Sample records for liquid-liquid extraction
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1

Extração líquido-líquido em sistemas de fluxo/ Liquid-liquid extraction in flow systems

Facchin, Ileana; Pasquini, Celio
1998-02-01

Resumo em inglês This review deals with principles of the liquid-liquid extraction, when performed in flow systems. This approach is frequently used for sample treatment to improve the selectivity and/or sensitivity in analytical measurements. The advances in this area are reported, including the use of monosegmented flow systems to perform metal extraction through both two-phase and single phase processes.

Scientific Electronic Library Online (Portuguese)

2

Extração líquido-líquido de ferro(III) e titânio(IV) pelo ácido bis-(2-etil-hexil) fosfórico (D2EHPA) em meio de ácido sulfúrico/ Liquid-liquid extraction (LLE) of Fe(III) and Ti(IV) by bis-(2-ethyl-hexyl) phosphoric acid (D2EHPA) in sulfuric acid medium

Silva, Glauco Corrêa da; Cunha, José Waldemar Silva Dias da; Dweck, Jo; Afonso, Julio Carlos
2008-01-01

Resumo em inglês This work presents a study on the separation of Fe(III) and Ti(IV) from sulfuric acid leaching solutions of ilmenite (FeTiO3) using liquid-liquid extraction with D2EHPA in n-dodecane as extracting agent. The distribution coefficients (K D) of the elements related to free acidity and concentration of Fe(III) and Ti(IV) were determined. Free acidity was changed from 3x10-2 to 11.88 mol L-1 and D2EHPA concentration was fixed at 1.5 mol L-1. Recovery of final products as well (mais) as recycling of wastes generated in the process were also investigated. The LLE process as a feasible alternative to obtain high-purity TiO2.

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3

Extração líquido-líquido de urânio(VI) do colofanito de itataia (Santa Quitéria, Ceará) por extratantes orgânicos em presença de ácido fosfórico/ Liquid-liquid extraction of uranium(VI) from colofanite of itataia (Santa Quitéria, Ceará) by organic extractants in the presence of phosphoric acid

Ribeiro, Valeria Aparecida Leitão; Afonso, Júlio Carlos; Wildhagen, Glória Regina da Silva; Cunha, José Waldemar Silva Dias da
2008-01-01

Resumo em inglês This work describes the liquid-liquid extraction of uranium after digestion of colofanite (a fluoroapatite) from Itataia with sulfuric acid. The experiments were run at room temperature in one stage. Among the solutions tested the highest distribution coefficient (D > 60) was found for 40%vol. DEHPA (di(2-ethyl-hexyl)phosphoric acid) + 20% vol. TOPO (trioctylphosphine oxide) in kerosene. Thorium in the raffinate was quantitatively extracted by TOPO (0.1% vol.) in cyclohex (mais) ane. Uranium stripping and separation from iron was possible using 1.5 mol L-1 ammonium or sodium carbonate (room temperature, one stage). However, pH control is essential for a good separation.

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4

Otimização e validação da técnica de extração líquido-líquido com partição em baixa temperatura (ELL-PBT) para piretróides em água e análise por CG/ Optimization and validation af liquid-liquid extraction with the low temperature partition technique (LLE-LTP) for pyrethroids in water and GC analysis

Vieira, Heulla Pereira; Neves, Antônio Augusto; Queiroz, Maria Eliana Lopes Ribeiro de
2007-06-01

Resumo em inglês The liquid-liquid extraction with the low temperature partition technique was developed for the analysis of four pyrethroids in water by CG. Using a factorial design the extraction technique was optimised evaluating the effect of the variables ionic strength, contact time and proportion between sample and solvent volumes. The validation parameters sensitivity, precision, accuracy and detection and quantification limits were evaluated. The LOD and LOQ of the method varied from 1.1 to 3.2 µg L-1 and 2.7 to 9.5 µg L-1, respectively.

Scientific Electronic Library Online (Portuguese)

5

Diazepam e nordiazepam em plasma: métodos de extração líquido-líquido e em fase sólida no pré-tratamento de amostras para análise cromatográfica em fase líquida/ Diazepam and nordiazepam in plasma: liquid-liquid and solid phase extraction in sample pre-treatment for high performance liquid chromatography analysis

Freire, Ellen Figueiredo; Miranda, Juniella Luiza; Maia, Patrícia Penido; Vieira, Elisabeth Pizzamiglio; Borges, Keyller Bastos; Siqueira, Maria Elisa Pereira Bastos de
2005-10-01

Resumo em inglês Analysis of diazepam (DZP) and its active metabolite nordiazepam (NDZP) in plasma is commonly performed in clinical medicine to ensure proper therapeutic effects while minimizing the incidence of toxicity. This study aimed to optimize analytical parameters and compare two pre-treatment techniques, liquid-liquid (LLE) and solid phase extraction (SPE), as well as liquid chromatographic conditions to analyze simultaneously DZP and NDZP in plasma from 20 patients treated with (mais) a daily dose of 10 mg. Both techniques showed to be well in line with the international criteria for analytical validation, which permitted to quantify DZP (66.2 - 1148.6 ng mL-1) and NDZP (138.5 - 808.6 ng mL -1) in all samples. The correlation coefficients between SPE and LLE were respectively 0.9729 for DZP and 0.9643 for NDZP.

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6

Pré-concentração de chumbo e cádmio em um sistema de micro extração líquido-líquido e determinação por espectrometria de absorção atômica com chama/ A liquid-liquid microextraction system for pb and cd enrichment and determination by flame atomic absorption spectrometry

Carasek, Eduardo; Tonjes, Jussara Wick; Scharf, Mauro
2002-09-01

Resumo em inglês A method for determination of lead and cadmium in aqueous samples using solvent microextraction and dithizone as complexing agent with FAAS was developed. Solvent microextraction parameters were optimized. The effect of foreign ions on the extraction yields was studied. The extraction was carried out until the aqueous to organic phase ratio achieved a 250 fold preconcentration of metals. For preconcentration times of 4 min the 3sigma detection limits, relative standard de (mais) viations (n=7) and linear calibration ranges were 1.6 mug L-1, 5.8% and 10.0 -- 80.0 mug L-1 for lead and 11.1 ng L-1, 5.9% and 0.3 -- 3.0 mug L-1 for cadmium, respectively. The solvent microextraction procedure presented here was applied to the determination of lead and cadmium in natural waters.

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7

Alternativas para o tratamento de efluentes da indústria galvânica/ Alternatives for the galvanic wastewater treatment

Pereira Neto, Artur; Bretz, Joana de Souza; Magalhães, Fernando Silva; Mansur, Marcelo Borges; Rocha, Sônia Denise Ferreira
2008-09-01

Resumo em português Os métodos de precipitação química, cristalização e extração líquido-líquido foram aplicados visando propor alternativas para o tratamento de efluentes líquidos gerados pela indústria de galvanoplastia. Efluentes de diversas empresas do setor, localizadas no estado de Minas Gerais (Brasil), foram coletados e caracterizados. O efluente estudado, proveniente de empresa de galvanização de zinco a quente, continha cerca de 90 g/L de ferro total, 35 g/L de zinco (mais) e menores quantidades de Al, Ni e Cu, em meio ácido clorídrico (pH = 0,6). A separação seletiva entre ferro e zinco não se mostrou eficiente por precipitação, sendo a técnica adequada somente no tratamento do efluente, ao contrário da cristalização e extração líquido-líquido utilizando-se TBP como agente extratante. A integração destas técnicas ainda requer estudos mais detalhados visando à otimização de custos e das condições operacionais. Resumo em inglês Separation methods such as chemical precipitation, crystallization and liquid-liquid extraction have been investigated aiming to treat effluents generated by the galvanic industry. Effluent samples generated by several companies located in the state of Minas Gerais (Brazil) were collected and chemically characterized. For this work, a typical zinc hot-dip galvanizing effluent containing about 90 g/L of total iron, 35 g/L of zinc and minor amounts of Al, Ni, Cu, in HCl med (mais) ium (pH = 0.6) was treated. A selective separation between metals zinc and iron was not achieved by chemical precipitation, which was found adequate to threat water only. On contrary, zinc and iron was separated very efficiently by crystallization and liquid-liquid extraction using TBP as extractant agent. The integration of these methods to recover zinc and iron from effluent still requires more detailed studies.

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8

Análise simultânea da mirtazapina e N-desmetilmirtazapina em plasma empregando a cromatografia líquida de alta eficiência/ Simultaneous analysis of mirtazapine and N-demethylmirtazapine in plasma by high-performance liquid chromatography

Briguenti, Ana Cecília Coragem; Bonato, Pierina Sueli
2005-12-01

Resumo em inglês Para avaliação das propriedades farmacocinéticas e monitorização terapêutica da mirtazapina, antidepressivo recentemente introduzido no mercado e que vem sendo bastante utilizado, são necessários métodos de análise simples, sensíveis e seletivos. Sendo assim, a cromatografia líquida de alta eficiência com detecção por fluorescência foi empregada para o desenvolvimento de um método para análise simultânea da mirtazapina e de seu metabólito, N-desmetilmi (mais) rtazapina, em plasma. Após extração líquido-líquido utilizando tolueno como solvente extrator, o fármaco, metabólito e padrão interno (metoprolol) foram separados em coluna LiChrospher 100 RP-8 capeada, utilizando fase móvel composta por tampão fosfato de sódio, 0,1 mol/L, pH 3,5-acetonitrila (82:18, v/v). O método apresentou linearidade no intervalo de 2,5 a 500 ng/mL para ambos os compostos, com recuperações médias de 77 e 66% para a mirtazapina e demetilmirtazapina, respectivamente. Os limites de quantificação (2,5 ng/mL), precisão (CV Simple, sensitive and selective analytical methods are required for pharmacokinetic studies and therapeutic drug monitoring of mirtazapine, a new antidepressant drug. Thus high-performance liquid chromatography with fluorescence detection was used for the simultaneous analysis of mirtazapine and its metabolite, N-demethylmirtazapine, in plasma. After liquid-liquid extraction with toluene, the drug, metabolite and internal standard (metoprolol) were resolved using a LiChrospher 100 RP-8 endcapped column with a mobile phase of 0.1 mol/L phosphate buffer, pH 3.5-acetonitrile (82:18, v/v). The method was linear in the range of 2.5 to 500 ng/mL for both analytes, with mean recoveries of 77% and 66% for mirtazapine and N-demethylmirtazapine, respectively. The quantification limits (2.5 ng/mL), precision (CV

Scientific Electronic Library Online (Portuguese)

9

Ocorrência, aspectos toxicológicos, métodos analíticos e controle da patulina em alimentos/ Occurrence, toxicological aspects, analytical methods and control of patulin in food

Welke, Juliane Elisa; Hoeltz, Michele; Dottori, Horacio Alberto; Noll, Isa Beatriz
2009-02-01

Resumo em português A patulina é uma micotoxina produzida por várias espécies de Penicillium, Aspergillus e Byssochlamys. Em experimentos com animais, ela demonstrou ter atividade mutagênica, carcinogênica e teratogênica. Tem sido freqüentemente encontrada em maçãs e derivados. A patulina é facilmente transferida da maçã para o suco durante o processamento devido a sua alta solubilidade em água. Essa micotoxina é muito estável ao aquecimento em meio ácido, como no suco de ma� (mais) �ã. Assim, a presença de patulina em suco de maçã é um indicador da qualidade das maçãs utilizadas no processamento. Muitos métodos têm sido desenvolvidos para a determinação da patulina, principalmente baseados na extração líquido-líquido com acetato de etila e determinação por CLAE. É importante evidenciar a necessidade de legislação que regulamente limites dessa micotoxina em alimentos no Brasil. Esta revisão bibliográfica tem como objetivos descrever as principais características da patulina, a ocorrência, os aspectos toxicológicose os métodos desenvolvidos para sua detecção e controle durante os estágios da produção da maçã e suco. Resumo em inglês Patulin is a mycotoxin produced by several Penicillium, Aspergillus and Byssochlamys species. Patulin is a highly toxic compound which has shown to be mutagenic, carcinogenic and teratogenic in experiments with animals. It has often been found in apples and apple products. Patulin is easily transfered into apple juice during processing due to its high solubility in water. This mycotoxin is very stable to heat in acidic medium as in apple juice. Thus, patulin content of ap (mais) ple juice is an indicator of the quality of the apples used to juice production. Many methods have been developed for the patulin determination mainly based on liquid-liquid extraction with ethyl acetate and use of HPLC for detection. It is important to show the need of legislation that imposes patulin limits in foods in Brazil. The objectives of this review are to describe the main patulin characteristics, occurrence, toxicological aspects, methods developed for patulin detection and control during the stages of apple and juice production.

Scientific Electronic Library Online (Portuguese)

10

Determinação de esteróides androgênicos anabólicos em urina por cromatografia gasosa acoplada à espectrometria de massas/ Detection of androgenic anabolic steroids (AAS) in urine samples by gas chromatography-mass spectrometry

Campos, Daniel Rossi de; Yonamine, Mauricio; Alves, Maria Janieire de Nazaré Nunes; Moreau, Regina Lucia de Moraes
2005-12-01

Resumo em português Esteróides androgênicos anabólicos (EAA) são substâncias naturais, sintéticas ou semi-sintéticas derivadas da testosterona, utilizadas em atividades esportivas com o objetivo de melhorar o desempenho físico pelo aumento de massa e força muscular. Apesar de causarem efeitos tóxicos graves, principalmente sobre os sistemas cardiovascular, hepático e neuro-endócrino, os EAA têm sido amplamente utilizados no âmbito esportivo. Desta forma, o presente trabalho tev (mais) e como objetivo a validação de um método para a determinação de esteróides e/ou seus produtos de biotransformação em amostras de urina por cromatografia gasosa acoplada à espectrometria de massas (CG-EM). O método baseou-se na hidrólise enzimática de esteróides conjugados, no emprego da extração líquido-líquido e na derivação do extrato para posterior análise por CG-EM, no modo de monitoramento seletivo de íons (SIM). O método validado cumpriu com os princípios de confiança necessários para a determinação de EAA em amostras de urina com a finalidade de controle de dopagem no esporte. Os limites de detecção dos esteróides analizados variaram de 0,5 a 15 ng/mL. Bons valores de precisão (intra e interensaio) também foram obtidos (CV Resumo em inglês Androgenic anabolic steroids (AAS) are defined as natural, synthetic or semi-synthetic drugs chemically derived from testosterone, used with the aim to improve physical performance by increasing both muscle strength and mass. Despite their reported toxicological effects on the cardiovascular, hepatic and neuro-endocrine systems, the AAS have been extensively used in sports activities. The objective of this study was to validate an analytical method for the detection of AA (mais) S and/or their metabolites in urine samples. The method was based on enzymatic hydrolysis, liquid-liquid extraction, derivatization and further analysis by gas chromatography-mass spectrometry (GC-MS) operated in the selected ion monitoring mode (SIM). The validated method agrees with the confidence concepts for AAS detection in urine samples for anti-doping control programs. The limits of detection of AAS varied from 0,5 to 15ng/mL. Good inter and intra-assay precisions were also observed (CV

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11

Determinação de tricotecenos em cerveja e avaliação de incidência no produto comercializado no Rio Grande do Sul/ Determination of trichothecenes in beer and evaluation of occurence in the product commercialized in Rio Grande do Sul

Garda, Jaqueline; Macedo, Rejane Martins; Badiale-Furlong, Eliana
2004-12-01

Resumo em português Este trabalho adaptou um método e avaliou os seus indicadores de mérito para determinação de tricotecenos, desoxinivalenol (DON) e toxina T-2, em cervejas comercializadas na região Sul do Rio Grande do Sul, empregando cromatografia gasosa. As adaptações foram realizadas na etapa de extração, purificação, derivação e condições cromatográficas usando amostras de cerveja artificialmente contaminadas, avaliando a adequação do procedimento pela recuperação (mais) obtida. Foram estudados os solventes acetonitrila, metanol e cloreto de metileno puro ou em misturas para a etapa de extração. A purificação do extrato foi realizada empregando ou não minicoluna de carvão:alumina:celite (7:5:3). Para a derivação testou-se basicidade do meio (bicarbonato de sódio, piridina), agente acilante (TFAA e HFBI), tempo (30 e 60 minutos) e temperatura (60 e 80ºC). Foram otimizadas as condições cromatográficas em cromatógrafo gasoso equipado com injetor split/splitless e detector de ionização de chama. A melhor recuperação foi obtida quando se empregou partição líquido-líquido com cloreto de metileno, seguida da limpeza em minicoluna e derivação com TFAA e piridina a 60°C durante 60 minutos. A recuperação média foi de 83 e 103% para DON e toxina T-2 respectivamente, para níveis de adição entre 50 e 200ng/mL. O coeficiente de variação assumiu valores de 2% e 4% e limite de detecção de 21 e 60 ng/mL. A aplicabilidade do método foi testada em um levantamento realizado em 72 amostras de cervejas. Destas 9,7% estavam contaminadas, sendo 5,3% com DON (50 a 336ng/mL) e 4,5% com toxina T-2 (114 a 249ng/mL). Resumo em inglês The present work adapted and evaluated a trichothecenes determination, DON and the T-2 toxin and conduted a survey of the product commercialized in Rio Grande do Sul in beer commercialized in Rio Grande do Sul State by gas chromatography. It studied extraction, purification, derivatization and chromatographic conditions using artificially contaminated samples. Acetonitrile, methylene chloride and methanol pure or in misture were tested for the extraction step. The extract (mais) was purified using a carbon:alumina:celite minicolumn (7:5:3). For derivatization, the following conditions were tested: the basicity of the medium (sodioum bicarbonate, pyridine),the derivatizing agent (TFAA and HFBI), reaction time (30 and 60 minutes) and temperature (60 and 80°C). The chromatographic conditions were optimized in a gas chromatograph, with a split/splitless injector and an ionization flame detector. The highest recovery was obtained when liquid-liquid partition was carried out with methylene chloride, followed by cleaning in a minicolumn and derivatization with TFAA and pyridine at a temperature of 60°C for 60 minutes. The average recovery for DON and the T-2 toxin were 83 and 103%, the coefficient variation 1.6 to 4% and the detection limit of 21 and 60ng/mL, respectively. The applicability of the method was tested in a survey carried out in 72 beer samples, 9.7 % of which were contaminated 5.3% with DON (50 to 336ng/mL) and 4.5% with the T-2 toxin (114 to 249ng/mL).

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12

Hidrocarbonetos aromáticos policíclicos em margarina, creme vegetal e maionese/ Polycyclic aromatic hydrocarbons in margarine, vegetable cream and mayonnaise

CAMARGO, M. Sílvia F. O.; TOLEDO, M. Cecília de F.
2000-04-01

Resumo em português Hidrocarbonetos aromáticos policíclicos (HAPs) são um grupo de compostos que têm sido objeto de muitas pesquisas devido ao seu potencial tóxico. Neste estudo, margarinas, cremes vegetais e maioneses disponíveis no mercado brasileiro foram analisadas quanto ao teor de pireno, fluoranteno, benzo(a)antraceno, criseno, benzo(b)fluoranteno, benzo(k)fluoranteno, benzo(a)pireno e dibenzo(a,h)antraceno. A metodologia analítica envolveu extração líquido-líquido, limpeza (mais) em coluna de sílica gel e determinação por cromatografia líquida de alta eficiência com detector de fluorescência. Níveis variáveis de contaminação foram encontrados em marcas diferentes do mesmo produto e em lotes diferentes da mesma marca. O teor médio de HAPs totais encontrados esteve na faixa de 4,1 a 7,1mig/kg em cremes vegetais, de 1,7 a 3,9mig/kg em margarinas e de 1,0 a 21,7mig/kg em maioneses. Em geral, os produtos que declaravam conter óleo de milho em sua formulação mostraram os maiores níveis de contaminação. Com base nestes resultados e na importância de gorduras, óleos e produtos derivados como fonte de ingestão de HAPs, recomenda-se aos produtores de margarinas, cremes vegetais e maioneses que iniciem o controle da contaminação dos óleos vegetais utilizados na elaboração destes produtos, de forma a reduzir a exposição do consumidor à quantidades excessivas de compostos potencialmente carcinogênicos. Resumo em inglês Polycyclic aromatic hydrocarbons (PAHs) are a group of compounds that have been the subject of much concern due to their toxic potential. In this study, margarine’s, vegetable cream and mayonnaise available on the Brazilian market were analyzed for pyrene, chrysene, benzo(a)pyrene, benzo(b)fluoranthene and dibenzo(a,h)anthracene. The analytical methodology involved liquid-liquid extraction, clean-up on silica gel column and determination by high performance liquid chroma (mais) tography using fluorescence detector. Variable levels of contamination were found within differents brands of the same product and within differents batches of the same brand. The total PAH content was in the range of 4.1 to 7.1mug/kg in vegetable cream, 1.7 to 3.9mug/kg in margarine and 1.0 to 21.7mug/kg in mayonnaise. In general the products which according to the label contain corn oil showed the highest levels of contamination. Based on these results and on the importance of fat, oils and derived products for the intake of PAHs, it is recommended that producers of margarine, vegetable creams and mayonnaise start to control the contamination of the vegetable oils used in the elaboration of these products, in order to reduce the exposure of consumers to excessive amounts of potentially carcinogenic compounds.

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13

Determinação de efedrinas em urina por cromatografia em fase gasosa (CG/DNP) para o controle da dopagem no esporte/ Gas chromatographic method for the determination of ephedrines in urine for doping control purposes

Garcia, Paula Rodrigues; Yonamine, Mauricio; Moreau, Regina Lúcia de Moraes
2005-09-01

Resumo em português Efedrinas são aminas simpatomiméticas componentes de diversas especialidades farmacêuticas, utilizadas no tratamento de doenças respiratórias devido à sua ação descongestionante e broncodilatora. Atualmente, diversos produtos comercializados como suplementos nutricionais contêm efedrinas e são amplamente utilizados no meio esportivo, com o objetivo de facilitar a queima de gorduras e melhorar o desempenho. Entretanto, o uso indiscriminado destas substâncias pod (mais) e acarretar série de efeitos tóxicos como hipertensão, taquicardia, cefaléia e tremores. Devido à sua ação psicoestimulante, foram incluídas na lista de substâncias proibidas nas atividades esportivas pelo Comitê Olímpico Internacional (COI) e estabelecidas concentrações na urina para o controle da dopagem (efedrina e metilefedrina: 10 µg/mL). O presente trabalho teve como objetivo a validação de um método para quantificação de efedrinas, por cromatografia em fase gasosa acoplada a detetor de nitrogênio/fósforo (CG/DNP), em amostras de urina com a finalidade de controle da dopagem. O método consistiu em extração líquido-líquido e posterior derivação das efedrinas com anidrido trifluoroacético, e demonstrou ser simples e prático, apresentando linearidade nas faixas de concentração estudadas. Amostras de urina de voluntários que relataram uso de efedrinas foram submetidas à análise pelo método proposto. Resumo em inglês Ephedrines are sympathomimetic amines present in many pharmaceutical preparations used in the treatment of respiratory diseases due to their actions against broncospasm and congestion. Nowadays, several products sold as nutritional supplements contain ephedrines and are widely used in a diverse range of sports as weight loss aids and enhancement of athletic performance. However, the abuse of ephedrines may lead to a number of adverse effects including hypertension, headac (mais) he, tachycardia and seizure. Due to their CNS stimulating action, ephedrines are included in the prohibited list of substances by the International Olympic Committee (IOC). Urinary threshold concentrations were established (ephedrine and methylephedrine >10 µg/mL). The aim of this work was to develop and validate a method for the simultaneous determination of ephedrines present in urine samples for doping purposes by gas chromatography with nitrogenous-phosphorous detector (GC/NPD). The method was based on a liquid-liquid extraction of alkalinized urine and further derivatization with trifluoroacetic anhydride (TFA). The validated method showed to be simple, practical and linear at the studied concentrations range. Urine samples collected from volunteers, who reported the use of ephedrines, were submitted to the proposed method.

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14

Determinação de fenol urinário por cromatografia em fase gasosa em trabalhadores que utilizam resinas fenólicas em fundições/ Determination of urinary phenol by gas chromatography in workers using phenolic resins in foundries

Peixe, Tiago Severo; Nascimento, Elizabeth de Souza; Della Rosa, Henrique Vicente
2006-06-01

Resumo em português O fenol é utilizado na indústria como agente desinfetante no preparo de resinas fenólicas e pigmentos de tintas. Apresenta-se no estado sólido à temperatura ambiente, com coloração fracamente rósea, odor acre e higroscópico. Na exposição ocupacional aguda o composto pode levar a lesões eritematosas e, cronicamente, afetar a maturação celular no compartimento medular ósseo devido à formação de quinonas livres e 1,4-benzoquinona, proveniente do metabolismo (mais) hepático da hidroquinona via CYP2E1. A monitorização biológica possui relevância nas situações de exposições ocupacionais. Para tal, utiliza-se o fenol urinário, considerado bioindicador de exposição a este composto. O objetivo do presente trabalho foi validar uma técnica de extração líquido-líquido para quantificar o fenol urinário, por meio da cromatografia em fase gasosa com detetor de ionização por chama (CG/DIC) em urina de trabalhadores expostos ao fenol em fundições. O método mostrou-se linear de 5 a 200 µg/mL; coeficiente de regressão linear (r²) de 0,999; limites de detecção e quantificação 2,0 e 5,0 µg/mL, respectivamente; precisão intra-ensaio entre 4,5 e 8,9% e inter-ensaio entre 5,7 e 14,2%; exatidão entre 6,2 e 11,9% e recuperação superior a 87%. O método demonstrou ser simples e rápido. Amostras provenientes de trabalhadores expostos ao fenol foram analisadas comprovando a aplicação da técnica na monitorização biológica. Resumo em inglês Phenol is used as an industrial chemical, disinfectant agent, in the preparation of phenolic resins and paint pigments. When in solid state, it shows a light pink color, ocre odor, and is hygroscopic. In acute occupational exposure, the compound can produce erythemic injuries and burn sensation and, chronically, affect the cellular maturation of bone marrow due the free quinones and 1,4-benzoquinone, deriving from hepatic metabolism of the hydroquinone by P450 isozyme (CY (mais) P2E1). The biological monitoring is important in occupational exposure situations. So, urinary phenol, considered the biological indicator of phenol exposure has to be determined. The aim of this work was to validate a method for urinary phenol quantification, using liquid-liquid extraction. Gas chromatography with flame ionization detector (GC/FID) was used in this method. The analytical procedure showed linearity in the dynamic range of the assay from 5 - 200 µg/mL. The limits of detection (LOD) and quantification (LOQ) were: 2.0 and 5.0 µg/mL, respectively. Intra-assay precision coefficient was between 4.5 - 8.9% and the inter-assay precision coefficient was between 5.7 - 14.2%. The accuracy coefficient was between 6.2 - 11.9%. Recovery values were higher than 87%. The coefficient of correlation was 0.999. The method is simple, rapid and efficient. Urine samples from workers exposed to phenolic resins were analyzed to show the method application in biological monitoring.

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15

Óleo essencial de limão no ensino da cromatografia em camada delgada/ Lime essential oil in the teaching of thin layer chromatography

Silva, Rosaly S.; Ribeiro, Carlos Magno R.; Borges, Márcia N.; Blois, Giselle S. O.
2009-01-01

Resumo em inglês This paper describes a simple experiment employing the essential oil of limes which can be applied in undergraduate organic chemistry laboratory classes for the teaching of thin layer chromatography (TLC). The experiment consists in submit lime peel oil to TLC separation employing hexane and dichloromethane as the eluents and five different systems for visualization of the chromatogram. In one experiment it is possible to teach the different variables of the TLC technique (mais) . This experiment may also be performed following vapor distillation and liquid-liquid extraction technique in experimental classes.

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Vitaminas lipossolúveis em alimentos: uma abordagem analítica/ Fat-soluble vitamins in food: an analytical approach

Paixão, José A. da; Stamford, Tânia L. M.
2004-02-01

Resumo em inglês This study concerns certain problems inherent to the determination of fat-soluble vitamins in food, from extraction methods to identification and quantification. The discussion involves the main official and unofficial extraction methods coupled with spectrophotometric and HPLC techniques in which vitamins samples are obtained through liquid-liquid-solid and liquid-liquid-solid-solid extraction, indispensable to the analytical separation of different chemical compounds wi (mais) th vitamin functions. A saponification stage, possibly coupled with supercritical fluid extraction appears to be mandatory in the determination of vitamins A and E in their alcoholic forms. Alternative identification and quantification procedures are outlined: biological and chemical assays, analytical separations by HPLC (normal and reversed-phase), UV detection (all fat-soluble vitamins) and fluorescence detection (retinoids and tocopherols). Automation from sample preparation to quantification stages increases the data acquisition rate.

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Purification of plasmid DNA vectors by aqueous two-phase extraction and hydrophobic interaction chromatography

Trindade, Inês P.; Diogo, Maria M.; Prazeres, Duarte M. F.; Marcos, João Carlos

The current study explores the possibility of using a polyethyleneglycol(PEG)/ammonium sulphate aqueous two-phase system (ATPS) as an early step in a process for the purification of a model 6.1 kbp plasmid DNA (pDNA) vector. Neutralised alkaline lysates were fed directly to ATPS. Conditions were sel...

DRIVER (Portuguese)

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Métodos de extração e/ou concentração de compostos encontrados em fluidos biológicos para posterior determinação cromatográfica/ Methods of extraction and/or concentration of compounds found in biological fluids for subsequent chromatographic determination

Queiroz, Sonia C. N.; Collins, Carol H.; Jardim, Isabel C. S. F.
2001-02-01

Resumo em inglês When organic compounds present in biological fluids are analysed by chromatographic methods, it is generally necessary to carry out a prior sample preparation due the high complexity of this type of sample, especially when the compounds to be determinated are found in very low concentrations. This article describes some of the principal methods for sample preparation in analyses of substances present in biological fluids. The methods include liquid-liquid extraction, soli (mais) d phase extraction, supercritical fluid extraction and extraction using solid and liquid membranes. The advantages and disadvantages of these methods are discussed.

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Microextração em fase líquida (LPME): fundamentos da técnica e aplicações na análise de fármacos em fluidos biológicos/ Liquid-phase microextraction (LPME): fundamentals and applications to the analysis of drugs in biological samples

Oliveira, Anderson Rodrigo Moraes de; Magalhães, Igor Rafael dos Santos; Santana, Fernando José Malagueño de; Bonato, Pierina Sueli
2008-01-01

Resumo em inglês The analysis of drugs and metabolites in biological fluids usually requires extraction procedures to achieve sample clean-up and analyte preconcentration. Commonly, extraction procedures are performed using liquid-liquid extraction or solid-phase extraction. Nevertheless, these extraction techniques are considered to be time-consuming and require a large amount of organic solvents. On this basis, microextraction techniques have been developed. Among them, liquid-phase mic (mais) roextraction has been standing out. This review describes the liquid-phase microextraction technique based on hollow fibers as a novel and promising alternative in sample preparation prior to chromatographic or electrophoretic analysis. The basic concepts related to this technique and its applicability in extraction of drugs are discussed.

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Enriquecimento de compostos fenólicos de folhas de Inga edulis por extração em fase sólida: quantificação de seus compostos majoritários e avaliação da capacidade antioxidante/ Purification of phenolic compounds from Inga edulis leaves using solid-phase extraction: major compounds quantification and antioxidant capacity evaluation

Dias, Aécio Luís de Sousa; Souza, Jesus Nazareno Silva de; Rogez, Hervé
2010-01-01

Resumo em inglês A phenolic fraction was obtained from of the acetone-water-acetic acid extract of Inga edulis leaves, by liquid-liquid partition and SPE-C18 cartridges. This method provided an increase of 108, 66, 51, 50 and 36% of flavonols, proanthocyanidins, total polyphenols, gallotannins and flavanols, respectively. The major phenolics in purified fraction were procyanidin B2, catechin and myricetin-3-O-α-L-rhamnopyranoside, which achieved increases of 111, 47 and 45%, respecti (mais) vely, after SPE. Acid hydrolysis confirmed the presence of procyanidins, prodelphinidins and glycosylated flavonoids.

Scientific Electronic Library Online (Portuguese)

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Determinação de resíduos de organoclorados em águas fluviais do município de Viçosa - MG/ Determination of organochlorinated present in river from the region of Viçosa, MG

Chagas, Cíntia Maria; Queiroz, Maria Eliana Lopes Ribeiro de; Neves, Antônio Augusto; Queiroz, José Humberto de; Oliveira, Tânia Toledo de; Nagem, Tânus Jorge
1999-07-01

Resumo em inglês In this work the contamination, by organochlorinated, of a drinking water source located in the region of Viçosa, MG, was evaluated. The identification and quantification of the analytes was carried out using a gas-chromatograph equipped with an electron capture detector after liquid-liquid extraction and concentration. Four insecticides, Aldrin, Epoxy heptachloride, Endrin and op'- DDT were detected in concentrations that are higher than the safety limits established in the Brazilian legislation.

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Determinação de resíduos de cloranfenicol em amostras de leite e mel industrializados utilizando a técnica de espectrometria de massas em "tandem" (CLAE-EM/EM)/ Determination of chloramphenicol residues in industrialized milk and honey samples using LC-MS/MS

Martins Júnior, Helio Alves; Bustillos, Oscar Vega; Pires, Maria Aparecida Faustino; Lebre, Daniel Temponi; Wang, Alexandre Yautin
2006-06-01

Resumo em inglês The present work shows a method for the determination of chloramphenicol (CAP) antibiotic in milk, powder milk and honey. The solid phase extraction and liquid-liquid extraction were applied as a clean-up and pre-concentration strategies followed by LC-ESI/MS/MS analysis. The recovery was studied for different fortification levels from 0.05 to 1.00 µg L-1 in milk, showing values between 91 101% and RSD bellow 8.0%, while honey was spiked with a concentration of 0.20 µg (mais) kg-1 yelding a mean recovery of 83% and RSD of 6.5%. The quantification transition 321>152 showed a LOD of 0.52 ng kg-1 and LOQ of 1.85 ng kg-1.

Scientific Electronic Library Online (Portuguese)

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Desenvolvimento e validação de método de análise de glifosato em grãos de soja/ Development and validation of a method of analysis of glyphosate in soy grains

Abreu, Adley Bergson Gonçalves de; Matta, Marcia Helena de Rizzo da; Montagner, Émerson
2008-01-01

Resumo em inglês The main objective of this work is to develop an efficient procedure to determine glyphosate in soybean grains. The cleanup of the aqueous extracts was done in two steps, beginning with liquid-liquid partitioning and then solid-phase extraction with anion exchange resin. After derivatization with a mixture of trifluoroacetic anhydride (TFAA) and trifluoroethanol (TFE), quantification was done by gas chromatography coupled to mass spectrometry. The mean recovery and RSD of (mais) the spiked samples were, respectively, 80.5% and 3.1% at level 0.200 mg kg-1, 93.3% and 18.7% at level 0.500 mg kg-1 and 92% and 3.5% at level 1.000 mg kg-1. The method was linear in the working range (correlation coefficient = 0.9965).

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