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Incorporation of dithiooxamide as a complexing agent into cellulose for the removal and pre-concentration of Cu(II) and Cd(II) ions from natural water samples

The present study describes the incorporation of a complexing agent, dithiooxamide, into microcrystalline cellulose for use in the pre-concentration of Cu(II) and Cd(II) ions from aqueous samples. The FTIR spectrum of the adsorbent exhibited an absorption band in the region of 800 cm-1, which confirmed the binding of the silylating agent to the matrix. Elemental analysis indicated the amount of 0.150 mmol g-1 of the complexing agent. The adsorption data were fit to the modified Langmuir equation, and the maximum amount of metal species extracted from the solution, Ns, was determined to be 0.058 and 0.072 mmol g-1 for Cu(II) and Cd(II), respectively. The covering fraction φ, which was 0.39 and 0.48 for Cu(II) and Cd(II), respectively, was used to estimate a 1:2 (metal:ligand) ratio in the formed complex, and a binding model was proposed based on this information. The adsorbent was applied in the pre-concentration of natural water samples and exhibited an enrichment factor of approximately 50-fold for the species studied, which enabled its use in the analysis of trace metals in aqueous samples. The system was validated by the analysis of certified standard (1643e), and the adsorbent was stable for more than 20 cycles, thus enabling its safe reutilization. © 2012 Elsevier B.V. All rights reserved.

Study of adsorption and preconcentration by using a new silica organomodified with [3-(2,2′-dipyridylamine)propyl] groups

In this work, a silica surface chemically modified with [3-(2,2′-dipyridylamine)propyl] groups, named [3-(2,2′- dipyridylamine)propyl]silica (Si-Pr-DPA) was prepared, characterized, and evaluated for its heavy metal adsorption characteristics from aqueous solution. To our knowledge, we are the first authors who have reported the present modification. The material was characterized using infrared spectroscopy, SEM, and NMR 29Si and 13C solid state. Batch and column experiments were conducted to investigate for heavy metal removal from dilute aqueous solution by sorption onto Si-Pr-DPA. From a number of studies the affinity of various metal ions for the Si-Pr-DPA sorbent was determined to follow the order Fe(III) > Cr(III) >> Cu(II) > Cd(II) > Pb(II) > Ni(II). Two standard reference materials were used for checking the accuracy and precision of the method. The proposed method was successfully applied to the analysis of environmental samples. This ligand material has great advantage for adsorption of transition-metal ions from aqueous medium due to its high degree of organofunctionalization associated with the large adsorption capacity, reutilization possibility, and rapidity in reaching the equilibrium. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Sequential Determination of Cd, Cu and Pb in Tea Leaves by Slurry Introduction to Thermospray Flame Furnace Atomic Absorption Spectrometry

A simple procedure for the sequential determination of Cd, Cu and Pb in tea leaves by slurry introduction to thermospray flame furnace atomic absorption spectrometry was developed. Detection limits were 0.05 mg kg-1 for Cd, 2.1 mg kg-1 for Cu and 0.68 mg kg-1 for Pb using 0.67 % (m/v) slurries (100 mg/15 mL). © 2013 Springer Science+Business Media New York.

Experimental NMR and MS study of benzoylguanidines. Investigation of E/Z isomerism

Molecules containing the guanidinic nuclei possess several pharmacological applications, and knowing the preferred isomers of a potential drug is important to understand the way it operates pharmacologically. Benzoylguanidines were synthesized in satisfactory to good yields and characterized by NMR, Electrospray Ionization Mass Spectrometry (ESI-MS) and Fourrier Transform InfraRed Spectroscopy techniques (FTIR). E/Z isomerism of the guanidines was studied and confirmed by NMR analysis in solution (1H-13C Heteronuclear Single Quantum Coherence (HSQC) and Heteronuclear Multiple-Bond Correlation (HMBC), 1H-15N HMBC, 1H- 1H Correlation Spectroscopy (COSY) and Nuclear Overhauser Effect Spectroscopy (NOESY) experiments) at low temperatures. Compounds with p-Cl and p-Br aniline moiety exist mainly as Z isomer with a small proportion of E isomer, whereas compounds with p-NO2 moiety showed a decrease in proportion of isomer Z. The results are important for the application of these molecules as enzymatic inhibitors. Copyright © 2013 John Wiley & Sons, Ltd.

Synthesis and characterization of 3-[(thiourea)-propyl]-functionalized silica gel and its application in adsorption and catalysis

The objective of this research was the preparation of a silica gel functionalized successively with 3-chloropropyltrimethoxysilane (SG-PrCl) and thiourea (SG-Pr-THIO), and its application in adsorption and catalysis. The materials were characterized by 13C and 29Si NMR, FTIR, scanning electron micrographs (SEM), analysis of nitrogen and elemental analysis. Aiming at its application in adsorption, the [3-(thiourea)-propyl] silica gel (SG-Pr-THIO) was tested as an adsorbent for transition-metal ions using a batchwise process. The organofunctionalized surface showed the ability to adsorb the metal ions Cd(ii), Cu(ii), Ni(ii), Pb(ii) and Co(ii) from water, ethanol and acetone. The adsorption isotherms were fitted by Langmuir, Freundlich, Temkin and Dubinin-Radushkevich (D-R) models. The kinetics of adsorption of metals were performed using three models such as pseudo-first order, pseudo-second order and Elovich. The Langmuir and pseudo-first order models were the most appropriate to describe the adsorption and kinetic data, respectively. With the purpose of application in catalysis, the SG-Pr-THIO was reacted with a Mo(ii) organometallic complex, forming the new material SG-Pr-THIO-Mo. Only a few works in the literature have reported this type of reaction, and none dealt with thiourea and Mo(ii) complexes. The new Mo-silica gel organometallic material was tested as catalyst in the epoxidation of cyclooctene and styrene. © 2013 The Royal Society of Chemistry and the Centre National de la Recherche Scientifique.

Characterization of flavonoids and phenolic acids in Myrcia bella cambess. Using FIA-ESI-IT-MSn and HPLC-PAD-ESI-IT-MS combined with NMR

The leaves of Myrcia DC. ex Guill species are used in traditional medicine and are also exploited commercially as herbal drugs for the treatment of diabetes mellitus. The present work aimed to assess the qualitative and quantitative profiles of M. bella hydroalcoholic extract, due to these uses, since the existing legislation in Brazil determines that a standard method must be developed in order to be used for quality control of raw plant materials. The current study identified eleven known flavonoid-O-glycosides and six acylated flavonoid derivatives of myricetin and quercetin, together with two kaempferol glycosides and phenolic acids such as caffeic acid, ethil galate, gallic acid and quinic acid. In total, 24 constituents were characterized, by means of extensive preparative chromatographic analyses, along with MS and NMR techniques. An HPLC-PAD-ESI-ITMS and FIA-ESI-IT-MSn method were developed for rapid identification of acylated flavonoids, flavonoid-O- glycosides derivatives of myricetin and quercetin and phenolic acids in the hydroalcoholic M. bella leaves extract. The FIA-ESI-IT-MS techinique is a powerful tool for direct and rapid identification of the constituents after isolation and NMR characterization. Thus, it could be used as an initial method for identification of authentic samples concerning quality control of Myrcia spp extracts. © 2013 by the authors.

Anthropogenic influences on Cd, Cr,Cu, Ni, Pb and Zn concentrations in soils and sediments in a watershed with sugar cane crops at São Paulo State, Brazil

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Avaliação do perfil de expressão gênica de células CD34+ e células CD CD133+ isoladas de medula óssea e de sangue de cordão umbilical

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Estruturação do Eumenine Mastroparano por dinâmica molecular em misturas de TFE-água

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Estudo estrutural por RMN do peptídeo policatiônico polybine I de veneno da vespa social Polybia paulista

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Contribuição eletrostática e não eletrostática na interação de peptídeos líticos com membranas modelo

Pós-graduação em Biofísica Molecular - IBILCE