Discriminação entre estádios de maturação e tipos de processamento de pós-colheita de cafés arábica por microextração em fase sólida e análise de componentes principais

A fruit chemical composition reflects its maturation stage. For coffee, it is also the reflex of the post-harvesting processing type, dry, semi-wet and wet. The object of this work was to verify if headspace solid phase microextraction coupled to gas chromatography (HS-SPME-GC) could be used to discriminate between samples harvested in different maturation stages and treated by different processes. With application of principal component analysis to the area of 117 compounds extracted by SPME, using divinylbenzene/Carboxen/polydimethylsiloxane fiber, it was possible to discriminate, in the roasted and ground coffee, the maturity stage and processing type used .

Análise de pesticidas organoclorados em água usando a microextração em fase sólida por headspace com cromatografia gasosa e espectrometria de massas

A method based on headspace - solid phase microextraction coupled with gas chromatography - mass spectrometry was validated for the quantitative determination of 18 organochlorine pesticides in water. For the extraction conditioning some parameters as the best type of coating fiber, time and temperature of extraction, pH and ionic strength were evaluated. The method HS-SPME/GC-MS/MS showed linear coefficient above 0.9948. The repeatability of the measurements were lower than 7.6%. Relative recoveries were between 88 and 110%. Limits of detection from 0.5 x 10-3 to 1.0 mg L-1 were obtained. A total of 31 samples were analyzed and 16 presented from 1 to 5 pesticides.

Interação de átomos leves com clusters de metais de transição

Density Functional Theory (DFT) calculations on the interactions of small atoms (H, C, O, and S) on first-row transition metal clusters were performed. The results show that the adsorption site may vary between the metal surface and the edge of the cluster. The adsorption energies, adatom-nearest neighbor and adatom-metal plane distances were also determined. Finally, the authors present a discussion about the performance of these metals as anodes on solid oxide fuel cells. The results obtained agree with empirical data, indicating that the theoretical model used is adequate

Análise e discriminação de quimiotipos de Lippia graveolens H.B.K. da Guatemala por microextração em fase sólida, CG-EM e análise multivariada

SPME-GC-MS, PCA and HCA multivariate techniques were used in order to evaluate their applicability to discriminate the three chemotypes (thymol, carvacrol and mixed) described for L. graveolens of Guatemala. The leaves of L. graveolens are used for treatment of colds, bronchitis, and as seasoning for food preparations, yielding essential oil up to 4.34 %. Leaves of 35 individuals from eight populations, and eight composite samples were analyzed using a DVB/Carboxen/PDMS fiber and GC-MS. PCA and HCA were carried out using eight markers (p-cymene, cis-sabinene hydrate, linalool, terpinen-4-ol, thymol, carvacrol, (E)-caryophyllene and caryophyllene oxide). The three chemotypes of L. graveolens were satisfactorily discriminated.

Investigando cinza da casca do arroz como fase estacionária em cromatografia: uma proposta de aula experimental nos cursos de graduação

This article describes an experiment that involves the extraction and separation of the pigments of spinach extract by column chromatography using the silica obtained from rice husk ash as a stationary phase. The experimental procedure is very simple to apply in the chemistry laboratory, and allowed to illustrate some concepts of organic chemistry: structure of organic molecules, solubility, polarity, extraction, partition coefficient, adsorption and retention factor (Rf), as well as objectives and fundamentals of chromatographic methods. The experiment can be carried out in a 4 h period.

Determinação de bifenilos policlorados em milho através de extração em fase sólida seguida de cromatografia a gás acoplada à espectrometria de massas

This paper describes an analytical method for analyzing polychlorinated biphenyls in corn samples using solid phase extraction (SPE) followed by determination by GC-MS. All calibration curves proved linear (r> 0.99). Recoveries ranged between 74.1 and 110.6% with relative standard deviation lower than 20% for all compounds. The limits of quantitation for the method were between 0.025 and 0.1 ng g-1. Of the 51 samples analyzed, PCB 180 showed the highest frequency, being detected in more than 39%, followed by PCB 138, detected in more than 33% of samples.

Adição de anilinas à naftoquinona em água e em fase sólida

Considering all the aspects of the principles of green chemistry, we present herein the addition reactions of amines to 1,4-naphthoquinone in water as solvent and also in solid phase. These reactions resulted in very colorful products that were easily monitored by thin layer chromatography and consequently easy to separate. Therefore, they are interesting experiments for experimental organic chemistry in the classrooms or in the laboratories.

Fatores que influenciam a formação da fase β-PbO2 em filmes eletrossintetizados galvanostaticamente sobre substrato de tecido de carbono

PbO2 films were electroformed onto carbon cloth substrates (twill woven type) in acid conditions using the nitrate precursor by changing the electrodeposition current density, temperature and pH, in order to optimize the formation of the β-PbO2 phase. The crystal structure and morphology of the PbO2 films were investigated using X-ray diffraction (XRD) and scanning electronic microscopy (SEM) techniques. The optimum conditions obtained for formation of the β-PbO2 were presented and discussed.

Resíduos de pesticidas em águas superficiais de área de nascente do Rio São Lourenço-MT: validação de método por extração em fase sólida e cromatografia líquida

A multiresidue method using HPLC/DAD for the determination of fourteen pesticides in water based on SPE, using SDVB (styrene divynilbenzene copolymer) as adsorbent was validated. Recoveries from 61 to 120%, relative standard deviation between 2 and 15% and detection limits from 0.07 to 0.75 µg L-1 were obtained. It was applied to 66 surface water samples collected in a degraded area at the headwaters of São Lourenço river, Mato Grosso, Brazil. Eight pesticides were detected in concentrations ranging from 0.15 to 35.25 µg L-1. Considering ecotoxicological data, carbendazim and carbofuran may represent a risk to aquatic organisms. These results draw attention to the contamination of this vulnerable degraded area.

Câmara de volatilização: uma alternativa para avaliação da eficiência de amostragem de α- e β-endossulfam em fase gasosa

The efficiency of XAD®-2 resin in sampling the pesticides α and β-endosulfan from air contaminated in the laboratory was evaluated. Sampling efficiency ranged from 87 to 108% for α-endosulfan and from 71 to 84% for β-endosulfan with relative standard deviation lower than 19%. The pesticides were not detected in the second section of the cartridge showing the good retention capacity of XAD®-2 for these analytes. Method quantification limits were 0.32 and 0.34 µg m-3 for α and β-endosulfan, respectively. These results suggest that the proposed method may be useful for evaluating occupational exposure to these compounds.

A etimologia de biomoléculas com metais de transição como auxiliar na aprendizagem de Química Biológica

Numerous functional biomolecules are associated with metals, i.e. the metallobiomolecules; more specifically, some are dependent on transition metals required for several crucial biological roles. Nevertheless, their names can lead to ambiguous interpretations concerning the properties and performances of this group of biological molecules. Their etymology may be useful by providing a more perceptive insight into their features. However, etymology can lead to incongruous conclusions, requiring an especially careful approach to prevent errors. Examples illustrating these subjects shall be examined.

Equipamento de baixo custo para extração em fase sólida em amostras aquosas de grande volume utilizando pressão positiva de N

Extraction/concentration is a crucial step for the analysis of organic compounds at trace level concentrations and dispersed in complex matrices. Solid-phase extraction (SPE) is one of the techniques used for this purpose. In this work, a low cost apparatus for SPE was developed that uses nitrogen under positive pressure and ensures the maintenance of the sample flow, while also allows the simultaneous extraction of different samples without cross-contamination and sample contact with plastic materials. For the system set up, easily accessible materials were used such as hypodermic needles, stainless steel tubes, rubber stoppers, and 3-way valves from serum delivery apparatus.

Biocatálise heterogênea em fase sólido/gás: princípios e aplicações

Enzymatic conversion of gaseous substrates into products in aquo-restricted media, using enzymes or whole cells (free and immobilized) as biocatalysts, constitutes a promising technology for the development of clearer processes. Solid-gas systems offer high production rates for minimal plant sizes, allow important reduction of treated volumes, and permit simplified downstream processes. In this review article, principles and applications of solid-gas biocatalysis are discussed. Comparisons of its advantages and disadvantages with those of the organic- and aqueous-phase reactions are also presented herein.

Determinação do coeficiente de atividade na diluição infinita em sistemas etanol-água-sal por microextração em fase sólida-gc-fid

A new method using the headspace solid phase microextraction (HS-SPME) technique was used to evaluate the infinite dilute activity coefficient (γ1∞) in an alcohol/water/salt system. The studied systems were ethanol and water with NaCl and NH4Cl at salt concentrations of 5, 10, 15, and 30% m/v and temperatures of 303.15 and 313.15 K. The method was used to investigate the salt effect on vapor/liquid equilibrium in an ethanol/water system, yielding satisfactory results. The study focused on the rich side in ethanol. The data were compared with the literature infinite dilution data determined by other methods such as differential ebulliometry (EBUL), differential static cell equilibrium (STAT), and gas-liquid chromatography with no gas phase correction (GC). In this study, NaCl showed better separation rates than NH4Cl.

Desenvolvimento de reator tipo "dip catalyst" para filmes poliméricos contendo nanopartículas de metais de transição

This article describes the development of a new catalytic reactor designed to operate with nanoparticle-embedded polymer thin films. Stabilization of metal nanoparticles in films that serve as catalysts in organic reactions is relatively new; therefore, the development of reactors to facilitate their use is necessary. We describe in detail the preparation of the GDCR reactor-type "dip catalyst" and its evaluation in the Suzuki - Miyaura cross-coupling reaction of phenylboronic acid and 4-bromoanisole catalyzed by palladium nanoparticle-embedded cellulose acetate thin film (CA/PD(0)). Compared with earlier prototypes, GDCR reactor showed excellent results when operating with CA/PD(0) thin films.