Table of contents
Química Nova, Volume: 36, Issue: 5, Published: 2013Química Nova, Volume: 36, Issue: 5, Published: 2013
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Editorial 36ª Reunião Anual da SBQ Zarbin, Aldo J. G. |
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Use of sorghum straw (Sorghum bicolor) for second generation ethanol production: pretreatment and enzymatic hydrolysis
Cardoso, Wilton Soares
Tardin, Flávio Dessaune
Tavares, Gabriella Peterlini
Queiroz, Paula Viana
Mota, Samuel Sampaio
Kasuya, Maria Catarina Megumi
Queiroz, José Humberto de
Abstract in English: Agronomic biomass yields of forage sorghum BRS 655 presented similar results to other energy crops, producing 9 to 12.6 tons/ha (dry mass) of sorghum straw. The objective of this study was to evaluate the lignocellulosic part of this cultivar in terms of its potential in the different unit processes in the production of cellulosic ethanol, measuring the effects of pretreatment and enzymatic hydrolysis. Three types of pre-treatments for two reaction times were conducted to evaluate the characteristics of the pulp for subsequent saccharification. The pulp pretreated by alkali, and by acid followed by delignification, attained hydrolysis rates of over 90%. |
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Artigo Phenolic constituents and antioxidant activity of geopropolis from two species of amazonian stingless bees Silva, Ellen Cristina Costa da Muniz, Magno Perêa Nunomura, Rita de Cássia Saraiva Nunomura, Sergio Massayoshi Zilse, Gislene Almeida Carvalho Abstract in English: We investigated the phenolic constituents and antioxidant activity of geopropolis from two species of stingless Amazonian bees, Melipona interrupta and Melipona seminigra. The chemical investigation of geopropolis from Melipona interrupta led to the isolation of 5,7,4'-trihydroxyflavonone, 3,5,6,7,4'-pentahydroxyflavonol, naringenine-4'-O-b-D-glucopyranoside and myricetin-3-O-b-D-glucopyranoside. Their structures were assigned based on spectroscopic analyses, including two-dimensional NMR techniques. Antioxidant activity of methanol and ethanol extracts of M. interrupta and M. seminigra were measured using the 1,2-diphenyl-2-picryl-hydrazyl (DPPH) free radical scavenging assay. This is also the first work reporting the chemical investigation of stingless bee species from the Amazonian region. |
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Xylitol from rice husks by acid hydrolysis and Candida yeast fermentation
Rambo, Magale K. D.
Bevilaqua, Daiane B.
Brenner, Carla G. B.
Martins, Ayrton F.
Mario, Débora N.
Alves, Sydney H.
Mallmann, Carlos A.
Abstract in English: An investigation was conducted into the production of xylose by acid hydrolysis of rice husks and its subsequent bioconversion to xylitol. The parameters were optimised using the response surface methodology. The fermentation stage took place with the aid of the yeast species Candida guilliermondii and Candida tropicalis. An evaluation of the influence of several biomass pre-treatments was also performed. The effects of the acid concentration and hydrolysate pH on xylitol global yield were also assessed, and the highest yield of xylitol was 64.0% (w/w). The main products, xylose and xylitol, were identified and quantified by means of liquid chromatography. |
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Artigo The organic waste stabilization process: composting versus vermicomposting Dores-Silva, Paulo R. Landgraf, Maria Diva Rezende, Maria Olímpia de O. Abstract in English: Two processes are used to stabilize organic wastes: composting and vermicomposting.There are no studies in the literature showing which process is most effective over the short term. In this study, 3 organic wastes were composted and vermicomposted for 90 days, and the parameters pH, effective cation exchange capacity, total organic carbon, total Kjeldahl nitrogen, Ptotal, E4/E6 ratio, hydrophobicity and aromaticity indexes were determined. In all experiments, vermicomposted materials showed higher stability, proving a superior tool for stabilization of these organic wastes. |
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Artigo Study of immobilized lipase Lipozyme RM IM in esterification reactions for biodiesel synthesis Aguieiras, Erika C. G. Souza, Susana L. Langone, Marta A. P. Abstract in English: The aim of this work was to study monoalkyl ester synthesis catalyzed by immobilized lipase Lipozyme RM IM via the esterification reaction. Yields of over 90% were obtained with butanol in esterification reactions with oleic acid. In the reactions with deodorizer distillates of vegetable oils and butanol, the conversion obtained was greater than 80% after 2.5 h. For the esterification reaction of palm fatty acid deodorizer distillate (PFAD) and butanol, seven reuse cycles of Lipozyme RM IM were carried out and the final conversion was 42% lower than the initial conversion. |
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Artigo Adsorption of Reactive Blue 19 dye in aqueous solution by red mud chemically treated with hydrogen peroxide Souza, Kelli Cristina de Antunes, Maria Lúcia Pereira Conceição, Fabiano Tomazini da Abstract in English: Adsorption of Reactive Blue 19 dye onto activated red mud was investigated. Red mud was treated with hydrogen peroxide (LVQ) and heated at both 400 ºC (LVQ400) and 500 ºC (LVQ500). These samples were characterized by pH, specific surface area, point of zero charge and mineralogical composition. Adsorption was found to be significantly dependent on solution pH, with acidic conditions proving to be the most favorable. The adsorption followed pseudo-second-order kinetics. The Langmuir isotherm was the most appropriate to describe the phenomenon of dye removal using LVQ, LVQ400 and LVQ500, with maximum adsorption capacity of 384.62, 357.14 and 454.54 mg g-1, respectively. |
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Polyurethane adhesives from castor oil and modified starch
Valero, Manuel F.
Abstract in English: This study reports the preparation of polyurethane adhesives using polyols obtained from castor oil modified by a transesterification reaction with pentaerythritol and starch modified by glycosylation. The physical properties of the polyols such as hydroxyl value were determined and the infrared spectroscopic analysis of the polyols reported. The effect of varying the hydroxyl value in the polyols on physical properties of polyurethane coatings on wood and steel panels was determined. The characterization of polyurethane coatings carried out by IR spectroscopic analysis, scratch hardness resistance, impact resistance, lap shear strength, T-peel strength measurements, solvent resistance and chemical resistant determination were reported. |
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Artigo Fast determination of hydroquinone by batch injection analysis (BIA) with amperometric detection Cunha, Rafael Rodrigues Tormin, Thiago Faria Richter, Eduardo Mathias Munoz, Rodrigo Alejandro Abarza Abstract in English: A fast analytical method for determination of hydroquinone in pharmaceutical formulations employing batch injection analysis (BIA) with amperometric detection using a boron-doped diamond electrode is described. The supporting electrolyte was a 0.1 mol L-1 H2SO4 solution (the single reagent used for analysis). The method showed good repeatability (RSD of 0.45%, n=20), wide linear range (from 10 to 2000 µmol L-1, R=0.9999), low detection limit (0.016 µmol L-1) and satisfactory recovery values (91-96%). Accuracy of the method was evaluated by comparative analyses using high-performance liquid-chromatography. The ability to replace the electronic pipette by disposable syringes (injection procedure) in BIA systems was also shown. |
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Content, distribution and origin of hydrocarbons in sediments from three urban lagoons in Concepción - Chile
González Sepúlveda, Elizabeth
Loyola Sepúlveda, Rodrigo
Neira Hinojosa, José
Neira González, Felipe
Abstract in English: Aliphatic hydrocarbon content, distribution and origin in superficial and deep sediments of three interconnected urban lagoons located in Concepción-Chile were studied. In all lagoons, the analysis showed that aliphatic hydrocarbons present were of biogenic and anthropogenic origin, and n-alkanes were predominantly from odd carbon, confirmed by a relatively high Pristane/Phytane ratio. The most abundant Polycyclic Aromatic Hydrocarbons (PAHs) were two high-molecular weight species (Fluoranthene and Pyrene) whose presence may be related with the regular activities of the area as well as with combustion processes. |
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Artigo Flavonoids and terpenoids from Croton muscicarpa (Euphorbiaceae) Barreto, Milena B. Gomes, Clêrton L. Freitas, João Vito B. de Pinto, Francisco das Chagas L. Silveira, Edilberto R. Gramosa, Nilce V. Torres, Daniela S. Carneiro Abstract in English: A new sesquiterpene and twelve known compounds comprising eight flavonoids and four terpenoids, were isolated from the leaves, stems, roots and exudate of Croton muscicarpa Müll. Arg.. Their structures were identified as the terpenoids 6α-methoxy-cyperene, dammaradienol, squalene, acetyl aleuritolic acid and spathulenol, and as the flavonoids retusin, 3,7,4'-trimethoxy kaempferol, ombuine, pachipodol, kaempferol, casticin, 5-hydroxy-3,6,7,4'-tetramethoxyflavone and artemetin. All isolated compounds were characterized based on IR, MS, ¹H and 13C NMR, including 2D analyses (COSY, HSQC, HMBC, NOESY) and comparison with data from the literature. |
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Artigo Biodegradable composites based on cassava starch and waste from agro-industry Marengo, Vitor Almeida Vercelheze, Ana Elisa Stefani Mali, Suzana Abstract in English: The objectives of this work were to produce biodegradable composites using starch and different agro-industrial wastes (coconut fiber, soy bran and sugarcane bagasse) using a baking process, and to study the effects of these components on the resultant composite properties. The addition of different residues yielded trays with different properties. Samples manufactured with soy bran showed the highest density and water uptake at relative humidities ≥ 60%. The addition of sugarcane bagasse resulted in less dense and resistant samples whereas coconut fiber composites showed the highest breaking stress. The samples fabricated in this study represent an alternative packaging option for foods with low water content. |
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Preparative separation and purification of bufadienolides from ChanSu by high-speed counter-current chromatography combined with preparative HPLC
Li, Jialian
Zhang, Yongqing
Lin, Yunliang
Wang, Xiao
Fang, Lei
Geng, Yanling
Zhang, Qinde
Abstract in English: Eight bufadienolides were successfully isolated and purified from ChanSu by high-speed counter-current chromatography (HSCCC) combined with preparative HPLC (prep-HPLC). First, a stepwise elution mode of HSCCC with the solvent system composed of petroleum ether - ethyl acetate - methanol - water (4:6:4:6, 4:6:5:5, v/v) was employed and four bufadienolides, two partially purified fractions were obtained from 200 mg of crude extract. The partially purified fractions III and VI were then further separated by prep-HPLC, respectively, and another four bufadienolides were recovered. Their structures were confirmed by ESI-MS and ¹H-NMR spectra. |
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Artigo 3D-QSAR/CoMFA in imidic compounds with antinociceptive activity Walter, Maria Elena Almeida, Vera Lúcia Nunes, Ricardo José Abstract in English: Imide compounds have shown biological activity. These compounds can be easily synthesized with good yields. The objective of this paper was the rational planning of imides and sulfonamides with antinociceptive activity using the 3D-QSAR/CoMFA approach. The studies were performed using two data sets. The first set consisted of 39 cyclic imides while the second set consisted of 39 imides and 15 sulfonamides. The 3D- QSAR/CoMFA models have shown that the steric effect is important for the antinociceptive activity of imide and sulphonamide compounds. Ten new compounds with improved potential antinociceptive activity have been proposed by de novo design leapfrog simulations. |
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Revisão The state of the art in determination of veterinary drug residues in foods of animal origin using chromatographic techniques coupled to mass spectrometry Prestes, Osmar D. Martins, Manoel L. Friggi, Caroline do A. Munaretto, Juliana S. Adaime, Martha B. Zanella, Renato Abstract in English: The determination of veterinary drug residues in foods of animal origin is an important issue because of the risk these compounds pose to human health in addition to their persistence and tendency to bioaccumulate. In recent years, significant progress has been made in the area and this review presents the state of the art in sample preparation procedures associated with chromatographic techniques coupled to mass spectrometry for multiresidue determination of veterinary drugs in food of animal origin at concentration levels suitable for the control of residues and contaminants in food. |
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Processing of spent NiW/Al2O3 catalysts
Paulino, Jéssica Frontino
Afonso, Julio Carlos
Cunha, José Waldemar Silva Dias da
Abstract in English: Spent oxidized (500 ºC, 5 h) commercial NiW/Al2O3 catalysts were processed using two different routes: a) fusion with NaOH (650 ºC, 1 h), the roasted mass was leached in water; b) leaching with HCl or H2SO4 (70 ºC, 1-3 h). HCl was the best leachant. In both routes, soluble tungsten was extracted at pH 1 with Alamine 336 (10 vol.% in kerosene) and stripped with 2 mol L-1 NH4OH (25 ºC, one stage, aqueous/organic ratio = 1 v/v). Tungsten was isolated as ammonium paratungstate at very high yield (> 97.5%). The elements were better separated using the acidic route. |
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Nota técnica Spectrophotometric determination of chloride in cement after sample preparation by pyrohydrolysis Duarte, Fabio A. Pereira, Ederson R. Flores, Eder L. M. Muller, Edson I. Flores, Erico M. M. Dressler, Valderi L. Abstract in English: A method based on pyrohydrolysis was proposed for cement sample preparation and further chloride determination by spectrophotometry using flow injection analysis. Analytical parameters were evaluated and, under the selected conditions, the calibration curve was linear in the range of 0.2 to 10.0 µg mL-1 with r2 = 0.998. The limit of detection was5 µg g-1 of chloride and the relative standard deviation was less than 7%. The proposed pyrohydrolysis method is relatively simple and can be used for sample preparation for further spectrophotometric determination of low concentrations of chloride in cement. |
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Nota técnica Simultaneous determination of topiramate, carbamazepine, phenytoin and phenobarbital in plasma by gas chromatography with nitrogen phosphorus detector Hahn, Roberta Zilles Kreutz, Olyr Celestino Antunes, Marina Venzon Linden, Rafael Silva, Juliana da Silva, Cléber Álvares da Abstract in English: Topiramate and the other frequently co-administered antiepileptic drugs carbamazepine, phenytoin and phenobarbital were determined in 100 µL plasma samples by gas chromatography with nitrogen phosphorus detection (GC-NPD), after a one-step liquid-liquid extraction with ethyl acetate, followed by flash methylation with trimethylphenylammonium hydroxide. Total chromatographic run time was 12.5 min. Intra-assay and inter-assay precision was 2.5-7.3% and 1.6-5.2%, respectively. Accuracy was 100.1-104.2%. The limit of quantitation was 1 µg mL-1 for all analytes, proving suitable for routine application in therapeutic drug monitoring of antiepileptic drugs. |
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Improved method to obtain pfaffic acid as a marker for quality control
Rodrigues, Marili Villa Nova
Vedovello, Amanda
Rodrigues, Rodney Alexandre Ferreira
Montanari Junior, Ilio
Rehder, Vera Lucia Garcia
Abstract in English: Pfaffic acid, a marker of Hebanthe eriantha (Brazilian ginseng), was first isolated in 1983 but is not yet commercially available. This lack of availability compromises the quality control of this plant and its derivatives. This paper proposes a process for pfaffic acid isolation from roots of H. eriantha at a purity suitable for analytical purposes. The steps involved in this process included extraction, hydrolysis, fractionation and purification by preparative HPLC. This process led to isolation of pfaffic acid with a chromatographic purity of 98.5% in a 0.25% yield from dried roots of H. eriantha; this yield is more than forty times higher than that of the current method in the literature. |
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Educação Study of homogeneous chemical reactions using Monte Carlo simulation Farias, Ravir Rodrigues Cardoso, Luiz Augusto Martins Oliveira-Neto, Nemesio Matos Nascimento Junior, Baraquizio Braga Abstract in English: By using the Monte Carlo simulation platform with probabilistic mathematical functions of the Boltzmann type, <img src="/img/revistas/qn/v36n5/a20res.jpg" align="absmiddle"/>, having activation energy and temperature as parameters, it was possible to assess important dynamic aspects of homogeneous chemical reactions of the types A → B and A <img src="/img/revistas/qn/v36n5/20s01.jpg" align="absmiddle"/> B. The protocol proved a useful tool in work with the basic concepts of Kinetics and Thermodynamics allowing its application both in class activities and for assisting experimental procedures. |
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Educação Transesterification double step process for biodiesel preparation and its chromatographic characterization: oils and fats in practical organic chemistry Oliveira, Diogo Müller de Ongaratto, Diego Paulo Fontoura, Luiz Antonio Mazzini Naciuk, Fabrício Fredo Santos, Vinícius Oliveira Batista dos Kunz, Jéssica Danieli Marques, Marcelo Volpatto Souza, Alexander Ossanes de Pereira, Claudio Martin Pereira de Samios, Dimitrios Abstract in English: Methanolic transesterification of oils and fats was carried out in a two steps procedure, under basic and acidic catalysis. Palm, soybean, canola, corn, rice, grapeseed, sunflower, peanut, pequi and olive oils, besides tallow and lard were used as feedstock. Specific gravity, relative viscosity, thin layer chromatography and gas chromatography were used to characterize the biodiesel. Biodiesel was obtained in high yield and purity. Results were used to discuss the following key-concepts: 1 - triglycerides, composition and properties; 2 - nucleophilic acyl substitution under basic and acid conditions, 3 - thin layer chromatography, 4 - gas chromatography and its quantitative methods. |
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Assuntos gerais Importance of Gay-Lussac's law for classification of organic compounds Camel, Tânia de Oliveira Filgueiras, Carlos Alberto Lombardi Abstract in English: This article shows the genesis of the law of volumes of combining gases, formulated by Gay-Lussac in 1808, and how it allowed the expression of the composition of organic compounds in terms of whole numbers of volumes, thus leading to the first classification of organic compounds, formulated by Dumas and Boullay in 1828. It was from this work that Organic Chemistry began to shed its purely taxonomic nature, analogous to what prevailed in Natural History, and to then develop in a vigorous and continuous process, initiating what may be the most significant historical phenomenon in the History of Chemistry of the nineteenth century. |
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Assuntos gerais Patents at the national level as an indicator of development of technologies for hydrogen production Moreira, Renata Carvalho, Fátima Maria Sequeira de Bergamaschi, Vanderlei Sérgio Politano, Rodolfo Abstract in English: Brazil is considered a major player in relation to renewable energy sources. Since 2005, the MME have encouraged scientific and technological development to advance the hydrogen economy in the country. In this work we identified the patents based on hydrogen production filed by the INPI by evaluating the energy production in Brazil in conjunction with data held in the BNE and the prediction of hydrogen production made by the CGEE. It can be observed that the country needs substantial technological stimulation, but shows promise for producing renewable energy sources. |
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