begins. This means that in the presence of a high density spark in premixed flow, there exists no traditional delay as defined by other researchers for auto ignition. A simple Radical Jet Generator (RJG) was developed that is able to ignite and stabilize a flame in a high-speed flow. The inductive spark initiates the combustion in the RJG chamber. The RJG then injects the partially-burned products carrying large amounts of heat and radicals into a rapidly moving flammable main stream. Then it ignites and stabilizes a flame. The RJG requires low levels of electrical power as long as the flow velocity is relatively low since most of the radicals are produced by the incomplete combustion in its chamber. The importance of radicals was analyzed by RJG experiments and numerical methods. The reaction zone for RJG using a rich mixture was located both inside and outside of the RJG chamber. Therefore, the RJG using a rich mixture performed better in the ignition and stabilization of combustion in the main flow. According to an analysis using the CHEMKIM simulation software combined with the San Diego chemical mechanism, the RJG jet resulting from a rich mixture contains more radicals and intermediates than that produced by a lean mixture for the same sensible enthalpy. In addition, the burned gas contains less radicals and intermediates than the partially burned gas. If the RJG is operating with a high speed main flow, the flow rate through the RJG chamber must be increased to allow the radical jet to penetrate well into the rapid flow due to their higher injection velocity. Unfortunately, this leads to unsteady combustion in the RJG, which results in the pulsation of the radical jet. This reduces the number of radicals injected into the main flow. To investigate this operating condition, special attention was focused on four possible factors: unburned reactant pockets caused by motion of the spark channel, spark frequency, flame propagation speed and ignition delay. It was shown that the unsteadiness is affected by the flame speed and ignition delay because the frequency of pulsation in the chamber is highly dependent on the equivalence ratio. In addition, the interaction between the RJG operation and the combustion dynamics in the main combustor was documented. The acoustic pressure oscillations in the main combustor were suppressed when the RJG jet was turned on because the reaction region is relocated by the operation of the RJG.

137 f. / Submitted by Ana Hilda Fonseca (anahilda@ufba.br) on 2013-03-27T16:17:33Z No. of bitstreams: 1 TESE_Daniele_V FINAL.pdf: 3318748 bytes, checksum: 5c34e1db8db6c739cde7c6d8b715fac2 (MD5) / Approved for entry into archive by Ana Hilda Fonseca(anahilda@ufba.br) on 2013-06-05T15:40:50Z (GMT) No. of bitstreams: 1 TESE_Daniele_V FINAL.pdf: 3318748 bytes, checksum: 5c34e1db8db6c739cde7c6d8b715fac2 (MD5) / Made available in DSpace on 2013-06-05T15:40:50Z (GMT). No. of bitstreams: 1 TESE_Daniele_V FINAL.pdf: 3318748 bytes, checksum: 5c34e1db8db6c739cde7c6d8b715fac2 (MD5) Previous issue date: 2012 / CNPq / Neste trabalho foram desenvolvidos métodos espectrométricos para a determinação de ozônio em águas e elementos traço em leite de coco. A primeira etapa foi desenvolvida, no âmbito de um projeto de doutorado sanduíche, na Faculdade de Farmácia da Universidade do Porto em Portugal e a segunda no Instituto de Química da Universidade Federal da Bahia, Brasil. Na primeira parte do trabalho foi proposto um sistema de análise por injeção sequencial para determinação de O3 em água baseado na quimiluminescência deste com luminol sem a presença de catalisadores. Parâmetros físico-químicos foram estudados para obter o melhor desempenho analítico. O ciclo analítico desenvolvido permitiu a determinação de ozônio em 20 segundos com um consumo de 200 μL de amostra e 200 μL de luminol. O método apresentou boa precisão (RSD < 2,9%) bons limites de detecção e quantificação foram 0,04 e 0,13 mg L-1, respectivamente e a taxa de amostragem foi de cerca de 140 determinações/h. O método desenvolvido foi aplicado para a determinação de ozônio residual em águas e os resultados concordam a 95% de confiança com os fornecidos pelo procedimento de referência, a espectrofotometria no UV-Vis e o teor de ozônio nas diferentes amostras variou entre 0,21 - 1,36 mg L-1. O método analítico proposto representou uma alternativa vantajosa, pois requer um baixo consumo de reagentes e produz um volume reduzido de resíduos. A segunda parte consistiu no desenvolvimento de estratégias para a determinação de constituintes inorgânicos em amostras de leite de coco comercializadas na cidade de Salvador, Bahia. Para a avaliação multielementar foram propostos dois procedimentos de decomposição: em bloco digestor e assistido radiação por micro-ondas. Também foi proposto um procedimento de extração assistida por energia ultrassônica (US). As técnicas espectrométricas empregadas para determinação dos analitos foram: espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES) e espectrometria de massas com plasma indutivamente acoplado (ICP-MS). A eficiência de decomposição foi avaliada considerando os parâmetros acidez e teor de carbono residual. Ferramentas estatísticas, PCA e HCA, evidenciaram que há diferença entre três fornecedores de leite de coco em relação aos analitos determinados após decomposição em forno de micro-ondas, bem como o tipo de embalagem. Para avaliação do US, foram aplicados planejamentos fatorial e Doehlert. A exatidão das metodologias propostas foi verificada com materiais de referência certificados (NIST SRM 8435 e 1549) e teste de adição e recuperação. As faixas de concentração, em μg g-1, para os analitos foram: Ca (10 - 138); Cu (0,15 – 1,7); Fe (0,9 – 4,9); K (97 - 1773); Mg (23 - 206); Mn (0,3 – 3,2); P (116 – 701); Zn (0,4 – 2,2); Cr (0,185 – 0,211), Na (59-1186); Ni (0,113 – 0,133) e Pb (0,0220 - 0,0296). As concentrações dos elementos As, Cd e Co estavam abaixo do limite de quantificação. Os teores dos macro e micronutrientes foram comparados com os valores apresentados na Tabela Brasileira de Composição de Alimentos (TACO) e foi possível perceber que as amostras analisadas apresentam composições diferentes, o que pode ser creditado aos diferentes tipos de solo e processamento. A concentração dos contaminantes estava abaixo do valor máximo permitido pela Agência Nacional de Vigilância Sanitária (ANVISA) / Salvador