QuEChERS: um método moderno de preparo de amostra para determinação multirresíduo de pesticidas em alimentos por métodos cromatográficos acoplados à espectrometria de massas

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.

Oxidação do borneol à cânfora com água sanitária - um experimento simples, de baixo custo e limpo

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.

Determinação de resíduos de pesticidas em plasma bovino por cromatografia gasosa-espectrometria de massas

An analytical method for the isolation based on matrix solid-phase dispersion technique and gas chromatographic determination of pesticides in cattle plasma is presented. It was fortified 0.25 g of plasma with pesticides and blended with 1 g each C18 and Na2SO4. The homogenized matter was transferred to a SPE cartridge, which contained 1 g of activated florisil with 5 mL acetonitrile. The analites were eluted under vaccum with 15 mL acetonitrile, the extract was analyzed by gas chromatography-mass spectrometry. The limit of quantification of the method was 0.04 mg L-1 for chlorphenvinfos and fipronil and 0.02 mg L-1 for cypermethrin..

Síntese e caracterização de nanopartículas de óxido de ferro suportadas em matriz carbonácea: remoção do corante orgânico azul de metileno em água

In this work were prepared composites of iron oxide and carbonaceous materials in two different weight proportions (Carbon/Fe 1/1 and 1/2). The physico-chemical properties of the composites were determined by temperature programmed reduction (TPR), adsorption/dessorption of N2, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and pulse titration H2. The XRD and XPS analysis showed a cubic iron oxide phase, identified as maghemite, formed over the carbon surface. The particle size of maghemite showed to be within 10-30 nm. Carbon/Fe 1/2 was the most active in MB removal kinetics and ESI-MS studies showed that MB removal by both composites leads to oxidized intermediates.

Caracterização de lodo gerado em estações de tratamento de água: perspectivas de aplicação agrícola

The work reported here involved the characterization of sludges produced at water treatment plants in Jaboticabal-SP using FeCl3 as flocculant, and in Taquaritinga-SP and Manaus-AM using Al2(SO4)3 as flocculant. An evaluation was also made of the interaction of organic matter extracted from the sludges with different metal species. The results indicated that all the sludges produced at water treatment plants have an important agricultural potential and that their use depends on the characteristics of the raw water and the type of flocculant employed in conventional treatment. The humic substances extracted from the sludges showed different affinities for metal species, favoring eventual exchanges between potentially toxic metals and macro- and micronutrients. An alternative for the use of sludge in agriculture is to pretreat it to remove potentially toxic metals and enrich it with micro- and macronutrients that can be released to the plant.

Estudo geoquímico da disposição de lodo de estação de tratamento de água em área degradada

This survey determined the physical and chemical properties of the gravel place where urban sludge from Rio Descoberto's Water Treatment Plant is disposed. Physical, chemical and biological analysis of the soil samples (n=54), sludge samples (n=2), chemical coagulant (n=20) and samples from superficial waters (n=9) and water table (n=60) were performed. As results we can emphasize the horizontal distribution of mineral phases like gibbsite, organic material, exchanged Ca, available Mn and P on the soils are originated from the sludge. Some of these mobile elements could stimulate the growing of the vegetation, but they also could contaminate the water table.

Concentrações de amônio na água da chuva e estimativa de emissão de amônia de rebanhos domésticos de Pinheiro e Viana, Baixada Maranhense

Rainwater samples (bulk deposition samples) were collected in Pinheiro and Viana. Rainwater pHs were higher than the range usually expected for unpolluted rain (5.0-5.6). The highest values were found in the beginning of the rainy season. High concentrations of ammonium found in the rainwater samples could probably explain the high pHs. Grazing animals and other human activities, combined with soil characteristics and climatic conditions can be the potential factors controlling the rainwater concentrations of ammonium in Baixada Maranhense.

A qualidade de água como indicador de uso e ocupação do solo: bacia do Gama - Distrito Federal

The spread of Brasília isn't accompanied by correct support of land occupation, situation that is reflected in water quality. Under the optics of land use and occupation, working with multivariate statistics as main tool, water physical and chemical quality of Gama Catchment were assessed. During two years samples were collected and analyzed for 24 parameters. The statistical analysis showed the influence of civil buildings, agricultural activities and the best statistical parameters to a quickly assessment: nitrate, ammonia, suspended solids and aluminium.

Influência de diferentes sistemas de solvente água-etanol sobre as propriedades físico-químicas e espectroscópicas dos compostos macrocíclicos feofitina e clorofila α

This work focus on the influence of solvent on the photophysical properties of chlorophyll α and pheophytin. Both compounds are related to the photosynthesis process and are considered prototypes of photosensitizers in Photodynamic Therapy. Fluorescence measurements were developed using water/ethanol mixtures at different compositions, since both solvents could be employed in biological applications. The spectroscopic properties of these compounds undergo profound changes depending on water content in the ethanol due to auto-aggregation processes. The major hydrophobicity and the lower dielectric constant of ethanol when compared with water precluded significantly the auto-aggregation process of these compounds.

Nanoemulsões óleo de laranja/água preparadas em homogeneizador de alta pressão

The objective of this work was to use the high-pressure homogenizer (HPH) to prepare stable oil/water nanoemulsions presenting narrow particle size distribution. The dispersions were prepared using nonionic surfactants based on ethoxylated ether. The size and distribution of the droplets formed, along with their stability, were determined in a Zetasizer Nano ZS particle size analyzer. The stability and the droplet size distribution in these systems do not present the significant differences with the increase of the processing pressure in the HPH). The processing time can promote the biggest dispersion in the size of particles, thus reducing its stability.

Otimização e validação de métodos analíticos para determinação de BTEX em água utilizando extração por headspace e microextração em fase sólida

Three analytical methods for the determination of BTEX in water were optimized and validated. With the best method the analytes were extracted of 10 mL of sample with 2.50 g of NaCl in headspace vial of 20 mL by HS and SPME to 40 ºC for 30 min for adsorption and to 250 ºC for 4 min for desorption and were analyzed by GC-MS. The recovery was between 97.9% and 104.3%, and the limit of detection was 2.4 ng L-1 for o-xylene. This method was using to analyze BTEX in water supply and surface water in Ouro Preto city. No sample had concentrations of BTEX above the legislation.

Caracterização de contaminantes presentes em sistemas de tratamento de esgotos, por cromatografia líquida acoplada à espectrometria de massas tandem em alta resolução

This work shows results on the characterization, by liquid chromatography coupled to high resolution tandem mass spectrometry (LC-IT-TOF-MS) with electrospray ionization, of organic compounds present in raw and treated effluents from a combined sewage treatment systems (upflow anaerobic sludge blanket-trickling filter). The sewage samples were prepared by C18 solid phase extraction and the spectra obtained from the various extracts were submitted to principal component analysis to evaluate their pattern and identify the major deprotonated species. Some target compounds were submitted to semiquantitative analysis, using phenolphtalein as internal standard. The results showed the anaerobic step had little impact on the removal of anionic surfactants (LAS), fatty acids, and some contaminantes such as bisphenol A and bezafibrate, whereas the aerobic post-treatment was very efficient in removing these organics.

Avaliação e identificação de parâmetros importantes para a qualidade de corpos d'água no semiárido baiano. Estudo de caso: bacia hidrográfica do rio Salitre

Objective of this work was identifying superficial water quality parameters, significant to semi-arid hydrographic basins, minimizing costs of water monitoring. The Salitre river basin, an important sub-basin of the São Francisco river, was used as a case study. STD, Cl-, DO, BOD, pH, NO3-, PO4(3-), Al, Cu, Fe, Mn, Ni and Pb were considered the most significant parameters, with concentration levels found in some stretches of the basin not compliant with the current legislation. Some of the Salitre river basin sediments may represent a risk to the quality of the water body in relation to levels of nickel and zinc.

Caracterização do material particulado fino e grosso e composição da fração inorgânica solúvel em água em São José dos Campos (SP)

Air samples of fine (PM2,5) and coarse (PM2,5-10) particulate matter were collected in São José dos Campos from February 2004 to February 2005. Average PM10 mass concentrations was 31.2 ± 14.0 μg m-3, half of which belonging to the PM2.5 fraction. Ammonium and SO4(2-) were predominantly found in the fine fraction. Average (NH4)2SO4 concentration was estimated to be about 2.9 μg m-3. Chloride, Na+ and NO3- were mostly associated with PM2,5-10. Chloride deficits with respect to sea-salt Cl/Na ratio were found in both size fractions.

Alternativas verdes para o preparo de amostra e determinação de poluentes fenólicos em água

The restricted availability of water sources suitable for consumption and high costs for obtaining potable water has caused an increase of the conscience concerning the use. Thus, there is a high demand for "environmentally safe methods" which are according to the principles of Green Chemistry. Moreover, these methods should be able to provide reliable results for the analysis of water quality for various pollutants, such as phenol. In this work, greener alternatives for sample preparation for phenol determination in aqueous matrices are presented, which include: liquid phase microextraction, solid phase microextraction, flow analysis, cloud point extraction and aqueous two-phase systems.