Table of contents
Química Nova, Volume: 35, Issue: 1, Published: 2012Química Nova, Volume: 35, Issue: 1, Published: 2012
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Editorial Vamos Continuar! Torresi, Susana I. Córdoba de Pardini, Vera L. Ferreira, Vitor F. |
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Artigo Nutrients fluxes from groundwater discharge into Mangueira Lagoon (Rio Grande do Sul, Brasil) Andrade, Carlos F. F. Niencheski, Luis F. H. Attisano, Karina K. Milani, Marcio R. Santos, Isaac R. Milani, Idel C. Abstract in English: This study assesses the importance of groundwater discharge to dissolved nutrient levels in Mangueira Lagoon. A transect of an irrigation canal in the margin of Lagoon demonstrated a strong geochemical gradient due to high groundwater inputs in this area. Using 222Rn as a quantitative groundwater tracer, we observed that the flux of dissolved inorganic nitrogen (DIN), silicate and phosphate (1178 and 1977; 26190 and 35652; 167 and 188 mol d-1 for winter and summer, respectively) can continually supply/sustain primary production. The irrigation canals act as an artificial underground tributary and represent a new source of nutrients to coastal lagoons. |
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Artigo Electrolyte influence on the Cu nanoparticles electrodeposition onto boron doped diamond electrode Matsushima, Jorge Tadao Santos, Laura Camila Diniz Couto, Andrea Boldarini Baldan, Maurício Ribeiro Ferreira, Neidenêi Gomes Abstract in English: This paper presents the electrolyte influence on deposition and dissolution processes of Cu nanoparticles on boron doped diamond electrodes (BDD). Morphological, structural and electrochemical analysis showed BDD films with good reproducibility, quality and reversible in a specific redox system. Electrodeposition of Cu nanoparticles on DDB electrodes in three different solutions was influenced by pH and ionic strength of the electrolytic medium. Analyzing the process as function of the scan rate, it was verified a better efficiency in 0,5 mol L-1 Na2SO4 solution. Under the influence of the pH and ionic strength, Cu nanoparticles on DDB may be obtained with different morphologies and it was important for defining the desired properties. |
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Artigo Absolute and general assignment of constitutional isomers by mass spectrometry: the case of methylpiperidines Eberlin, Marcos N. Benassi, Mario Abstract in English: An absolute method is described via mass spectrometry (MS) for the structural assignment of isomers within the class of methylpiperidines. The method explores both the unimolecular and bimolecular gas phase behavior of structurally diagnostic fragment ions (SDFI). For the methylpiperidnes, the isomeric 2-methyl, 3-methyl and 4-methyl 2-azabutadienyl cations are found to function as SDFI. These fragment ions are expected to be formed from all members within the class, to be stable and to retain the structural information of the precursor molecule, and to not interconvert into one another. To characterize these SDFI, both the collision induced dissociation (CID) in argon and bimolecular ion/molecule chemistry with ethyl vinyl ether were compared. |
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Artigo Lead and zinc in water and sediments of a metal mining and metallurgy area Melo, Vander de Freitas Andrade, Maísa de Batista, Araína Hulmann Favaretto, Nerilde Grassi, Marco Tadeu Campos, Mônica Soares de Abstract in English: Lead metallurgy at Adrianópolis is the largest environmental problem of Paraná, Brazil. The objective of this study was to determine Pb and Zn levels in water and sediment in two catchments by different extraction methods. The high levels of lead in water in most of samples do not allow the human use. Total Pb concentration as high as 795.3 µg L-1 was observed in Ribeira River bank, in a pluvial water stream flowering from a abandoned factory. Due to the high Pb levels in sediments from some sites (maximum of 24,300 mg kg-1) is recommended to avoid the water turbulence. |
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Artigo Photoelectrodegradation of AO7 dye by ZnO-TiO2 nanocomposite films Frade, Tânia Gomes, Anabela Pereira, Maria Isabel da Silva Lopes, Ana Ciríaco, Lurdes Abstract in English: The Zn-TiO2nanocomposite films were prepared by electrodeposition, using an acidic zinc sulphate solution with TiO2 nanoparticles in suspension. The as-deposited samples have been heated in air at 450 ºC for 6 h. The XRD and SEM analyses pointed out to the metal matrix conversion from Zn to ZnO and a rich morphology of needles-shaped grains. These materials were used on the photoelectrochemical degradation of AO7, which was efficiently degraded, with 40% of color removal, after 2 h period at 1.0 V, under white light irradiation. The apparent first order rate constant of the photoelectrodegradation reaction was 4.12 x 10-3 min-1. |
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Artigo Physico-chemical evaluation of an effluent treated in anaerobic biodigester regarding its efficience and application as fertilizer Silva, Wilson Tadeu Lopes da Novaes, Antonio Pereira de Kuroki, Vivian Martelli, Lilian Fernanda de Almeida Magnoni Júnior, Lourenço Abstract in English: The use of biodigester for basic and environmental sanitation has large demand in Brazil. A biodigester was built to treat conjunctly the human and pig feces and urine, regarding to its future application in rural small towns. The results show that the biodigester can reduce 90% of COD and BOD and, up to 99.99% of thermotolerant coliforms. The treated effluent has variable quantities of macro- and micro-nutrients; and organic matter. However, the concentration variability of the nutrients makes difficult a dosed application into soil. The soluble salts (mainly as Na+ form) make necessary a controlled use to avoid environmental degradation. |
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Artigo Potassium iodine supported on mesoporous molecular sieves (SBA-15 and MCM-41) as basic catalyst for synthesis of biodiesel Galvão, Luzia Patricia Fernandes de Carvalho Barbosa, Marcela Nascimento Araujo, Antonio Souza Fernandes Júnior, Valter José Santos, Anne Gabriela Dias Luz Jr, Geraldo E. Abstract in English: Iodide potassium incorporated on mesoporous molecular sieves (SBA-15 and MCM-41) was used as heterogeneous catalysts in the transesterification of sunflower oil under different conditions of reaction time and ratio catalyst/oil (w/w). The results have showed that the system supported in SBA-15 has been more active than the supported in MCM-41, promoting a conversion to methyl esters of 84.98%. |
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Organic and total mercury determination in sediments by cold vapor atomic absorption spectrometry: methodology validation and uncertainty measurements
Franklin, Robson L.
Bevilacqua, Jose E.
Favaro, Deborah I. T.
Abstract in English: The purpose of the present study was to validate a method for organic Hg determination in sediment. The procedure for organic Hg was adapted from literature, where the organomercurial compounds were extracted with dichloromethane in acid medium and subsequent destruction of organic compounds by bromine chloride. Total Hg was performed according to 3051A USEPA methodology. Mercury quantification for both methodologies was then performed by CVAAS. Methodology validation was verified by analyzing certified reference materials for total Hg and methylmercury. The uncertainties for both methodologies were calculated. The quantification limit of 3.3 µg kg-1 was found for organic Hg by CVAAS. |
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Artigo Study of an electrochemical method to sunflower oil to biodiesel conversion assessment Sousa, Rogério Adelino de Ribeiro, Caue Abstract in English: The development of analytical procedures to evaluate transesterification process is still a challenge in biodiesel production. Then, this paper shows an electroanalytical methodology to transesterification process assessment, proposing the application of nanostructured TiO2 electrodes. The results showed, for sunflower oil - methanol reaction catalyzed by KOH, a reduction peak in - 1050 mV and the gradual appearance of a second peak at - 1160 mV. This peak was observed as originated by the transesterification process and is probably related to intermediates. By measuring the intensity of this peak a kinetic profile was determined, showing that the conversion is almost finished in 2 h. |
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Artigo Quality of honey produced by Meipona fasciculata Smith of cerrado region from Maranhão state, Brazil Holanda, Carlos Alexandre Oliveira, Alene Ramos Costa, Maria Célia Pires Ribeiro, Maria Nilce de Sousa Souza, Janilson Lima Araújo, Maria José Abigail Mendes Abstract in English: The honey of Melipona fasciculata is few known in terms of composition, and therefore generally associated with the characteristics of the honey of Apis mellifera. This study contributes to the knowledge of the physico-chemical characteristics of honey of M. fasciculata of the municipalities of Barra do Corda, Jenipapo dos Vieiras, Fernando Falcão, Carolina and Riachão, in cerrado region from Maranhão. The parameters studied were: moisture, pH, acidity, reducing sugars, apparent sucrose, hydroxymethylfurfural, diastase activity, insoluble solids, ash and color. Some of the observed patterns may conform to the established for A. mellifera, but others must be accompanied by a specific legislation. |
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Artigo Evaluation of the corrosion resistance of stainless steel ISO 5832-9 and F138 implants removed from patients Silva, Elison da Fonseca e Oliveira, Luiz Fernando Cappa de Abstract in English: This work has compared the surfaces of two different steel samples used as orthopedical implants, classified as ASTM F138 and ISO5832-9, through optical emission spectroscopy, by means of SEM and EDS. The samples (implants) were also submitted to potentiodynamic cyclic polarization in Ringer lactate and NaCl 0.9 M L-1 solutions; ISO5832-9 sample did not show any kind of localized corrosion, but in the case of F138 steel was observed a pit localized corrosion in both solutions. In Ringer lactate solution it was observed a loss of about 63% for nickel and 26% for iron for F138 stell, compared to the initial composition. |
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Development and validation of a method for the analysis of Ochratoxin A in roasted coffee by liquid chromatography/electrospray-mass spectrometry in Tandem (LC/ESI-MS/MS)
Bandeira, Raquel D. C. C.
Uekane, Thais M.
Cunha, Carolina P. da
Geaquinto, Luths R. O.
Cunha, Valnei S.
Caixeiro, Janaina M. R.
Godoy, Ronoel Luiz O.
de la Cruz, Marcus Henrique C.
Abstract in English: A method using LC/ESI-MS/MS for the quantitative analysis of Ochratoxin A in roasted coffee was described. Linearity was demonstrated (r = 0.9175). The limits of detection and quantification were 1.0 and 3.0 ng g-1, respectively. Trueness, repeatability and intermediate precision values were 89.0-108.8%; 2.4-13.7%; 12.5-17.8%, respectively. To the best of our knowledge, this is the first report in which Ochratoxin A in roasted coffee is analysed by LC/ESI-MS/MS, contributing to the field of mycotoxin analysis, and it will be used for future production of Certified Reference Material. |
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Liquid-phase microextraction for simultaneous chromatographic analysis of three antidepressant drugs in plasma
Porto, Carlos Eduardo Dobrovolskni
Maia, Patrícia Penido
Freitas, Daniela Fernanda de
Araújo, Rafhaella Carolina Cedro
Siqueira, Maria Elisa Pereira Bastos de
Martins, Isarita
Santos-Neto, Álvaro José dos
Abstract in English: A method using Liquid Phase Microextraction for simultaneous detection of citalopram (CIT), paroxetine (PAR) and fluoxetine (FLU), using venlafaxine as internal standard, in plasma by high performance liquid chromatography with fluorescence detection was developed. The linearity was evaluated between 5.0 and 500 ng mL-1 (r > 0.99) and the limit of quantification was 2.0, 3.0 and 5.0 ng mL-1 for CIT, PAR and FLU, respectively. Therefore, it can be applied to therapeutic drug monitoring, pharmacokinetics or bioavailability studies and its advantages are that it necessary relatively inexpensive equipment and sample preparation techniques. |
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Artigo Modeling of the kinetics biodegradation of paclobutrazol in two soils of the semiarid northeast Brazil Vaz, Fernanda Leitão Maciel Netto, André Antonino, Antonio Celso Dantas Afonso, Antonio Cláudio Marques Martins, Jean Manuel Fonseca Gouveia, Ester Ribeiro Abstract in English: Mathematical models can help to prevent high levels of toxic substances in soil or fruits of plants treated with pesticides and indicate that such substances should be systematically monitored. The aim of this research was to study the kinetics of paclobutrazol biodegradation by soil native bacteria using mathematical models. Three models were used to assess the kinetics of paclobutrazol biodegradation obtained experimentally. Excellent fits were obtained using dual kinetic and logistic models. The use of glycerol as additional carbon source increased the biodegradation of PBZ and consequently decreased the time required for a given PBZ initial concentration be halved. |
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Artigo Simulation of natual weathering of zinc-carbon and alkaline batteries Câmara, Sílvio Carrielo Afonso, Júlio Carlos Silva, Lilian Irene Dias da Domingues, Nelma Nogueira Alcover Neto, Arnaldo Abstract in English: Spent alkaline and Zn-C batteries were placed in seawater, rainwater or landfill leachate at room temperature for up 30 days in order to simulate natural weathering. After the experiments pH and electrical conductivity of the liquid were measured. The precipitate formed and the filtrate were submitted to metal analysis by ICP-OES. Seawater is the most corrosive medium, followed by landfill leachate. Pb, Cd and Hg were mainly in the filtrate. Fe, Mn and Zn were generally dominant in the precipitate. Na and K account for the electrical conductivity and are good indicators of the corrosion stage of the batteries. |
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Artigo Use of recurrent neural networks for determination of 7-epiclusianone acidity constants in ethanol-water mixtures Costa, Éderson D' Martin Lemes, Nelson Henrique Teixeira Santos, Marcelo Henrique dos Braga, João Pedro Abstract in English: This work propose a recursive neural network to solve inverse equilibrium problem. The acidity constants of 7-epiclusianone in ethanol-water binary mixtures were determined from multiwavelength spectrophotmetric data. A linear relationship between acidity constants and the %w/v of ethanol in the solvent mixture was observed. The proposed method efficiency is compared with the Simplex method, commonly used in nonlinear optimization techniques. The neural network method is simple, numerically stable and has a broad range of applicability. |
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Artigo Analysis and discrimination of the chemotypes of Lippia graveolens H.B.K. of guatemala by solid phase microextraction, GC-MS and multivariate analysis Pérez Sabino, Juan Francisco Mérida Reyes, Max Farfán Barrera, Christian Daniel Silva, Antonio Jorge Ribeiro da Abstract in English: SPME-GC-MS, PCA and HCA multivariate techniques were used in order to evaluate their applicability to discriminate the three chemotypes (thymol, carvacrol and mixed) described for L. graveolens of Guatemala. The leaves of L. graveolens are used for treatment of colds, bronchitis, and as seasoning for food preparations, yielding essential oil up to 4.34 %. Leaves of 35 individuals from eight populations, and eight composite samples were analyzed using a DVB/Carboxen/PDMS fiber and GC-MS. PCA and HCA were carried out using eight markers (p-cymene, cis-sabinene hydrate, linalool, terpinen-4-ol, thymol, carvacrol, (E)-caryophyllene and caryophyllene oxide). The three chemotypes of L. graveolens were satisfactorily discriminated. |
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Artigo Effect of the association of clomazone in alginate/chitosan nanoparticles under soil sorption Silva, Mariana dos Santos Cocenza, Daniela Sgarbi Rosa, André Henrique Fraceto, Leonardo Fernandes Abstract in English: Agrochemicals constitute the class of products most commonly found in water resources. Their high level of concentration is due to the fact that less than 0.1% of pesticides applied to crops reach their target. The present work aims to study the sorption of clomazone herbicide (associated or not with nanoparticles). The sorption tests, performed with the 2(4) factorial design, showed that the form of herbicide is the main factor for sorption of clomazone. The application of nanoparticles as delivery system for agrochemicals is a pressing area of study and can contribute for decrease in effects of clomazone in the environment. |
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Artigo Assessment of the catalytic properties of bismuth compounds in soybean oil methanolysis Silva, Fabiano Rosa da Brugnago, Ricardo José Marangoni, Rafael Cordeiro, Claudiney Soares Nakagaki, Shirley Wypych, Fernando Ramos, Luiz Pereira Abstract in English: Sodium bismuthate dihydrate and two species derived from its thermal treatment were investigated as catalysts for soybean oil methanolysis and, regardless of the type of solid used, ester yields always above 76 wt% were obtained. After a single reaction course, both liquid and solid phases were characterized using several analytical methods such as X-ray diffraction and thermogravimetric analysis. As a result, the catalytic phenomenon was shown to be solely due to the leaching of alkalinecatalytic species from the solid materials. |
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Artigo Flow-injection spectrophotometric determination of glyphosate in commercial formulations of herbicides Silva, Aline Santana da Pezza, Leonardo Pezza, Helena Redigolo Abstract in English: A flow injection spectrophotometric procedure for the determination of glyphosate in commercial formulations of herbicides is proposed. The determination is based on the reaction of glyphosate and p-dimethylaminocinnamaldehyde, in acid medium, yielding a colored compound (l máx = 495 nm). Under optimal conditions, Beer's law is obeyed in a concentration range 40-640 mg mL-1 with a correlation coefficient of 0.9996. The detection limit was 8.60 mg mL-1 for glyphosate. The method was successfully applied for the determination of glyphosate in commercial formulations of herbicides. Recovery of glyphosate from various commercial samples of herbicides range from 91.0 to 110%. |
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Artigo Biodiesel production via ethylic transesterification with basic zeolites Ghesti, Grace F. Macedo, Julio L. de Dias, José A. Dias, Sílvia C. L. Abstract in English: Soybean oil transesterification with ethanol was carried out in a batch reactor using USY zeolites modified with barium and strontium (15 wt.%) as catalysts. A series of three catalytic cycles were performed for each zeolite without any loss of activity. The biodiesel product was analyzed by HPLC and FT-Raman, and the catalysts by pyridine and CO2 adsorption. Ba/USY provided higher conversions (> 97%) than Sr/USY (< 75%). The increased catalytic activity of Ba/USY was attributed to two different effects: a larger number of basic sites; and a lower interaction between barium species and HUSY BrØnsted sites. |
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Artigo Synthesis and characterization of acrylic beads obtained by suspension polymerization process for use as pharmaceutical excipient for direct compression Villanova, Janaina Cecília Oliveira Lima, Tadeu Henrique Patrício, Patrícia Santiago Pereira, Fabiano Vargas Ayres, Eliane Abstract in English: One of the difficulties reported for the suspension polymerization is control the size and granulometry of beads. The purpose of this work was to evaluate the use of cellulose nanowhiskers and mesoporous silica as stabilizers to reduce the size and the particle distribution. To monitor polymerization process was used FTIR-ATR spectroscopy. The morphology was analyzed by scanning electron microscopy. The particle size distribution was characterised using a CILAS granulometer. Thermal stability was studied by thermogravimetric analysis. The results indicated that cellulose nanowhiskers may provide stabilization and increase the thermal stability of the beads in contrast to mesoporous silica. |
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Artigo Development of nanocapsules of poly-ε-caprolactone containing herbicide atrazine Souza, Patrícia Moraes Sinohara Lobo, Fabiana Aparecida Rosa, André Henrique Fraceto, Leonardo Fernandes Abstract in English: In this study, polymeric nanocapsules of PCL containing the herbicide atrazine were prepared. In order to optimize the preparation conditions, a 2³ factorial design was performed using different formulations of nanocapsules, which investigated the influence of three variables at two levels. The factors varied were the quantities of PCL, Span 60 and Myritol. The results were evaluated considering the size, polydispersity, zeta potential and association rate and the measures of these parameters were taken immediately after preparation and after 30 days of preparation. The formulations with minimum level of polymer in the preparation showed better stability results. |
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Artigo Chemical constituents of the leaves from Rollinia leptopetala R. E. Fries Costa, Vicente Carlos de O. Tavares, Josean F. Queiroga, Cinthia S. Castello-Branco, Marianna V. S. Diniz, Margareth F. F. Melo Lima, Carolina Uchôa G. B. de Santos, Bárbara Viviana de O. Pita, João Carlos L. R. Silva, Marcelo Sobral da Sette, Ivana Maria Fechine Abstract in English: The phytochemical investigation of Rollinia leptopetala led to the isolation of a new compound named α-terpinyl caffeate, and five known compounds, being three sesquiterpenes, spathulenol, β-caryophyllene and 4β,10α-aromadendrane-diol, and two alkaloids, (-)-3-hydroxynornuciferine and (+)-norisocorydine. These alkaloids are being described for the first time in this genus. The structures of the compounds were determined by analysis of IR, MS and NMR data, as well as by comparison with literature data. The crude extract of R. leptopetala leaves demonstrated a weak cytotoxicity on sarcoma 180 cells with an IC50 of 512.3 µg/mL. However, the in vivo results showed that the extract exhibited a significant dose-dependent tumor growth reduction. |
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Artigo Production and characterization of ceramic foams obtained from Al-anodizing sludge Moraes, Graziela Guzi de Rodrigues Neto, João Batista Hotza, Dachamir Oliveira, Antonio Pedro Novaes de Oliveira, Bianca Goulart de Oliveira, Therezinha Maria Novais de Abstract in English: Ceramic foams were produced from a sludge generated in the aluminum anodizing process by using an industrial polyurethane foam (replication method) with open cell sizes of 10 ± 5 ppi (porosity = 97%) which were impregnated with suspensions containing 50-61 wt.% alumina, 1 wt.% citric acid, 6 wt.% bentonite and fired at 1600 ºC for 2 h. The aluminum anodizing sludge shows a high alumina content (87.5 wt.%) and a low particle size (~1.7 mm) after calcination and milling. The obtained filters show porosity of approximately 70%, filtration capability (mass water flow) of 1.7 kg/s and mechanical strength under compression of 2.40 MPa. |
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Revisão Designer drugs: analytical and biological aspects Bulcão, Rachel Garcia, Solange Cristina Limberger, Renata Pereira Baierle, Marília Arbo, Marcelo Dutra Chasin, Alice Aparecida da Matta Thiesen, Flávia Valladão Tavares, Rejane Abstract in English: In the recent years, analytical toxicologists have been facing difficulties in detecting designer drugs due to the chemical modifications on the existing structures and the speed in which they are released into the market, requiring the development and improvement of specific and appropriate analytical methods. This work is a review of the literature which summarizes the characteristics of the drugs and the analytical validated methods using conventional and unconventional matrices currently used for correct identification and quantification of the following classes of emerging drugs of abuse: derivatives of opiates, amphetamines, tryptamines, piperazines and cannabinoids. |
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Revisão Occurrence, behavior and environmental impacts caused by the presence of veterinary antimicrobials in soils Pereira, Leandro Alves Jardim, Isabel Cristina Sales Fontes Fostier, Anne Hélène Rath, Susanne Abstract in English: Antimicrobials, among other veterinary drugs, are used worldwide in industry and agriculture to protect animal health and prevent economic loss. In recent years, they have been detected in various environmental compartments, including soil, surface and groundwater and have become a topic of research interest. Emphasizing this class of compounds, this review presents the different pathways which veterinary drugs enter in the environment, in particular contaminate soils. Also are presented regulatory aspects and guidelines, adsorption/desorption and degradation of these compounds in soils and the consequences of its dispersal in the environment. |
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Nota técnica Speciation analysis of copper and zinc using differential pulse anodic stripping voltammetry Tonietto, Alessandra Emanuele Grassi, Marco Tadeu Abstract in English: This work describes methodologies for speciation analysis of the metals copper and zinc as total, total dissolved, labile, as well as complexation capacity (conditional stability constants and available ligand concentration), using the same technique, differential pulse anodic stripping voltammetry (DPASV). Several supporting electrolytes were tested, and the results showed that KNO3 and HNO3 resulted in voltamograms without interferences as well as excellent resolution for the total and labile fractions. The methodology using the DPASV technique allows a simple and low cost analysis of copper and zinc speciation, with high precision and sensitivity, with limits of quantification (LOQ) of 1.8 nmol L-1 for copper and 2.1 nmol L-1 for zinc. |
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Nota técnica Application of chemometric methods to the optimization of extraction of Ca, Mg, K, Fe, Zn, Cu and Mn in Brachiaria sp. leaves Souza, Diego M. Madari, Beata E. Sena, Marcelo M. Abstract in English: This work applied a 2² factorial design to the optimization of the extraction of seven elements (calcium, magnesium, potassium, iron, zinc, copper and manganese) in brachiaria leaves, determined by flame atomic absorption spectrometry. The factors sample mass and digestion type were evaluated at two levels: 200/500 mg, and dry/wet, respectively. Principal component analysis allowed simultaneous discrimination of all the significant effects in one biplot. Wet digestion and mass of 200 mg were considered the best conditions. The decrease of 60% in sample mass allowed to save costs and reagents. The method was validated through the estimation of figures of merit. |
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Nota técnica Saponification influence in carotenoid determination in cerrado passion fruit Wondracek, Daniele Cristina Vieira, Roberto Fontes Silva, Dijalma Barbosa da Agostini-Costa, Tânia da Silveira Sano, Sueli Matiko Faleiro, Fábio Gelape Abstract in English: This work describes the evaluation of the effect of saponification process in the carotenoid's content of three species of passion fruit. The results indicated the saponification of the extract was necessary to obtain cis-violaxanthin, trans-violaxanthin and β-cryptoxanthin hydrolyzed. These compounds were found in fruits of commercial P. edulis and yellow wild P. edulis. However, the extract saponification did not permitted to obtain free carotenes in fruits of wild purple P. edulis and P. setacea, and to trans-violaxanthin of P. cincinnata, therefore saponification was not indicated in the carotenoid analysis of these three accessions of passion fruit. |
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Nota técnica Multiresidue method validation for determination of pesticides in food using QuEChERS and UPLC-MS/MS Queiroz, Sonia C. N. Ferracini, Vera L. Rosa, Maria A. Abstract in English: This paper presents a practical and rapid method which was validated for simultaneous quantification and confirmation of 29 pesticides in fruits and vegetables using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were extracted following the method known as QuEChERS. Using the developed chromatographic conditions, the pesticides can be separated in less than 9 min. Two multiple reaction monitoring (MRM) assays were used for each pesticide. Four representative matrices (lettuce, tomato, apple and grapes) were selected to investigate the effect in recoveries and precision. Typical recoveries ranged from 70-120%, with relative standard deviation (RSDs) lower than 20%. |
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Gemifloxacin mesylate: UV spectrophotometric method for quantitative determination using experimental design for robustness
Paim, Clésio Soldateli
Führ, Fernanda
Steppe, Martin
Schapoval, Elfrides Eva Scherman
Abstract in English: This study describes the validation of UV spectrophotometric method for quantitative determination of gemifloxacin mesylate (GFM) in tablets using methanol as solvent. The method was specific, linear, precise, exact and robust at 272 and 343 nm. The results confirmed that the method in both wavelengths is valid and useful to the routine quality control of GFM in coated tablets. The validate method was compared to liquid chromatography (HPLC), microbiological assay and visible (VIS) spectrophotometry, which were previously developed and validated to the same drug. There was not significative difference between the methods for GFM quantitation. |
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Dispersive liquid-liquid microextraction for the simultaneous separation of trace amounts of zinc and cadmium ions in water samples prior to flame atomic absorption spectrometry determination
Mohammadi, Sayed Zia
Baghelani, Yar Mohammad
Mansori, Fatemeh
Shamspur, Tayebeh
Afzali, Daryoush
Abstract in English: In the proposed method, carbon tetrachloride and ethanol were used as extraction and dispersive solvents. Several factors that may be affected on the extraction process, such as extraction solvent, disperser solvent, the volume of extraction and disperser solvent, pH of the aqueous solution and extraction time were optimized. Under the optimal conditions, linearity was maintained between 1.0 ng mL-1 to 1.5 mg mL-1 for zinc and 1.0 ng mL-1 to 0.4 mg mL-1 for cadmium. The proposed method has been applied for determination of trace amount of zinc and cadmium in standard and water samples with satisfactory results. |
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Derivative spectrophotometric method for determination of acyclovir in polymeric nanoparticles
Tavares, Guilherme Diniz
Ishikawa, Gisele Miki
Monteiro, Talita Ferreira
Zanolini, Carolina
Kedor-Hackmann, Érika Rosa Maria
Bou-Chacra, Nádia Araci
Consiglieri, Vladi Olga
Abstract in English: A derivative spectrophotometric method was validated for quantification of acyclovir in poly (n-butylcyanoacrylate) (PBCA) nanoparticles. Specificity, linearity, precision, accuracy, recovery, detection (LOD) and quantification (LOQ) limits were established for method validation. First-derivative at 295.2 nm eliminated interferences from nanoparticle ingredients and presented linearity for acyclovir concentrations ranging from 1.25 to 40.0 µg/mL (r = 0.9999). Precision and accuracy data demonstrated good reproducibility. Recovery ranged from 99.3 to 101.2. LOD was 0.08 µg/mL and LOQ, 0.25 µg/mL. Thus, the proposed method proved to be easy, low cost, and accurate, and therefore, an useful alternative to quantify acyclovir in nanoparticles. |
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Development and validation of a stability-indicating HPLC method for the determination of buclizine hydrochloride in tablets and oral suspension and its application to dissolution studies
Kuminek, Gislaine
Stulzer, Hellen K.
Tagliari, Monika P.
Oliveira, Paulo R.
Bernardi, Larissa S.
Rauber, Gabriela
Cardoso, Simone G.
Abstract in English: A method using liquid chromatography has been developed and validated for determination of buclizine in pharmaceutical formulations and in release studies. Isocratic chromatography was performed on a C18 column with methanol:water (80:20 v/v, pH 2.6) as mobile phase, at a flow rate of 1.0 mL/min, and UV detection at 230 nm. The method was linear, accurate, precise, sensible and robust. The dissolution test was optimized and validated in terms of dissolution medium, apparatus agitation and rotation speed. The presented analytical and dissolution procedures can be conveniently adopted in the quality and stability control of buclizine in tablets and oral suspension. |
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Nota técnica Use of the linear light sensor ILX554 in optical spectroscopy Assirati, Lucas Terra, Idelma A. A. Nunes, Luiz A. O. Abstract in English: This technical note describes the construction of a low-cost optical detector. This device is composed by a high-sensitive linear light sensor (model ILX554) and a microcontroller. The performance of the detector was demonstrated by the detection of emission and Raman spectra of the several atomic systems and the results reproduce those found in the literature. |
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Nota técnica Development of an electrochemical microcell for studies of micro regions Akita, Adriano Heleno Barragan, José Tiago Claudino Fugivara, Cecílio Sadao Benedetti, Assis Vicente Abstract in English: The construction and optimization of a device that can be applied to electrochemical studies in flat micro regions are described. This was developed as an attempt to study small regions of metallic samples, whose properties may differ completely from its macroscopic behavior and for studies in highly resistive medium. Some results were obtained for individual grains of polycrystalline samples, welded regions, pure copper, platinum, glassy carbon, single crystals of Cu-Zn-Al alloy, and steel in biodiesel without electrolyte intentionally added. The device showed to be useful for the proposed purpose, allowing to be automated and has potential possibilities of other applications. |
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Educação Teaching experiment of chemometrics for exploratory analysis of edible vegetable oils by mid infrared spectroscopy and principal component analysis: a tutorial, part I Souza, André Marcelo de Poppi, Ronei Jesus Abstract in English: This manuscript aims to show the basic concepts and practical application of Principal Component Analysis (PCA) as a tutorial, using Matlab or Octave computing environment for beginners, undergraduate and graduate students. As a practical example it is shown the exploratory analysis of edible vegetable oils by mid infrared spectroscopy. |
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