Espectrometria de massas com ionização por "electrospray": processos químicos envolvidos na formação de íons de substâncias orgânicas de baixo peso molecular

An overview of the current literature on the chemical processes involved in the ion formation from low molecular weight organic compounds by electrospray ionization mass spectrometry is given.

Distribution Patterns of Soil Properties in a Rural Mediterranean Area in Northeastern Spain

Soil properties on the Cap de Creus Peninsula, NE Spain depend primarily on scarce agricultural practices and early abandonment. In the study area, 90% of which is mainly covered by Cistus shrubs, 8 environments representing variations in land use/land cover and soil properties at different depths were identified. In each environment variously vegetated areas were selected and sampled. The soils, collected at different depths, were classified as Lithic Xerorthents according to the United States Department of Agriculture system of soil classification (USDA-NRCS 1975). Differences in soil properties were largely found according to the evolution of the plant canopy and the land use history. To identify underlying patterns in soil properties related to environmental evolution, factor analysis was performed and factor scores were used to determine how the factor patterns varied between soil variables, soil depths and selected environments. The three-factor model always accounted for 80% of the total variation in the data at the different soil depths. Organic matter was the more relevant soil property at 0–2 cm depth, whereas active minerals (silt and clay) were found to be the most relevant soil parameters controlling soil dynamics at the other depths investigated. Results showed that vineyards and olive tree soils are poorly developed and present worse conditions for mineral and organic compounds. Analysis of factor scores allowed independent assessment of soils, depth and plant cover and demonstrated that soils present the best physico-chemical characteristics under Erica arborea and meadows. In contrast, soils under Cistus monspeliensis were less nutrient rich and less well structured

O pKa de indicadores ácido-base e os efeitos coloidais

An experiment is proposed that can be included in undergraduate courses of chemistry. The subject is the acidity of organic compounds, which are employed as pH indicators, particularly in acid-base titrations. The indicators used are methyl orange, bromophenol blue and bromocresol green in aqueous medium. The influence of colloidal systems on the equilibrium is evaluated by the pKa. The colloids employed are surfactants like sodium dodecyl sulfate, cetyl-trimethylammonium bromide and a polymeric non-ionic F127 (pluronics). The effect of stabilization promoted by the system on the acidic or basic structureof the indicator establishes the action mechanism of the colloid on the pKa values.

Métodos emergentes para aumentar a eficiência do ozônio no tratamento de águas contaminadas

Many industrial processes produce effluents with a wide variety of xenobiotic organic pollutants, which cannot be efficiently degraded by conventional biological treatments. Thus, the development of new technologies to eliminate these refractory compounds in water has become very imperative in order to assure the quality of this important resource. Ozonation is a very promising process for the treatment of wastewaters containing non-easily removable organic compounds. The present work aims at highlighting new methods of enhancing the efficiency of ozone towards the removal organic pollutants in aqueous solution. Special attention is given to catalytic ozonation processes contemplating homo- and heterogeneous catalysis, their activity and mechanisms. Recent results and future prospects about the application of these processes to real effluents are also evaluated.

Esquema geral para elucidação de substâncias orgânicas usando métodos espectroscópico e espectrométrico

This work describes a systematic method to be applied in undergraduate courses of organic chemistry, correlating infrared spectra, hydrogen and carbon-13 nuclear magnetic resonance, and mass spectra. To this end, a scheme and a table were developed to conduct the elucidation of the structure of organic compounds initially using infrared spectra. Interpretation of hydrogen and carbon-13 nuclear magnetic resonance spectra and of mass spectra is used to confirm the proposed structure.

Synthesis and multi-target biological profiling of a novel family of rhein derivatives as disease-modifying anti-Alzheimer agents

We have synthesized a family of rhein-huprine hybrids to hit several key targets for Alzheimer"s disease. Biological screening performed in vitro and in Escherichia coli cells has shown that these hybrids exhibit potent inhibitory activities against human acetylcholinesterase butyrylcholinesterase, and BACE-1, dual Aβ42 and tau anti-aggregating activity, and brain permeability. Ex vivo studies with the leads (+)- and (-)-7e in brain slices of C57bl6 mice have revealed that they efficiently protect against the Aβ-induced synaptic dysfunction , preventing the loss of synaptic proteins and/or have a positive effect on the induction of long term potentiation. In vivo studies in APP-PS1 transgenic mice treated i.p. for 4 weeks with (+)- and (-)-7e have shown a central soluble Aβ lowering effect, accompanied by an increase in the levels of mature amyloid precursor protein (APP). Thus, (+)- and (-)-7e emerge as very promising disease-modifying anti-Alzheimer drug candidates.

Synthesis and multi-target biological profiling of a novel family of rhein derivatives as disease-modifying anti-Alzheimer agents

We have synthesized a family of rhein-huprine hybrids to hit several key targets for Alzheimer"s disease. Biological screening performed in vitro and in Escherichia coli cells has shown that these hybrids exhibit potent inhibitory activities against human acetylcholinesterase butyrylcholinesterase, and BACE-1, dual Aβ42 and tau anti-aggregating activity, and brain permeability. Ex vivo studies with the leads (+)- and (-)-7e in brain slices of C57bl6 mice have revealed that they efficiently protect against the Aβ-induced synaptic dysfunction , preventing the loss of synaptic proteins and/or have a positive effect on the induction of long term potentiation. In vivo studies in APP-PS1 transgenic mice treated i.p. for 4 weeks with (+)- and (-)-7e have shown a central soluble Aβ lowering effect, accompanied by an increase in the levels of mature amyloid precursor protein (APP). Thus, (+)- and (-)-7e emerge as very promising disease-modifying anti-Alzheimer drug candidates.

Synthesis and multi-target biological profiling of a novel family of rhein derivatives as disease-modifying anti-Alzheimer agents

We have synthesized a family of rhein-huprine hybrids to hit several key targets for Alzheimer"s disease. Biological screening performed in vitro and in Escherichia coli cells has shown that these hybrids exhibit potent inhibitory activities against human acetylcholinesterase butyrylcholinesterase, and BACE-1, dual Aβ42 and tau anti-aggregating activity, and brain permeability. Ex vivo studies with the leads (+)- and (-)-7e in brain slices of C57bl6 mice have revealed that they efficiently protect against the Aβ-induced synaptic dysfunction , preventing the loss of synaptic proteins and/or have a positive effect on the induction of long term potentiation. In vivo studies in APP-PS1 transgenic mice treated i.p. for 4 weeks with (+)- and (-)-7e have shown a central soluble Aβ lowering effect, accompanied by an increase in the levels of mature amyloid precursor protein (APP). Thus, (+)- and (-)-7e emerge as very promising disease-modifying anti-Alzheimer drug candidates.

Elucidação estrutural de substâncias orgânicas com auxílio de computador: evoluções recentes

The development of new tools for chemoinformatics, allied to the use of different algorithms and computer programmes for structure elucidation of organic compounds, is growing fast worldwide. Massive efforts in research and development are currently being pursued both by academia and the so-called chemistry software development companies. The demystification of this environment provoked by the availability of software packages and a vast array of publications exert a positive impact on chemistry. In this work, an overview concerning the more classical approaches as well as new strategies on computer-based tools for structure elucidation of organic compounds is presented. Historical background is also taken into account since these techniques began to develop around four decades ago. Attention will be paid to companies which develop, distribute or commercialize software as well as web-based and open access tools which are currently available to chemists.

Degradação do pesticida Padron® por processos fotoquímicos utilizando luz artificial e solar

Destruction of Padron® (dye and picloram) was evaluated using a photoreactor and a solar reactor. Photolysis was observed using only a germicide lamp (GL). Black light (BL) and H2O2 (172 mmol L-1) promoted a conversion of 49% and 6% of dye and picloram, respectively. Photocatalytic processes were more efficient using TiO2/GL (96%-dye; 60%-picloram) than TiO2/BL (44%-dye; 40%-picloram). Photolysis using sunlight was not observed during PadronÒ recirculation in the reactor constructed with four borosilicate tubes. Meanwhile, adding H2O2 resulted in 12% conversion of dissolved organic compounds. Finally, the most efficient mineralization (60%) was obtained using the Fenton reaction ( H2O2-176 mmol L-1; FeSO4x6H2O-90 mmol L-1) and sunlight.

Aplicação do ultra-som em sistemas eletroquímicos: considerações teóricas e experimentais

The aim of this review is to present and discuss the applications of ultrasound in electrochemical systems such as in sonoelectroanalysis and sonoelectrolysis for the electrochemical combustion of organic compounds. Initially, theoretical and experimental aspects are discussed, particularly those related to the enhancement of mass transport and the surface cleaning effects. Some results are included to illustrate alternative geometries for the experimental measurements and the working electrodes used in these systems. In the sequence, the available publications are presented and discussed to demonstrate that ultrasound combined with electrochemical techniques is a powerful set-up for the detection of analytes such as metals and/or organic compounds in hostile media and for the effective destruction of toxic organic substances. At the end, a table summarizes the results already published in the literature.

Nióbia magnética como adsorvente de contaminantes orgânicos em meio aquoso: efeito da temperatura e do pH

This work describes novel materials based on pure iron oxide and iron oxide/niobia composite to produce a magnetic adsorbent. These materials were prepared with synthetic iron oxide and characterized by powder XRD, SEM, FTIR, TPR and Mössbauer spectroscopy. Results showed that the main iron oxides formed were goethite (aFeOOH) and maghemite (gFe2O3) with small particle size. The iron oxide and iron oxide/niobia composite showed high adsorption ability for organic compounds. The positive enthalpy indicated an endothermic adsorption process suggesting physical adsorption.

Aplicação da química quântica computacional no estudo de processos químicos envolvidos em espectrometria de massas

The field of application of mass spectrometry (MS) has increased considerably due to the development of ionization techniques. Other factors that have stimulated the use of MS are the tandem mass spectrometry (MS/MS) and sequential mass spectrometry (MSn) techniques. However, the interpretation of the MS/MS and MSn data may lead to speculative conclusions. Thus, various quantum chemical methods have been applied for obtaining high quality thermochemical data in gas phase. In this review, we show some applications of computational quantum chemistry to understand the formation and fragmentation of gaseous ions of organic compounds in a MS analysis.

Métodos simples de formação de monocristal de substância orgânica para estudo estrutural por difração de raios X

This work presents three operationally simple laboratory protocols for monocrystal growth of small-molecule organic compounds, which have been applied with success in the last ten years for the formation of single crystals for X-ray structural studies. In addition, five structure hints were formulated as general guidelines for selecting a small-molecule organic compound as a candidate for monocrystal growth: molecular weight >200 D, melting point >100 ºC, two or more aromatic rings in the structure, at least two sites for intermolecular hydrogen bond formation, and a halogen or other heavy atom in the structure.

Remoção do íon amônio de águas produzidas na exploração de petróleo em áreas offshore por adsorção em clinoptilolita

This work describes the use of clinoptilolite for removal of ammonium ions present in waters produced at the Campos' Basin. Samples were previously treated in order to remove organic compounds and metals. Experiments were run in fixed- and fluidized-bed systems, at room temperature. The fluidized-bed systems did not remove efficiently the ammonium ion. The best operational conditions were obtained with clinoptilolite particle size in the range 0.30-0.50 mm, under ascendant flow (3 mL min-1), in a fixed-bed system. The best zeolite performance was found when it was pretreated with 0.5 mol L-1 NaOH. Na+ was the most important interfering ion due to its high concentration in the water. Clinoptilolite lost partially its capacity to retain ammonium ions after several regeneration cycles with NaOH.