Scielo RSS <![CDATA[Química Nova]]> http://www.scielo.br/rss.php?pid=0100-404220140006&lang=en vol. 37 num. 6 lang. en <![CDATA[SciELO Logo]]> http://www.scielo.br/img/en/fbpelogp.gif http://www.scielo.br <![CDATA[<b>37ª Reunião anual da Sociedade Brasileira de Química</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600001&lng=en&nrm=iso&tlng=en <![CDATA[<b>Nanocomposite of papaya puree and chitosan nanoparticles for application in packaging</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600002&lng=en&nrm=iso&tlng=en Nanocomposite materials have been incorporated into biopolymers, (e.g. hydroxypropyl methylcellulose), to improve their physical and chemical properties and enable them to be applied in food packaging, especially for their biodegradable and renewable properties. With this addition, fruit puree has been incorporated into the films to confer nutritional properties besides color and flavor. Chitosan is of interest in the packaging field since it is a biodegradable, bioabsorbable, antimicrobial agent. Furthermore, chitosan nanoparticles have been widely explored for their interesting properties and potential applications in food packaging. This work was divided into two stages: (1) chitosan nanoparticle synthesis; (2) addition of nanoparticles into HPMC and papaya puree films. Addition of chitosan nanoparticles to HPMC and papaya puree films improved film properties: mechanical, thermal and water vapor barrier. We have developed a novel nanomaterial with great potential for application in packaging to prolong the shelf life of food. <![CDATA[<b>Starch/poly (butylene adipate-co-terephthalate)/montmorillonite films produced by blow extrusion</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600003&lng=en&nrm=iso&tlng=en This study aims to prepare biodegradable films from cassava starch, poly (butylene adipate-co-terephthalate) (PBAT), and montmorillonite (MMT) using blow-extrusion process and analyze the effects of different types and concentrations of MMT on the microstructure, physicochemical, and mechanical properties of the resulting films. The films were produced by blending 30% of PBAT with glycerol (17.5%), starch (49.0-52.5%), and four different types of montmorillonite (Cloisite® Na+, 10A, 15A, and 30B) at two different concentrations (1.75% and 3.5%). All the films prepared in this study showed an increase in the basal spacing of MMT layers. In particular, the films with 10A and 30B showed the highest increase in intercalation basal spacing, suggesting the formation of intercalated composites. The addition of nanoclays decreased the elongation of films. The addition of Cloisite® 10A resulted in films with the lowest WVP values and the highest stability to water adsorption under different RH conditions. <![CDATA[<b>Influence of sediment humic substances on the bioavailability of metals in the aquatic system</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600004&lng=en&nrm=iso&tlng=en In rivers, sediments act as sinks for retaining contaminants. This study evaluated the influence of sediment humic substances (HS) on the bioavailability of metals. The levels of metals in sediments and HS indicated that most are complexed with HS. Characterization of HS showed a high degree of humification. The complexation capacity of HS for metals established the affinity order:Pb2+<Cd2+<Co2+<Ni2+<Cu2+<Zn2+<Mn2+<Fe2+. Chemometric analysis demonstrated a correlation between the structural characteristics of HS and complexation capacity of metals. <![CDATA[<b>Adsorption of alpha-lactalbumin from milk whey on hydroxyapatite</b>: <b>effect of pH and temperature and thermodynamic analysis</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600005&lng=en&nrm=iso&tlng=en The nutritional and functional benefits offered by whey protein α-lactalbumin justify the great interest in its manufacture in large quantities at a high purity level. Hydroxyapatite is a calcium phosphate material able to adsorb proteins and can be synthesized at low production cost. Therefore, this work evaluated the adsorption of α-lactalbumin on hydroxyapatite using solid-liquid phase equilibrium data reported as adsorption isotherms. Van't Hoff's thermodynamics analysis showed that the adsorption process is entropically driven. <![CDATA[<b>Cadmium-contaminated soil</b>: <b>metal extractability and chemical kinetics of filter cake organic matter degradation</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600006&lng=en&nrm=iso&tlng=en The chemical kinetics of sugarcane filter cake (FC) organic matter degradation at rates (0, 40, 80, and 120 t ha-1) in non-contaminated and different degrees of cadmium-contaminated Oxisol (0.19, 28, 56, 112 and 200 mg Cd kg-1) and DTPA-extractable Cd was studied. FC degradation was determined by quantifying CO2 emitted from soil samples during 72 days of incubation. DTPA-extractable Cd was performed after the incubation period. FC degradation was described by a two-stage equation of chemical kinetics. FC degradation rates were between 15 and 33%. Total CO2 emitted from FC declined with increasing degree in Cd-contamination and the DTPA-extractable Cd declined with FC rates. <![CDATA[<b>Bromine and iodine determination in edible seaweed by ICP-MS after digestion by microwave-induced combustion</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600007&lng=en&nrm=iso&tlng=en A method based on microwave-induced combustion (MIC) was applied for the decomposition of different types of edible seaweed (Nori, Hijiki and Wakame) for subsequent determination of bromine and iodine by inductively coupled plasma mass spectrometry (ICP-MS). Decomposition of 500 mg of each sample was achieved in less than 30 min. A single and diluted solution (150 mmol L-1 (NH4)2CO3) was used for the absorption of both analytes and a reflux step of 5 min was applied to improve analyte recoveries. Accuracy was evaluated using certified reference materials and agreement was between 103 and 108% for both elements. <![CDATA[<b>Immobilization of lipase by encapsulation in silica aerogel</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600008&lng=en&nrm=iso&tlng=en Lipase from Burkholderia cepacia was immobilized in a silica matrix and dried in high pressure carbon dioxide media (aerogel). The protic ionic liquid (PIL) was used in the immobilization process by encapsulation. The objective of this work was to evaluate the influence of the drying technique using supercritical carbon dioxide in biocatalysts obtained through the sol-gel technique by evaluating temperature and pressure and, after selecting the best drying conditions, to investigate the application of the technique for the biocatalyst using ionic liquid as an additive in the immobilization process. The results for immobilized biocatalysts showed that the best conditions of pressure and temperature were 100 bar and 25 ºC, respectively, giving a total activity recovery yield of 37.27% without PIL (EN) and 44.23% with PIL (ENLI). The operational stability of the biocatalysts showed a half-life of 11.4 h for ENLI and 6 h for EN. Therefore, solvent extraction using supercritical CO2, besides shortening drying time, offers little resistance to the immobilization of lipases, since their macropores provide ample room for their molecules. The use of the ionic liquid as an additive in the process studied for the immobilization of enzymes produced attractive yields for immobilization and therefore has potential for industrial applications in the hydrolysis of vegetable oils. <![CDATA[<b>Volatile constituents of <i>Aristolochia trilobata</i> L. (<i>Aristolochiaceae</i>)</b>: <b>a rich source of sulcatyl acetate</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600009&lng=en&nrm=iso&tlng=en Analysis of the volatile fraction of Aristolochia trilobata stem led to the identification of 6-methyl-5-hepten-2-yl acetate (23.31 ± 0.28%), limonene (15.43 ± 0.030%), linalool (8.70 ± 0.29%), p-cymene (7.81 ± 0.12%), bicyclogermacrene (4.21 ± 0.11%), and spathulenol (4.17 ± 0.14%) as the major constituents of the essential oil. Linalool (29.51 ± 0.49%), 6-methyl-5-hepten-2-ol (19.54 ± 0.82%), 6-methyl-5-hepten-2-yl acetate (8.92 ± 0.16%), and a-terpineol (4.62 ± 0.05%) were identified as major constituents of the hydrolate. The compound 6-methyl-5-hepten-2-yl acetate was isolated for the first time from this plant and was identified as the major component of the volatile fraction. <![CDATA[<b>Development of prepolymer technology in the synthesis of a polyurethane binder used in solid rocket fuels</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600010&lng=en&nrm=iso&tlng=en The aim of this work was to synthesize a polyurethane polymer matrix using polyols as a raw material to obtain a binder such as the hydroxyl terminated polybutadiene (HTPB) pre-polymer in energetic material formulation. The soybean-based polyol was the best starting raw material for producing a binder for solid fuel formulation in rocket motor applications. Characterization of the obtained soybean-based polyurethane binder was carried out by employing FT-IR analysis and thermo analytical techniques that showed similar HTPB binder thermo decomposition behaviors, confirming their potential for use as polymer matrix composites. <![CDATA[<b>Synthesis, characterization, and biological activity of a new class of dialkylphosphorylhydrazone derivatives of isatin</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600011&lng=en&nrm=iso&tlng=en Sixteen dialkylphosphorylhydrazones were synthesized by condensation of phosphorylhydrazines with substituted isatins. Products were characterized by FTIR, ¹H-NMR, 13C-NMR, and 31P-NMR. Fungicidal activities of these compounds against Rhizoctonia solani and Fusarium oxysporum were also evaluated. Some compounds inhibited the growth of Rhizoctonia solani and Fusarium oxysporum by 43% and 51%, respectively. These compounds exhibited no effects on germination of lettuce seeds (Lactuca sativa L). <![CDATA[<b>Development of a method for determination of tioconazole associated with polymeric nanocapsules by liquid chromatography</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600012&lng=en&nrm=iso&tlng=en The aim of this work was to develop and validate an analytical method for the quantification of tioconazole in polymeric nanocapsule suspensions by high performance liquid chromatography with UV detection. The analysis was performed with a mobile phase composed of methanol:water (80:20) and 0.18% ammonium hydroxide; RP-18 column and UV detection at 219 nm. The method proved to be linear in the concentration range of 5-50 µg mL-1 (r = 0.9999), specific, precise (repeatability RSD = 1.42%, intermediate precision RSD = 1.17%), accurate (98 - 102%) and robust (RSD < 2.0%). In conclusion, a simple and rapid method was validated proving suitable for quantification of tioconazole in polymeric nanocapsules. <![CDATA[<b>Simple method for mass production of polypyrrole/carbon nanotubes hybrid artificial muscle</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600013&lng=en&nrm=iso&tlng=en Large scale preparation of hybrid electrical actuators represents an important step for the production of low cost devices. Interfacial polymerization of polypyrrole in the presence of multi-walled carbon nanotubes represents a simple technique in which strong interaction between components is established, providing composite materials with potential applications as actuators due to the synergistic interaction between the individual components, i.e., fast response of carbon nanotubes, high strain of polypyrrole, and diversity in the available geometry of resulting samples. <![CDATA[<b>Synthesis and evaluation of octocrylene-inspired compounds for UV-filter activity</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600014&lng=en&nrm=iso&tlng=en Octocrylene (2-ethylhexyl 2-cyano-3,3-diphenyl-2-propenoate) is present in several sunscreens and is known to work synergistically with UV filters. We prepared eight octocrylene-related compounds to test their photoprotective activities by measuring diffuse transmittance. The compounds had varied photoprotection profiles, with Sun Protection Factors (SPF) ranging from 1 to 5 and UVA Protection Factors (UVAPF) ranging from 1 to 8. Compounds 4, 5, and 7 showed the best protection against UVB sunrays, while compounds 5, 6, and 7 presented the best results for protection from UVA, so compound 7 had the most balanced protection overall. Results for compounds 4, 8, and 9 are reported for the first time in the literature. <![CDATA[<b>Terpenoids and coumarins from <i>Jatropha ribifolia</i> (Pohl) Baill</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600015&lng=en&nrm=iso&tlng=en Eight compounds, including terpenoids (jatrophone, hydroxyjatrophone, 6-hydroxycyperene, cabraleadiol monoacetyl, and cabraleadiol) and coumarins (fraxetin, fraxidin, and isofraxidin), were isolated from Jatropha ribifolia (Euphorbiaceae). Their structures were established by 1D and 2D NMR (COSY, HSQC, and HMBC) spectra, HRESIMS and comparison with published data. <![CDATA[<b><i>In vitro</i></b><b> radical-scavenging activity, toxicity against <i>A. salina</i>, and nmr profiles of extracts of lichens collected from Brazil and Antarctica</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600016&lng=en&nrm=iso&tlng=en Extracts of six lichen species collected from Brazil and Antarctica were investigated for their potential toxicity and radical-scavenging properties. The composition of the extracts was investigated using TLC and NMR, leading to identification of atranorin (1), along with salazinic (2), barbatic (3), α-alectoronic (4), α-collatolic (5), cryptochlorophaeic (6), caperatic (7), lobaric (8), and protolichesterinic (9) acids. All acetone extracts were evaluated for their 2,2'-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging ability and subjected to Artemia salina bioassay. The free-radical-scavenging activities of each extract (100 µg) ranged from 8.9 ± 0.1% to 38.7 ± 2.5% and the EC50 values ranged from 0.24 ± 2.10 to 3.54 ± 0.28 mg mL-1, while the toxicity of the extracts against A. salina were low (151.0 to >600 µg mL-1). <![CDATA[<b>Chemo-enzymatic epoxidation of</b> <b>β</b><b>-caryophyllene using lipases immobilized in agar gel</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600017&lng=en&nrm=iso&tlng=en The immobilization of enzymes and microorganisms on solid supports has been developed in recent years. These biocatalysts may be used in organic media allowing their storage and reuse, thus reducing costs of the process. Herein, lipases from various sources were immobilized in agar gel and used as catalysts in the chemo-enzymatic epoxidation of β-caryophyllene. Several experimental parameters, such as the use of different organic solvents including ionic liquids, time, temperature, and agitation rate were evaluated. The mono-epoxide was obtained as a single product. The best result was achieved using immobilized F-AP15 lipase, forming the corresponding β-caryophyllene epoxide at a conversion of 96% in an 8h reaction at 35 ºC. <![CDATA[<b>Monitoring enzymatic activities with fluorogenic probes</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600018&lng=en&nrm=iso&tlng=en Latent fluorogenic probes are essential tools for molecular and chemical biology, providing valuable information about enzymatic activity and occurrence. In this review, a brief outline of fluorophores and latent fluorogenic probes is given. Furthermore, advances and challenges in the development of fluorogenic chemical probes to visualize enzymatic activities (hydrolases and oxidoreductases) of biotechnological and biomedical interest are highlighted, including some methodologies for intracellular imaging. <![CDATA[<b>The chemistry and toxicity of hair dyes</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600019&lng=en&nrm=iso&tlng=en The market for hair dye involves a growing range of products, which requires greater understanding of hair properties, mechanisms of action and color development. In this work, we present a critical analysis of the classification, physical and chemical characteristics, chemical analysis and toxicological/mutagenic potential of dyes used in the hair dyeing process. A compilation of some studies was carried out, focusing on the available knowledge about these dyes and their effects on the environment and human health. <![CDATA[<b>Super/subcritical fluid chromatography with packed columns</b>: <b>state of the art and applications</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600020&lng=en&nrm=iso&tlng=en Separations using supercritical fluid chromatography (SFC) with packed columns have been re-discovered and explored in recent years. SFC enables fast and efficient separations and, in some cases, gives better results than high performance liquid chromatography (HPLC). This paper provides an overview of recent advances in SFC separations using packed columns for both achiral and chiral separations. The most important types of stationary phases used in SFC are discussed as well as the most critical parameters involved in the separations and some recent applications. <![CDATA[<b>Inertization of small-scale chemical wastes using iron phosphate glass</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600021&lng=en&nrm=iso&tlng=en The viability of small-scale heavy-metal waste immobilization into iron phosphate glasses was investigated. Several waste forms containing different amounts of heavy-ion wastes were evaluated (5%, 10%, 15%, 20%, 26%, 33%, 40% and 50% by mass) and their X-ray diffraction patterns revealed that no crystallization occurred in glasses with waste concentrations up to 26%. The dissolution rates for all of the reported glass compositions (ca. 10-8 g cm-2 min-1) are similar to those reported for the materials most commonly used for waste vitrification. Iron phosphate glasses thus proved to be very useful for the immobilization of heavy-metal wastes, exhibiting good contention and chemical durability comparable to that of borosilicate glasses. <![CDATA[<b>Method for determining the photocatalytic potential of portland cement mortar containing TiO<sub>2</sub> for decomposing the pollutant nitrogen monoxide</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600022&lng=en&nrm=iso&tlng=en Photocatalytic materials can minimize atmospheric pollution by decomposing certain organic and inorganic pollutants using sunlight as an energy source. In this paper, the development of a methodology to measure the photocatalytic potential of mortar containing TiO2 nanoparticles is reported. The results indicate that up to 40% of NOx can be degraded by Portland cement mortar containing 30-50% of TiO2, which validates the method developed for evaluating the photocatalytic potential of materials. <![CDATA[<b>Simultaneous determination of carbamazepine, phenytoin and phenobarbital in dried blood spots by high performance liquid chromatography</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600023&lng=en&nrm=iso&tlng=en Carbamazepine, phenobarbital and phenytoin were determined in dried blood spots (DBS) by high performance liquid chromatography, after extraction of 8 mm DBS using a mixture of acetonitrile and methanol. Analytes were separated by reversed-phase chromatography, with a run time of 17 minutes. Intra-assay and inter-assay precisions were in the 5.3 to 8.4% and 3.3 to 5.2% ranges, respectively. Accuracy was in the 98.8 to 104.3% range. The method had sensitivity to detect all analytes at levels below minimum therapeutic concentrations. The analytes were stable at 4 ºC and room temperature for up to 12 days and at 45 ºC for 9 days. The method was applied to 14 paired clinical samples of blood serum and DBS. <![CDATA[<b>Guidelines for training teachers of basic education with chemistry teacher education interfaces</b>: <b>education possiblities in context</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600024&lng=en&nrm=iso&tlng=en We developed and applied an educational instrument (ID) to discuss, in the discipline of Supervised Pre Service Teachers Practice 1, guidelines for teacher education to redefine teacher knowledge with a specific focus on chemistry teachers. The study used methodological fundamentals of Discursive Textual Analysis that involves identifying and isolating a set of materials subjected to analysis, categorizing these statements and producing texts, integrating these descriptions and interpretations, basing its construction on the category system built. Data were collected through participant observation and text readings used by the students in performing the activity. It was noted that the chemistry teachers trained were able to express opinions that indicated the Construction of Meanings Interface that was the category of analysis established a priori. <![CDATA[<b>Construction of a graphite electrode removed from common batteries</b>: <b>didactic applications</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600025&lng=en&nrm=iso&tlng=en This paper presents a proposal for using recycled graphite electrodes obtained from exhausted commercial 1.5 V batteries and its application in electroanalysis. The electrode could be prepared by the students and applied in the simple didactic experiments suggested, such as determination of active electrode area, cyclic voltammetry and useful potential range (also called "potential window"), demonstration and effect of scan rate on cyclic voltammograms. The possibility of using the graphite electrode in quantitative analysis was also demonstrated using the ferricyanide/ferrocyanide reversible redox couple ([Fe(CN)6]3-/[Fe(CN)6]4-) as an electrochemical probe by the dependence of peak current with the analyte concentration and flow injection analysis with amperometric detection. <![CDATA[<b>Assessment of the "micro-greenness" of syntheses using the green star</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600026&lng=en&nrm=iso&tlng=en This article reports a study to increase the overall greenness of chemical syntheses for first-year university laboratories. The separate evaluation of the micro-greenness of the three stages of synthesis (reaction, isolation and purification) using the Green Star (GS) was implemented and their respective contribution to overall greenness was investigated for two examples: syntheses of cobalt (III) tris(acetylacetonate) and potassium nitrilosulfonate. Results showed that the post-reaction (work-up) steps are the most problematic for overall greenness. Greenness optimization can be achieved by combining the greenest procedures for each step obtained from different protocols available in the literature. <![CDATA[<b>Battery of metrics for evaluating the material greenness of synthesis reactions</b>]]> http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0100-40422014000600027&lng=en&nrm=iso&tlng=en The use of a battery of three mass metrics (atomic economy - AE, reaction mass efficiency - RME, and mass intensity - MI) for systemic evaluation of the material greenness of synthesis reactions is presented. Material greenness is discussed in terms of materialization/dematerialization of the reaction system and also according to the first two Principles of Green Chemistry, and is shown to involve two components: atomic greenness (incorporation of the atoms provided by reagents into the product, evaluated by AE and RME); and massic greenness (global mass of reagents and non-stoichiometric materials, evaluated by MI, related to the production of residues).