Editorial Fraudes, plágios e currículos Torresi, Susana I. Córdoba de Pardini, Vera L. Ferreira, Vitor F. |
Artigo Nióbia sintética modificada como catalisador na oxidação de corante orgânico: utilização de H2O2 e O2 atmosférico como oxidantes Carvalho, Kele T. G. Silva, Adilson C. Oliveira, Luiz C. A. Gonçalves, Maraisa Magriotis, Zuy M. Resumo em Inglês: In this work synthetic niobia was used to promote the oxidation of methylene blue dye in aqueous medium. The niobia was characterized by N2 adsorption/desorption, XRD and TG measurements. The presence of reactive species on the niobia surface strongly increased the oxidation rate of the methylene blue dye. The reaction mechanism was studied by ESI-MS suggesting that the oxidation of the organic dye involve oxidizing species generated mainly after previous treatment with H2O2. It can be observed that the catalyst is a good material in the activation of gas (atmospheric oxygen) or liquid (hydrogen peroxide) oxidant agent with a total discoloration of the dye solution after only 1 h of reaction. |
Artigo Uso da cinza da casca do arroz (CCA) obtida da geração de energia térmica como adsorvente de Zn(II) em soluções aquosas Chaves, Thiago Faheina Queiroz, Zilvanir Fernandes de Sousa, Diana Nara Ribeiro de Girão, José Hélio Saraiva Rodrigues, Esiana de Almeida Resumo em Inglês: The removal study was conducted using 1.00 g of the rice husk ash (RHA) and 20.0 mL solution with concentrations in the range of 10-1000 mg/L of Zn(II). The influence of contact time, initial metal concentration, agitation and pH of the removal process was investigated. Superior removals to 95% were obtained at the end of 24 h of contact. The agitation increased in 20% the removal of Zn(II), being needed only 5 min to reach the equilibrium. The adsorption process was studied by the models of isotherms of Langmuir, Freundlich and BET, obtaining results of R L and 1/n for a process favorable of adsorption. BET isotherm best represents the equilibrium adsorption. The results showed that the RHA has the largest capacity and affinity for the removal of Zn(II). |
Artigo Utilização de pelos de animais silvestres para monitoramento ambiental de Cd, Cr, Cu, Fe, Mn, Pb e Zn Brait, Carlos Henrique Hoff Antoniosi Filho, Nelson Roberto Furtado, Mariana Malzoni Resumo em Inglês: This study investigates the use of wild animal hair of C. brachyurus, C. thous and L. pardalis as biomonitors of trace metal at Parque Nacional das Emas, Brazil. Results reveal a strong correlation between Cd and Pb as well as Cu and Zn, which suggests a single source of emission. Most metals showed a lower or equal concentration than those obtained in previous studies. The research shows that monitoring may be performed only with Zn, Pb, Cd, and Cr because of statistical similarity and of a non-natural occurrence of large amounts of the material under analysis. |
Artigo Estudo de liberação e permeação in vitro do diclofenaco de dietilamônio em microemulsão gel-like Silva, José Alexsandro da Santana, Davi Pereira de Bedor, Danilo Galindo César Borba, Valeria Ferreira da Costa Lira, Ana Amélia Moreira Egito, Eryvaldo Socrates Tabosa do Resumo em Inglês: The goal of this study was to produce and characterize a new microemulsion gel-like carrier system (MEG) by using the pseudo-ternary phase-diagram concept. The diclofenac diethylamine (DDA) was incorporated in the MEG and its in vitro release and permeation profiles were performed using Franz-type diffusion cells. The results revealed that the commercial DDA emulgel provided significantly higher Kp of DDA (2.2-fold) as compared to the MEG. Similar data were obtained in the permeation studies in which DDA Kp 4.7-fold higher. Therefore, MEG presents higher potential as a topical delivery system for DDA when compared to the commercial DDA emulgel. |
Artigo Efeito da adição de precursores na produção de alcaloide anticancerígeno usando a técnica de planejamento experimental Justo, Oselys Rodriguez Haber-Perez, Victor Viana, Cláudia de Oliveira Alegre, Ranulfo Monte Resumo em Inglês: The effect of precursors on the anticancer alkaloid production by submerged fermentation using M. anisopliae 3935 was studied, according to complete experimental design 2² with three central points. The results showed that lysine was the most important variable, however, when both lysine and glucose were added to the fermentation medium, the alkaloid production reached, approximately, 17 mg L-1 after 120 hours of fermentation. Then, the scale-up of the process was carried out and these results were confirmed. Finally, 35 mg L-1 of alkaloid at 192 h were attained after increment of added aminoacid lysine. |
Artigo Efeitos de agentes oxidantes e oxigênio dissolvido na descoloração do azo corante acid orange 7 por fotólise e fotocatálise Lucilha, Adriana Campano Takashima, Keiko Resumo em Inglês: The decolorization of acid orange 7 azo dye by photolysis and photocatalysis by ZnO was investigated in the presence of oxidants such as NaClO3, NaBrO3, NaIO4, and K2S2O8 in an open reactor at 30 ºC. The decolorization was relatively fast at lower oxidants concentrations and slow rate at larger concentrations, except for persulfate in the photocatalysis. Concerning photolysis the rate constant enhanced gradually, except for chlorate, outreaching the obtained values by photocatalysis, at higher concentrations. The air saturation decreased the rate constant in both processes and indicated that the azo dye can be decolorized without dissolved oxygen in persulfate medium. |
Artigo Síntese e avaliação da atividade antimicrobiana de novas 4-tiazolidinonas obtidas a partir de formilpiridina tiossemicarbazonas Verçoza, George Leonardo Feitoza, Danniel Delmondes Alves, Antônio José Aquino, Thiago Mendonça de Lima, José Gildo de Araújo, Janete Magali Cunha, Ivana Gláucia B. Góes, Alexandre José da Silva Resumo em Inglês: Twelve novel 4-thiazolidinone derivatives (2a-l) have been synthesized by reacting formilpyridine thiosemicarbazones (1a-l) and anhydride maleic in toluene. Their chemical structures were confirmed by IR, ¹H and 13C NMR. The new compounds were submitted to in vitro evaluation against pathogenic Gram-positive, Gram-negative bacteria and yeasts. The findings obtained showed that the compounds 2a, 2d, 2e and 2g were effective against some of the bacterial strains used, whereas the compounds 2d, 2e and 2i exhibited a moderate antifungal activity against the yeast strains evaluated. An initial structure activity relationship (SAR) was established. |
Artigo Nutrientes (K, P, Ca, Na, Mg e Fe) em sedimentos (solos aluviais) e cultivares (feijão e milho) de praias e barrancos de rios de água branca: a bacia do purus no estado do Acre, Brasil Martins, Milta Mariane da Mata Costa, Marcondes Lima da Resumo em Inglês: The present research highlights the macronutrient abundance in the sediments of beaches and cliffs and cultivates in the river Purus and flowing, southwest of Amazon. The concentrations found in leaves and bean seeds and corn leaves reflect the mineralogical and chemical nature of those rich sediments in K2O and Na2O, which are formed by smectite, illite and K-feldspar. The factors of transfer of the elements in the corn leaves and bean (Ca>K>Na) and bean seeds (Na>K>Ca) demonstrate that the nutrient needs of the cultivate were found appropriately in the sediments (soils) of the beaches and cliffs. |
Combined application of continuous wavelet transform-zero crossing technique in the simultaneous spectrophotometric determination of perindopril and indapamid in tablets Pektaş, Gözde Dinç, Erdal Baleanu, Dumitru Resumo em Inglês: Signal processing methods based on the combined use of the continuous wavelet transform (CWT) and zero-crossing technique were applied to the simultaneous spectrophotometric determination of perindopril (PER) and indapamide (IND) in tablets. These signal processing methods do not require any priory separation step. Initially, various wavelet families were tested to identify the optimum signal processing giving the best recovery results. From this procedure, the Haar and Biorthogonal1.5 continuous wavelet transform (HAAR-CWT and BIOR1.5-CWT, respectively) were found suitable for the analysis of the related compounds. After transformation of the absorbance vectors by using HAAR-CWT and BIOR1.5-CWT, the CWT-coefficients were drawn as a graph versus wavelength and then the HAAR-CWT and BIOR1.5-CWT spectra were obtained. Calibration graphs for PER and IND were obtained by measuring the CWT amplitudes at 231.1 and 291.0 nm in the HAAR-CWT spectra and at 228.5 and 246.8 nm in BIOR1.5-CWT spectra, respectively. In order to compare the performance of HAAR-CWT and BIOR1.5-CWT approaches, derivative spectrophotometric (DS) method and HPLC as comparison methods, were applied to the PER-IND samples. In this DS method, first derivative absorbance values at 221.6 for PER and 282.7 nm for IND were used to obtain the calibration graphs. The validation of the CWT and DS signal processing methods was carried out by using the recovery study and standard addition technique. In the following step, these methods were successfully applied to the commercial tablets containing PER and IND compounds and good accuracy and precision were reported for the experimental results obtained by all proposed signal processing methods. |
Artigo Previsão das propriedades físicas do papel kraft por espectroscopia no infravermelho próximo (NIR) e regressão por mínimos quadrados parciais (PLS) Samistraro, Gisely Muniz, Graciela I. B. de Peralta-Zamora, Patricio Cordeiro, Gilcélia A. Resumo em Inglês: The main objective of the present work is represented by the characterization of the physical properties of industrial kraft paper (i.e. transversal and longitudinal tear resistance, transversal traction resistance, bursting or crack resistance, longitudinal and transversal compression resistance (SCT (Compressive Strength Tester) and compression resistance (RCT-Ring Crush Test)) by near infrared spectroscopy associated to partial least squares regression. Several multivariate models were developed, many of them with high prevision capacity. In general, low prevision errors were observed and regression coefficients that are comparable with those provided by conventional standard methodologies. |
Un método reproducible para obtener peg biramificado monofuncional de alta pureza Ramón, José A. Peniche, Carlos Castro, Fidel R. Sáez, Vivian M. Colás, Rosa M. Páez, Rolando Resumo em Inglês: PEGylation has become a widely applied technique to enhancing in vitro and in vivo stability of therapeutic proteins and to increasing materials biocompatibility. PEG branched structures have proven useful for protein and peptide modification. Furthermore, they may be better than linear structures for many purposes. This paper describes an improved procedure for obtaining 2-arms PEG based on L-lysine. The efficiency of the synthesis was not related to moisture of the raw materials. This procedure does not use hazardous reagents as previous protocols do. It implemented a purification process for obtaining the desired structure with high purity ( > 99%). Finally, the procedure described here allows the obtaining of others PEGylation reagents. |
Artigo Sorção do inseticida tiametoxam em latossolos sob efeito de fosfato e vinhaça Oliveira, Vitória de Souza de Lima, José Maria de Carvalho, Renato Fráguas de Rigitano, Renê Luís Oliveira Resumo em Inglês: Little information is available on the behavior of thiamethoxam in soils, whereas many studies show the effect of phosphate and vinasse in soils in Brazil. This study evaluated the sorption, desorption and retention of thiamethoxam in vinasse- and phosphate-amended samples of a dystrophic Red-Yellow Latosol (LVAd) and a distroferric Red Latosol (LVdf). The LVAd presented higher sorption of thiamethoxam. Phosphate did not affect the sorption or retention and vinasse increased the interaction of the compound with the soil particles, reducing desorption to the soil solution. |
Artigo Perfil espacial e temporal de poluentes nas águas da represa municipal de São José do Rio Preto, São Paulo, Brasil Melo, Camila de Almeida Moreira, Altair B. Bisinoti, Márcia Cristina Resumo em Inglês: In this manuscript, seasonal and spatial trends of water collected from two sampling places in the Preto River in the Turvo-Grande watershed were evaluated. Water samples were collected during June/07 to July/08 and parameters sulphate, total organic carbon, ammonia, conductivity, dissolved oxygen, temperature, dissolved total solids and nitrate were quantified. Seasonal trend indicated sanitary effluents as a point source of contamination in both sampling points. Vertical trends demonstrated that the Municipal Dam was not stratified and received a diffuse source of pollutants from flooding and agriculture runoffs. It was also verified that there is relatively fast ammonia consumption kinetics having a half-life time of 1.43 h which can explain the low ammonia concentrations found in these aquatic bodies. |
Artigo Determinação de As, Cd e Pb em amêndoas e mesocarpo de babaçu, sapucaia, xixá e castanha-do-pará por espectrometria de absorção atômica Souza, Marielle Garcia Vieira, Edivan Carvalho Oliveira, Pedro Vitoriano Resumo em Inglês: This work describes methods for the simultaneous determination of Cd and Pb by graphite furnace atomic absorption spectrometry and As by hydride generation atomic absorption spectrometry in Brazilian nuts. The samples (~ 0.300 g) were digested to clear solutions in a closed vessel microwave oven. The pyrolysis and atomization temperatures for simultaneous determinations of Cd and Pb were 1100 and 2100 °C, respectively, using 0.5% (w v-1) NH4H2PO4 + 0.03% (w v-1) Mg(NO3)2 as chemical modifier. The limits of detection (3Δ) were 3.8 μg kg-1 for As, 0.86 μg kg-1 for Cd and 13 μg kg-1 for Pb. The reliability of the entire procedures was confirmed by peach leaves (No. 1547 - NIST) certified reference material analysis and addition and recovery tests. The found concentrations presented no statistical differences at the 95% confidence level. |
Artigo Hidrocarbonetos policíclicos aromáticos (HPAS) em cachaça, rum, uísque e álcool combustível Galinaro, Carlos Alexandre Franco, Douglas Wagner Resumo em Inglês: The concentration of 15 polycyclic aromatic hydrocarbons (PAHs) in 57 samples of distillates (cachaça, rum, whiskey, and alcohol fuel) has been determined by HPLC-Fluorescence detection. The quantitative analytical profile of PAHs treated by Partial Least Square - Discriminant Analysis (PLS-DA) provided a good classification of the studied spirits based on their PAHs content. Additionally, the classification of the sugar cane derivatives according to the harvest practice was obtained treating the analytical data by Linear Discriminant Analysis (LDA), using naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, benz[b]fluoranthene, and benz[g,h,i]perylene, as a chemical descriptors. |
Artigo Aplicação de espectroscopias raman e infravermelho na identificação e quantificação de plastificantes em filmes comerciais de PVC esticável Souza, Michele Lemos de Corio, Paola Temperini, Marcia L. A. Temperini, José Aparício Resumo em Inglês: This paper reports the use of Raman and infrared techniques for the qualitative and quantitative analysis of plasticizers in polyvinylchloride (PVC) commercial films. FT-Raman marker bands were indentified for di-2-ethyl-hexyl adipate (DEHA) and di-2-ethyl-hexyl phthalate (DEHP), allowing for the rapid identification of these species in the commercial film. Quantitative analysis by FT-IR resulted in plasticizers concentrations ranging from 11 to 27% (w/w). Considering the little sample preparation and the low cost of the techniques, FT-IR and FT-Raman are viable techniques for a first assessment of plasticizers in commercial samples. |
Rapid and accurate hplc-dad method for the determination of the herbicide bispyribac-sodium in surface water, and its validation Kurz, Márcia H. S. Gonçalves, Fábio F. Martel, Samile Adaime, Martha B. Zanella, Renato Machado, Sérgio L. de O. Primel, Ednei G. Resumo em Inglês: A new method is described for the determination of the herbicide bispyribac-sodium in surface water, especially from river and irrigated rice water samples. The method involves extraction in solid phase and quantification by high performance liquid chromatography with diode array detection (HPLC-DAD). After optimization of the extraction and separation parameters, the method was validated. The method presented average recoveries of 101.3 and 97.7%, under repeatability and intermediate precision conditions, respectively, with adequate precision (RSD from 0.9 to 7.5%). The method was applied for the determination of bispyribac-sodium in surface water samples with a limit of detection of 0.1 μg L-1. |
Artigo Estudo das interações entre o complexo polieletrolítico trimetilquitosana/carboximetilcelulose e Cu+2, ácido húmico e atrazina em solução aquosa Campana-Filho, Sergio P. Britto, Douglas de Resumo em Inglês: The polyelectrolyte complex (PEC) resulting from the reaction of sodium carboxymethylcellulose (CMC) and N,N,N-trimethylchitosan hydrochloride (TMQ) was prepared and then characterized by infrared spectroscopy and energy dispersive X rays analysis. The interactions involving the PEC and Cu2+ ions, humic acid and atrazine in aqueous medium were studied. From the adsorption isotherms the maximum amount adsorbed (Xmax) was determined as 61 mg Cu2+/g PEC, 171 mg humic acid/g PEC and 5 mg atrazine/g PEC. The results show that the CMC/TMQ complex has a high affinity for the studied species, indicating its potential application to remove them from aqueous media. |
Antioxidant capacity of eugenol derivatives Hidalgo, María E. De la Rosa, Carlos Carrasco, Héctor Cardona, Wilson Gallardo, Claudio Espinoza, Luis Resumo em Inglês: Toxicity and antioxidant capacity of eugenol derivatives (E2 = 2-Methoxy-4-[1-propenylphenyl]acetate, E3 = 4-Allyl-2-methoxyphenylacetate, E4 = 4-Allyl-2-methoxy-4-nitrophenol, E5 = 5-Allyl-3-nitrobenzene-1,2-diol, E6 = 4-Allyl-2-methoxy-5-nitrophenyl acetate) were evaluated in order to determine the influence of the sustituents. E2-E6 were synthesized from eugenol (E1). E1 was extracted from cloves oil, and E2-E6 were obtained through acetylation and nitration reactions. Antioxidant capacity evaluated by DPPH (1, 1-Diphenyl-2-picrylhydrazil) and ORAC fluorescein demonstrated that E1 and E5 have a higher capacity and the minor toxicity evaluated by red blood cells haemolysis and the Artemia saline test. In accordance with our results, the compound's (E1-E5) use in the pharmaceutical, cosmetic and or food industries could be suggested. |
Artigo Fotocatálise heterogênea com TiO2 para oxidação de arsênio e sua remoção de águas por coprecipitação com sulfato férrico Mendes, Gisele Bellato, Carlos Roberto Marques Neto, José de Oliveira Resumo em Inglês: The oxidation of arsenic (As(III) to As(V)) in water samples was performed by heterogeneous photocatalysis using a TiO2 film immobilized inside a photochemical reactor. After oxidation, As(V) was removed from the water samples by coprecipitation with ferric sulfate. The final conditions of oxidation and arsenic removal (TiO2 film prepared with a suspension: 10% (w/v); pH: 7.0; oxidation time: 30 min and Fe3+ concentration: 50 mg L-1) were applied in natural water samples which were supplemented with 1.0 mg L-1 of As(III) to verify the influence of the matrix. After treatment, more than 99% of arsenic was removed from the water. |
Artigo Estudo da oxidação dos sulfetos sintéticos molibdenita (MoS2) e covelita (CuS) por Acidithiobacillus ferrooxidans via respirometria celular Francisco Junior, Wilmo E. Bevilaqua, Denise Garcia Júnior, Oswaldo Resumo em Inglês: This paper analyses the oxidation of covellite and molybdenite by Acidithiobacillus ferrooxidans strain LR using respirometric experiments. The results showed that both sulfides were oxidized by A. ferrooxidans, however, the covellite oxidation was much higher than molybdenite. Regarding the kinetic oxidation, the findings revealed that just molybdenite oxidation followed the classical Michaelis-Menten kinetic. It is probably associated with the pathway which these sulfides react to chemistry-bacterial attack, what is influenced by its electronic structures. Besides, experiments conducted in the presence of Fe3+ did not indicate alterations in molybdenite oxidation. Thus, ferric ions seem not to be essential to the sulfide oxidations. |
Artigo Correlação entre parâmetros da cinética de intumescimento com características estruturais e hidrofílicas de hidrogéis de poliacrilamida e metilcelulose Aouada, Fauze A. Muniz, Edvani C. Vaz, Carlos M. P. Mattoso, Luiz H. C. Resumo em Inglês: In this paper, the effects of acrylamide (AAm), methylcellulose (MC) contents, pH and ionic strength on kinetic, network and hydrophilic properties of polyacrylamide and methylcellulose hydrogels were investigated. The hydrogels were characterized by evaluating of network [average molecular weight between crosslinks (M C), crosslink density (q) and the number of elastically effective chains (Ve)], and kinetic parameters [diffusional exponent (n), diffusion constant (k) and diffusion coefficient (D)]. Such properties were controlled by adjusting of the AAm, MC contents, pH and ionic strength factors. Due to high hydrophilicity and fast water-uptake, the PAAm-MC hydrogels can be considered as materials for potential applications in agricultural fields, mainly in controlled release of water or pesticides. |
Artigo Estudo da adsorção de compostos sulfurados empregando zeólitas contendo zinco Malvesti, Álvaro L. Mignoni, Marcelo L. Scherer, Robison P. Penha, Fábio G. Pergher, Sibele B. C. Resumo em Inglês: This paper deals with an adosrption of sulphur compounds employing zeolites containing zinc. The zeolites employed were commercial NaY and Beta. The zinc was incorporated in three levels: 0.5; 1.0 and 5%. The sulphur compounds studied were benzothiophene and dibenzothiofene. The results showed that both zeolites can be employed for adsorption of benzothiophene and dibenzothiophene. The Zn incorporation (0.5%) promotes an increase in zeolites adsorption ability. The DBT adsorbs more than BT, probably because it strongly interacts with zeolite structure. The BT adsorbs more in NaY than in beta probably because the NaY zeolite has a high intern volume. This is not observed for DBT. |
Immobilization of laccase on hybrid layered double hydroxide Camacho Córdova, David Isidoro Morales Borges, Rogelio Arizaga, Gregorio Guadalupe Carbajal Wypych, Fernando Krieger, Nádia Resumo em Inglês: Crystals of Mg/Al layered double hydroxide were synthesized by alkaline precipitation and treated in an aqueous solution of glutamic acid. The glutamate ions were not intercalated into the interlayer space, but were detected in the material by Fourier transform infrared spectroscopy, suggesting that only the external surfaces of crystals were modified with glutamate ions. The resulting hybrid material was tested as a support for immobilization of the enzyme laccase (Myceliophthora thermophila). The immobilized enzyme preparation was characterized by electronic paramagnetic resonance spectroscopy and by assays of catalytic activity. The activity of the immobilized laccase was 97% of the activity in the free enzyme. Layered double hydroxide is a suitable support for use in remediation of soil studies. |
Artigo Validação de metodologia para a caracterização química de bagaço de cana-de-açúcar Gouveia, Ester Ribeiro Nascimento, Renata Trajano do Souto-Maior, Ana Maria Rocha, George Jackson de Moraes Resumo em Inglês: In this work, a methodology for the characterization of sugar cane bagasse was validated. Bagasse pre-treated with steam in a 5000 L reactor at a pressure of 15.3 kgf/cm², during 7 min, was used to test the methodology. The methodology consisted of the hydrolysis of the material with H2SO4 at 72% v/v, for the quantification of carbohydrates, organic acid, furfural and hydroxymethylfurfural by HPLC; insoluble lignin and ash by gravimetry; and soluble lignin by spectrophotometry. Linearity, repeatability, reproducibility and accuracy of the results obtained in two Research Laboratories were determined, and were considered to be suitable for the validation of the methodology. |
Artigo Degradação de espécies nitroaromáticas e remediação de efluentes da indústria de explosivos, utilizando-se processos redutivos-oxidativos fundamentados no uso de ferro metálico Cavalotti, Luiz Fernando Rocha Peralta-Zamora, Patricio Rodrigues, Marcio Barreto Paiva, Teresa Cristina Brazil de Resumo em Inglês: In this work the potentiality of reductive-oxidative processes based on zero-valent iron was studied aiming the degradation of nitroaromatic compounds and the remediation of residues from the explosive industry. The reductive process was applied as a continuous treatment system, using steel-wool as zero-valent iron source. The process permitted an almost total degradation of nitrobenzene, nitrophenol, nitrotoluene, dinitrotoluene and trinitrotoluene, probably with generation of the respective amine-derivative. The yellow-water residue, containing soluble trinitrotoluene, was notably modified by the reductive process, a fact that permitted a substantial enhancement of its biodegradability. Furthermore, the subsequent photo-Fenton process allowed TOC removal of about 80%. |
Artigo Constituintes químicos e atividade antioxidante de extratos das folhas de Terminalia fagifolia Mart. et Zucc Ayres, Mariane Cruz Costa Chaves, Mariana H. Rinaldo, Daniel Vilegas, Wagner Vieira Júnior, Gerardo Magela Resumo em Inglês: Phytochemical investigation of ethanolic leaves extracts of T. fagifolia led to the isolation of (+)-catechin, sitosterol-3-O-β-D-glucopyranoside, α- and β-tocopherol, a mixture of lupeol, α- and β-amyrin, sitosterol and a mixture of glicosid flavonoids (CP-13). The structures of these compounds were identified by ¹H and 13C NMR spectral analysis and comparison with literature data. Absolute configuration of the catechin was determinate by circular dichroism. Antioxidant activity (EC50), evaluated by 2,2-diphenyl-1-picrylhidrazyl (DPPH) assay system, decreased in the order: (+)-catechin > hydroalcoholic fraction > CP-13 > aqueous fraction > EtOH extract. |
Determination of ambroxol in syrups using diffuse reflectance spectroscopy Rufino, José L. Santos, Joel M. Rodrigues, Mayra A. Pezza, Helena R. Pezza, Leonardo Resumo em Inglês: This paper reports an analytical method for the determination of ambroxol in micellar medium by spot test-diffuse reflectance spectroscopy. The reflectance measurements were performed analyzing the colored compound (λ= 520 nm) produced from the reaction between ambroxol and p-dimethylaminocinnamaldehyde on the surface filter paper. The linear range was from 1.21 × 10"3 to 9.65 × 10"3 mol L-1 (500 - 4000 μg mL-1). The limit of detection and quantification were 3.50 x 10-4 mol L-1 (145 μg mL-1) and 1.16 x 10-3 mol L-1 (481 μg mL-1), respectively. Five commercial samples were analysed and the results obtained by the proposed method were in good agreement with those obtained by the literature method at 95% confidence level. |
Extracción de compuestos con actividad antioxidante de frutos de guayaba cultivada en Vélez-Santander, Colombia Restrepo-Sánchez, Diana-Chavely Narváez-Cuenca, Carlos-Eduardo Restrepo-Sánchez, Luz-Patricia Resumo em Inglês: The effects of the extraction system (50% methanol or 50% methanol pH 2.0), volume/material ratio, temperature, time and extractions with 70% acetone were evaluated in the total phenolic compounds (TPC) extraction and in antioxidant activities (AA) using FRAP and ABTS assays in guava fruit. The best yield was obtained when 0.5 g of guava were extracted first with 20 mL 50% methanol and then four times with 20 mL 70% acetone during 30 min at 50 °C. Among the different trials guava fruit exhibited high levels of AA as well as TPC. |
Artigo Composição fenólica, atividade antibacteriana e antioxidante da própolis vermelha brasileira Cabral, Ingridy Simone Ribeiro Oldoni, Tatiane Luiza Cadorin Prado, Adna Bezerra, Rosângela Maria Neves Alencar, Severino Matias de Ikegaki, Masaharu Rosalen, Pedro Luiz Resumo em Inglês: Propolis is a resinous hive product collected by honeybees from various plant sources. It has a complex chemical composition, constituted by various phenolic compounds. Extracts of increasing polarity (n-hexane, chloroform, and ethanol) were obtained from a sample of red propolis from the state of Alagoas. Assays were carried out for determination of contents of phenolics, along with antibacterial and antioxidant activities. The EEP, fractions and sub-fractions showed strong biological activities and were related with phenolic the content compounds contents. The sub-fractions were more bioactive than the EEP and fractions, demonstrating that the antioxidant and antibacterial activities are not a result of synergistic effect between the various chemical compounds in propolis. |
Artigo Composição molecular e origem paleobotânica de âmbares da bacia do Araripe, Formação Santana Pereira, Ricardo Carvalho, Ismar de Souza Fernandes, Antônio Carlos Sequeira Azevedo, Débora de Almeida Resumo em Inglês: The terpenoid composition of seven amber samples from Araripe Basin (Santana Formation, Crato Member) has been analyzed by gas chromatography-mass spectrometry to determine their botanical origin. The diterpenoids, which have been identified in the fossil resin extracts are derived primarily from the abietane class, e.g., dehydroabietane, 4-epidehydroabietol, 16,17,18-trisnorabieta-8,11,13-triene, 7-oxo-16,17,19-trisnorabieta-8,11,13-trieno, dehydroabietic acid, ferruginol, hinokiol and hinokione. Their composition is certainly typical for conifers, and angiosperms can be excluded as the botanical source, as no triterpene was identified. The terpenoid characteristics strongly support a relationship to the Araucariaceae or Podocarpaceae families. In addition, the fossil record of the embedding sediments (pollen and fossil leaves) also supports the proposal of these paleobotanical origins for the ambers. |
Artigo Parâmetros indicativos do processo de salinização em rios urbanos do semi-árido brasileiro Santos, José Soares dos Santos, Marcio José Silva dos Santos, Maria Lúcia Pires dos Resumo em Inglês: This study examined the spatial and temporal variations of six important parameters of the salt accumulation process in water samples collected along section urban of Contas River. The Na+, K+, Ca2+ and Mg2+ concentrations were determined by FAAS. The conductivity, total dissolved solids, Na+ and Ca2+ presented the largest seasonal and spatial variations in the urban area demonstrated that are appropriate indicators of urban contamination. The readily soluble salts in drainage urban, contribute for the degradation of the water of rivers located in semi-arid zones. |
Artigo Produção de monoacilgliceróis e diacilgliceróis via glicerólise enzimática e destilação molecular Fregolente, Patricia Bogalhos Lucente Pinto, Gláucia Maria F. Wolf-Maciel, Maria Regina Maciel Filho, Rubens Batistella, César Benedito Resumo em Inglês: Monoacilglycerides and diacilglycerides are produced through lipase-catalyzed glycerolysis of soybean oil using Candida antarctica B in a solvent-free system. The reaction was carried out at a glycerol to triacylglycerol molar ratio of 8:1 with 2% of lipase. Acylglycerides, free fatty acids (FFA) and glycerol produced were separated employing the molecular distillation process. Starting from a product of enzymatic reaction 25.06% of triacylglycerols, 46.63% of diacylglycerides, 21.72% of monoacylglycerides, 5.38% of FFA and 1.21% of glycerol and after consecutively distillations, monoacylglycerides with 80% of purity was obtained and also oil with 54% of diacylglycerides to be used in human dietary. |
Artigo Variação sazonal da composição do óleo essencial de Myrcia salzmannii Berg. (Myrtaceae) Cerqueira, Martins Dias de Marques, Edson de Jesus Martins, Dirceu Roque, Nídia F. Cruz, Frederico Guaré Guedes, Maria Lenise da Silva Resumo em Inglês: This work report the seasonal variation of composition of the volatile oils from leaves and from flowers of Myrcia salzmannii harvested in the sand dunes of Salvador, Bahia, northeastern region of Brazil in the years 2001 and 2003. The oils were analyzed by GC-FID and GC-MS being identified 49 components. Nine essential oil samples of leaves collected on different months and years and one sample of flowers were analyzed. β-Caryophyllene and α-humulene were the only compounds present in all of the samples being the first the majority compound. |
Artigo Bioacetilação de álcoois catalisada por Saccharum officinarum Assunção, João Carlos C. Lemos, Telma Leda G. Monte, Francisco José Q. Resumo em Inglês: Lipase-catalysed esterifications of alcohols using immobilized enzyme system from sugar cane (Saccharum officinarum) as biocatalyst afforded the corresponding esters in considerable yields (68-93%). Under optimized conditions, the material was utilized for reactions of acetylation with several advantage. It also investigated the possibility of reuse of immobilized enzymes of S. officinarum as biocatalyst under optimal reaction conditions. |
Artigo Constituintes químicos e atividade inseticida dos extratos de frutos de Trichilia elegans E T. catigua (Meliaceae) Matos, Andréia Pereira Nebo, Liliane Vieira, Paulo Cezar Fernandes, João Batista Silva, Maria Fátima das Graças Fernandes da Rodrigues, Ricardo Ribeiro Resumo em Inglês: Phytochemical investigation of the fruits extracts of Trichilia elegans and Trichilia catigua (Meliaceae) has led to the identification of the limonoids 11β-acetoxyobacunone, cedrelone, methylangolensate and epimeric mixture of photogedunin besides known coumarins (scoparone, scopoletin, umbeliferone) and the steroids stigmasterol, β-sitosterol, sitostenone and campesterol. The structures of the compounds were proposed by spectroscopic analysis and comparison with literature data. An evaluation of the insecticidal activity of the fruits extracts of Trichilia ssp. was carried out and the extracts of T. elegans revealed to have strong insecticidal activity and the extracts of T. catigua showed moderate larval mortality on Spodoptera frugiperda. |
Synthesis and antitubercular activity of isoniazid condensed with carbohydrate derivatives Cardoso, Sílvia H. Assis, João Vítor de Almeida, Mauro V. de Lourenço, Maria Cristina S. Vicente, Felipe R. C. Souza, Marcus V. N. de Resumo em Inglês: A series of 13 compounds analogous of isoniazid condensed with carbohydrate was synthesized and evaluated for their in vitro antibacterial activity against Mycobacterium tuberculosis H37Rv using Alamar Blue susceptibility test and the activity expressed as the minimum inhibitory concentration (MIC90) in μg/mL. Several compounds exhibited antitubercular activity (0.31-3.12 μg/mL) when compared with first line drugs such as isoniazid (INH) and rifampicin (RIP) and could be a good starting point to develop new compounds against tuberculosis. |
Artigo Remoção de compostos orgânicos em água empregando carvão ativado impregnado com óxido de ferro: ação combinada de adsorção e oxidação em presença de H2O2 Castro, Cínthia S. Guerreiro, Mário C. Oliveira, Luiz C. A. Gonçalves, Maraísa Resumo em Inglês: In this work, composites based on activated carbon/iron oxide (AC/Fe) were prepared in two different proportions (AC/Fe 5/1 and 1/1) and evaluated in the removal of the organic dye methylene blue (MB). Physical-chemical properties of the composites were determined by X-ray diffraction (XRD), adsorption/dessorption of N2 isotherm, temperature programmed reduction (TPR) and scanning electron microscopy (SEM). Results showed that goethite (α- FeOOH), with nanometer particle size, was formed over carbon surface for both composites. These materials showed high efficiency to remove MB from solution by combined adsorption and oxidation process. The AC/Fe 1/1 showed to be more active in (MB) oxidation then AC/Fe 5/1. |
Artigo Alcaloides e outros constituintes de Xylopia langsdorffiana (Annonaceae) Silva, Marcelo Sobral da Tavares, Josean Fechine Queiroga, Karine Formiga Agra, Maria de Fátima Barbosa Filho, José Maria Almeida, Jackson Roberto Guedes da Silva Silva, Sâmia Andrícia Souza da Resumo em Inglês: The phytochemical investigation of Xylopia langsdorffiana led to the isolation of corytenchine, xylopinine, discretamine, xylopine, ent-atisan-16α-hydroxy-18-oic acid, 13² (S) hydroxy-17³-ethoxyphaephorbide and quercetin-3-α-rhamnoside. Their structures were assigned based on spectroscopic analyses, including two-dimensional NMR techniques. Antioxidant activities of discretamine were measured using the 1,2-diphenyl- 2-picryl-hydrazyl (DPPH) free radical scavenging assay. |
Artigo Validação da metodologia da avaliação de incerteza em curvas de calibração melhor ajustadas por polinômios de segundo grau Oliveira, Elcio Cruz de Aguiar, Paula Fernandes de Resumo em Inglês: The most widespread literature for the evaluation of uncertainty - GUM and Eurachem - does not describe explicitly how to deal with uncertainty of the concentration coming from non-linear calibration curves. This work had the objective of describing and validating a methodology, as recommended by the recent GUM Supplement approach, to evaluate the uncertainty through polynomial models of the second order. In the uncertainty determination of the concentration of benzatone (C) by chromatography, it is observed that the uncertainty of measurement between the methodology proposed and Monte Carlo Simulation, does not diverge by more than 0.0005 unit, thus validating the model proposed for one significant digit. |
Revisão Traçadores: o uso de agentes químicos para estudos hidrológicos, ambientais, petroquímicos e biológicos Silva, Láuris Lucia da Donnici, Claudio Luis Ayala, José Danilo Freitas, Cíntia Helena de Moreira, Rubens Martins Pinto, Amenônia Maria Ferreira Resumo em Inglês: This paper presents a revision of the history, definitions, and classification of tracers (natural and artificial, internal and external). The fundamental ideas concerning tracers are described, followed by their application illustrated by typical examples. The advantages and disadvantages of five classes among the most frequently used external tracers (fluorescent, microbial, chemical, radioactive and activable isotopes) are also described in detail. This review also presents some interesting and modern applications of tracers in the areas of diagnostics in medical practice, environmental pollution, hydrology and petroleum chemistry. |
Revisão Relevância de compostos de baixa massa molar produzidos por fungos e envolvidos na biodegradação da madeira Arantes, Valdeir Milagres, Adriane M. F. Resumo em Inglês: Over the last decade, evidences have been shown that the wood biodegradation by fungi is not only a result of the action of their enzymatic machinery but also of various low molecular weight non-enzymatic compounds, especially in fungi that promote brown and white decay, which in nature are the major wood decaying microorganisms. The present review focuses on the recent theories involving these low molecular weight compounds that act direct or synergistically with lignocellulolytic enzymes to attack the wood main macromolecular constituents, their relevance as potential degradative systems, in the overall wood biodegradation, and also outlines their potential biotechnological applications. |
Revisão Biodiesel: parâmetros de qualidade e métodos analíticos Lôbo, Ivon Pinheiro Ferreira, Sérgio Luis Costa Cruz, Rosenira Serpa da Resumo em Inglês: The establishment of quality standards for biodiesel was a key step to win the confidence of the market and the automotive industry, thus ensuring the success of the new fuel. In this review are presented standard methods and other analytical methods suggested for analysis of biodiesel. The methods of analysis were divided into groups according to information that may be provided on the contaminants from the raw material of the production process, the molecular structures of biodiesel and its degradation during storage. |
Revisão Polímeros com capacidade de reconhecimento molecular no controlo da libertação de fármacos. Parte 1: síntese e caracterização Sousa, Margarita Domingues Barbosa, Carlos Maurício Resumo em Inglês: Molecularly imprinted polymers (MIPs) consist of synthetic macromolecular matrix, obtained through molecular imprinting-based methods that show ability to selectively recognize important biological molecules and its application in the drug delivery field is under development. In the present review the main aspects related to the synthesis and characterization of MIPs are studied. The fundamental variables participating in the synthesis process, such as template molecule, functional monomers, cross-linking agents, solvents and imprinting approaches are discussed. Moreover, the main available methods for MIPs chemical and morphological characterization are presented and the importance of the obtained information is discussed. |
Revisão QuEChERS: um método moderno de preparo de amostra para determinação multirresíduo de pesticidas em alimentos por métodos cromatográficos acoplados à espectrometria de massas Prestes, Osmar D. Friggi, Caroline A. Adaime, Martha B. Zanella, Renato Resumo em Inglês: This review attempts to provide an updated overview of the Quick, Easy, Cheap, Effective, Ruged and Safe (QuEChERS) multiresidue extraction method, that involves initial extraction in acetonitrile, an extraction/partition step after the addition of salt, and a cleanup step utilizing dispersive solid phase extraction. QuEChERS method is nowadays the most applied extraction method for the determination of pesticide residues in food samples, providing acceptable recoveries for acidic, neutral and basic pesticides. Several applications for various food matrices (fruits, vegetables, cereals and others) in combination with chromatographic mass spectrometry analysis were presented. |
Revisão Sensores ópticos com detecção no infravermelho próximo e médio Lima, Kássio M. G. Raimundo Jr., Ivo M. Silva, Andréa Monteiro S. Pimentel, Maria Fernanda Resumo em Inglês: Optical chemical sensors with detection in the near and mid infrared region are reviewed. Fundamental concepts of infrared spectroscopy and optical chemical sensors are briefly described, before presenting some aspects on optical chemical sensors, such as synthesis of NIR and IR reagents, preparation of new materials as well as application in determinations of species of biological, industrial and environmental importance. |
Nota técnica Autoamostrador de baixo custo para análise por injeção em fluxo Kamogawa, Marcos Y. Teixeira, Marcelo Alves Resumo em Inglês: This paper describes a homemade autosampler for flow injection analysis (FIA), constructed with two step motors from old floppy disk drives (5¼-inch). The autosampler was connected to a computer through the parallel port and the sampling process was controlled by software in Quick Basic. The performance of the system was assessed by the determination of ammonium, based on the gaseous diffusion into a bromocresol purple solution, following the spectrophotometric determination of change in absorbance. The easy and simple construction is the main characteristics of this equipment and analytical results with RSD lower than 1% were obtained. |
Determination of nitrate in lettuce by ion chromatography after microwave water extraction Novaes, Humberto Brevilato Vaitsman, Delmo Santiago Dutra, Paulo Bechara Pérez, Daniel Vidal Resumo em Inglês: Lettuce is worldwide known as the most important vegetable. In this context, most farmers are searching new techniques for best quality products including hydropony. However, nitrate is of great concern, since it has a negative impact on human metabolism. The main objective of the present work was to evaluate the nitrate content of lettuce produced by conventional and hydroponic systems. The determination was conducted by ion chromatography and a new method of extraction was tested using microwave oven digestion. The results indicated that nitrate level produced in the conventional system was lower than in the hydroponic system. |
Nota técnica Construção de um calorímetro isotérmico diferencial de alta sensibilidade e baixo custo Trinca, Rafael Bergamo Perles, Carlos Eduardo Volpe, Pedro Luiz Onófrio Resumo em Inglês: The high cost of sensitivity commercial calorimeters may represent an obstacle for many calorimetric research groups. This work describes the construction and calibration of a batch differential heat conduction calorimeter with sample cells volumes of about 400 μL. The calorimeter was built using two small high sensibility square Peltier thermoelectric sensors and the total cost was estimated to be about US$ 500. The calorimeter was used to study the excess enthalpy of solution of binary mixtures of liquids, as a function of composition, for the following binary systems of solvents: water + 1,4-dioxane or + dimethylsulfoxide at 298,2 ± 0,5 K. |
Nota técnica Comparação de diferentes abordagens para avaliação da incerteza na cromatografia gasosa do gás natural Oliveira, Elcio Cruz de Aguiar, Paula Fernandes de Resumo em Inglês: The evaluation of uncertainty associated with an analytic result is an essential part of the measurement process. Recently, several approaches to evaluate the uncertainty in measurement have been developed. Here, the gas chromatography assay uncertainty for natural gas is compared by some of these approaches: the guide to the expression of uncertainty in measurement (GUM) approach, top-down approach (reproducibility estimate from an inter-laboratory study), Barwick & Ellison (data from validation), study of variability and fuzzy approach. The comparison shows that GUM, Barwick & Ellison and fuzzy approaches lead to comparable uncertainty evaluations, which does not happen with the top-down approach and study of variability by the absence of data normality. |
Educação Termogravimetria: um novo enfoque para a clássica determinação de cálcio em cascas de ovos Pereira, Júnia G. Okumura, Fabiano Ramos, Luiz A. Cavalheiro, Éder T. G. Nóbrega, Joaquim A. Resumo em Inglês: The use of thermoanalytical data in sample preparation is described as a tool to catch the students' attention to some details that can simplify both the analysis and the analytical procedure. In this case, the thermal decomposition of eggshells was first investigated by thermogravimetry (TGA). Although the classical procedures suggest long exposure to high temperatures, the TGA data showed that the decomposition of organic matter takes place immediately when the sample is heated up to 800 °C under air atmosphere. After decomposition, the calcium content was determined by flame atomic emission photometry and compared with the results obtained using classical volumetric titration with EDTA. |
Educação Oxidação do borneol à cânfora com água sanitária - um experimento simples, de baixo custo e limpo Santos, Ana Paula Bernardo dos Gonçalves, Idila Rafaela Carvalho Pais, Karla Ceodaro Martinez, Sabrina Teixeira Lachter, Elizabeth Roditi Pinto, Angelo C. Resumo em Inglês: Regulatory pressure is increasingly focusing on the use and disposal of substances hazardous to human health and environment. In the last years efforts have also been made to introduce green chemistry concepts in undergraduate courses. In this paper we present an experiment on the oxidation reaction of borneol to camphor with bleach in acetone. This experiment is important to show undergraduate students that a cheap and non hazardous commercial product can be a useful oxidation agent of alcohols. |
Educação Extração e purificação de clorofila a, da alga Spirulina maxima: um experimento para os cursos de química Maestrin, Ana Paula Jecks Neri, Cláudio Roberto Oliveira, Kleber Thiago de Serra, Osvaldo Antonio Iamamoto, Yassuko Resumo em Inglês: This work describes a simple and economical experiment for the extraction and purification of chlorophyll a from Spirulina maxima. Extraction and purification of natural compounds can be considered one of the most illustrative experiments that can be performed in Organic Chemistry courses. Particularly, the chromatography of dyes and pigments allows students to have a better comprehension of the chromatography separations. These compounds represent an important class of organic pigments applied in pharmaceutical, cosmetic, detergent compositions, and various other fields and can be extracted from plants and algae. To extract, separate and purify chlorophyll a from associated pigments such as xanthophylls, carotenes, and pheophytins, very costly processes are reported. The present approach is perfectly adequate for use in Chemistry experiments for undergraduate students. |
Educação Hidrólise parcial da superfície do polyethylene terephthalate (PET): transformando um rejeito em um material de troca catiônica para aplicação ambiental Rosmaninho, Marcelo G. Jardim, Erika Ferreira, Gilmara L. Araújo, Maria H. Lago, Rochel M. Moura, Flávia C. C. Resumo em Inglês: In this work it is proposed a simple and versatile undergraduate chemical experiment in polymer and environmental technology based on the process of polyethylene terephthalate (PET) hydrolysis. Polyethylene terephthalate from post-consume bottles is submitted to a controlled partial hydrolysis which allows the students to follow the reaction by a simple procedure. The students can explore the reaction kinetics, the effect of catalysts and the exposed polyethylene terephthalate surface area on the hydrolysis reaction. The second and innovative part of this experiment is the technological and environmental application of the hydrolyzed polyethylene terephthalate as a material with cation exchange properties. The surface hydrolyzed polyethylene terephthalate can be used as adsorbent for cationic contaminants. |
The pre-history of cryoscopy: what was done before raoult? Reif-Acherman, Simón Resumo em Inglês: Cryoscopy is considered one of the foundations of the modern theory of solutions and of physical chemistry. This paper shows in order the first regularities pointed out by several scientists on the subject, in the first chapter of its birth as a scientific discipline. The study is focused on the identification of the different steps that helped, first qualitatively and then quantitatively, to adjust the different classes of possible solutions, including those that formed hydrates, to a basic formulation that the French scientist François-Marie Raoult would later generalize in the law that bears his name. |
Assuntos gerais Carta ao editor Ferraz, Márcia H. M. |