Integração de técnicas analíticas e proposta de experimentos para cursos de graduação em análise instrumental: uso de espectrômetro de absorção atômica para medidas de absorção molecular

Simple experiments are proposed for measuring molecular absorption of chromate and dichromate ions using an atomic absorption spectrometer. The experiments can help undergraduate students in instrumental analysis courses understand important aspects involving conceptual and instrumental similarities and differences between frequently used analytical techniques. Hollow cathode lamps were selected with wavelengths in the region of molecular absorption of chromate and dichromate. Calibration curves were obtained and the linear dynamic range was evaluated. Results were compared with those obtained in a molecular absorption spectrometer. The molar absorptivities obtained were also compared.

Avaliação dos tratamentos eletroquímico e fotoeletroquímico na degradação de corantes têxteis

This paper presents the study of the oxidation of three textile dyes (Remazol black B, Remazol Brilliant Orange 3R and Remazol Golden Yellow RNL) using electrochemical and photoelectrochemical methods. In both methods, electrolysis experiments were performed at a current density of 50 mA cm-2 in an aqueous solution of each dye (30 mg L-1), using a photoelectrochemical flow-cell. For all the dyes studied, the photoelectrochemical method was demonstrated to be more efficient than the electrochemical one. Photoelectrochemical oxidation resulted in complete decoloration after 90 min of electrolysis and total organic carbon (TOC) removal reached up to 36%. It was observed that the dyes presenting chromophores at higher wavelengths are removed the quickest, which indicates that photosensitised (photoassisted) oxidation occurs. The level of color was reduced to levels below the standards presented in the literature, which indicates the viability of the photoelectrochemical process as part of the treatment of textile effluents.

Simultaneous spectrophotometric determination of ezetimibe and simvastatin in pharmaceutical preparations using chemometric techniques

Two spectrophotometric methods are described for the simultaneous determination of ezetimibe (EZE) and simvastatin (SIM) in pharmaceutical preparations. The obtained data was evaluated by using two different chemometric techniques, Principal Component Regression (PCR) and Partial Least-Squares (PLS-1). In these techniques, the concentration data matrix was prepared by using the mixtures containing these drugs in methanol. The absorbance data matrix corresponding to the concentration data matrix was obtained by the measurements of absorbances in the range of 240 - 300 nm in the intervals with Δλ = 1 nm at 61 wavelengths in their zero order spectra, then, calibration or regression was obtained by using the absorbance data matrix and concentration data matrix for the prediction of the unknown concentrations of EZE and SIM in their mixture. The procedure did not require any separation step. The linear range was found to be 5 - 20 µg mL-1 for EZE and SIM in both methods. The accuracy and precision of the methods were assessed. These methods were successfully applied to a pharmaceutical preparation, tablet; and the results were compared with each other.

Cromatografia gasosa bidimensional abrangente (GC × GC)

This paper presents the fundamental principles, instrumentation and selected applications of comprehensive two-dimensional gas chromatography (GC × GC). In this technique, introduced in 1991, two capillary columns are coupled and proper modulating interfaces continuously collect the eluate from the first column, transferring it to the second column. The result is a geometric increment in the chromatographic resolution, ensuring separation of extremely complex mixtures in time periods shorter or comparable to those of analysis using conventional gas chromatography and with better detectabilities and sensitivities.

Sustainable drugs and global health care

Each day, Earth's finite resources are being depleted for energy, for material goods, for transportation, for housing, and for drugs. As we evolve scientifically and technologically, and as the population of the world rapidly approaches 7 billion and beyond, among the many issues with which we are faced is the continued availability of drugs for future global health care. Medicinal agents are primarily derived from two sources, synthetic and natural, or in some cases, as semi-synthetic compounds, a mixture of the two. For the developed world, efforts have been initiated to make drug production "greener", with milder reagents, shorter reaction times, and more efficient processing, thereby using less energy, and reactions which are more atom efficient, and generate fewer by-products. However, most of the world's population uses plants, in either crude or extract form, for their primary health care. There is relatively little discussion as yet, about the long term effects of the current, non-sustainable harvesting methods for medicinal plants from the wild, which are depleting these critical resources without concurrent initiatives to commercialize their cultivation. To meet future public health care needs, a paradigm shift is required in order to adopt new approaches using contemporary technology which will result in drugs being regarded as a sustainable commodity, irrespective of their source. In this presentation, several approaches to enhancing and sustaining the availability of drugs, both synthetic and natural, will be discussed, including the use of vegetables as chemical reagents, and the deployment of integrated strategies involving information systems, biotechnology, nanotechnology, and detection techniques for the development of medicinal plants with enhanced levels of bioactive agents.

Determinação de heparina fracionada em preparações farmacêuticas utilizando turbidimetria

A turbidimetric method has been used for quantification of fractionated heparin (FH) in pharmaceutical dosage. The UV detection at two wavelengths (290 and 500 nm) showed a significant increase in sensitivity of the method, specificity, and linearity to range 5.0-50.0 µg mL-1 and 50.0-200.0 µg mL-1, respectively (r < 0.99). At both wavelengths, the method was precise (inter-assay CV < 5.0%, and intra-assay CV < 3.0%), accurate (maximum deviation of ± 12%), and robust to the parameters evaluated. Turbidimetry proved to be easy, inexpensive and relatively fast. The results obtained attest to the reliability of the method.

Gemifloxacin mesylate: UV spectrophotometric method for quantitative determination using experimental design for robustness

This study describes the validation of UV spectrophotometric method for quantitative determination of gemifloxacin mesylate (GFM) in tablets using methanol as solvent. The method was specific, linear, precise, exact and robust at 272 and 343 nm. The results confirmed that the method in both wavelengths is valid and useful to the routine quality control of GFM in coated tablets. The validate method was compared to liquid chromatography (HPLC), microbiological assay and visible (VIS) spectrophotometry, which were previously developed and validated to the same drug. There was not significative difference between the methods for GFM quantitation.

Aplicação da radiação ultravioleta como forma de contribuição para a química verde e construção de um reator fotoquímico alternativo e de baixo custo, para pré-tratamento de amostras

Ultraviolet radiation corresponds to a fraction of electromagnetic radiation, covering wavelengths between 1 and 400 nm. Methods based on UV irradiation have become popular because it is possible to treat samples simply by applying energy, avoiding procedures that require the use of toxic substances, thus contributing to the development of Green Chemistry. This study aimed to assess the main applications of UV radiation reported in the literature and thoroughly described the construction of an alternative and low-cost photochemical reactor to be used for the pretreatment of samples in the laboratory. The use of this new photochemical reactor in the clean-up of milk samples for spectrofluorimetric measurements was also reported.

DFT study on low molecular weight α,α-ditert-butyl-4H-cyclopenta[2,1-b,3;4-b']dithiophene and α,α-ditert-butyl-4H-cyclopenta[2,1-b,3;4-b']dithiophene S-oxide bridged derivatives

The equilibrium geometries of α,α-ditert-butyl-4H-cyclopenta[2,1-b,3;4-b']dithiophene (DBDT) and α,α-ditert-butyl-4H-cyclopenta[2,1-b,3;4-b']dithiophene S-oxide (DBDTO) were studied at the DFT level of theory with a standard 6-311G* basis set. The molecular structures of the DBDT series were more planar than the corresponding DBDTO series, as revealed by dihedral angles. The UV-visible absorption calculated at TD-DFT/6-311G* showed two absorption peaks for all the molecules except C=S and C=O bridged molecules. In DBDTOs, C=S and C=O bridged molecules showed three and four absorption peaks, respectively. The DBDTOs had lower band gaps and longer wavelengths compared to the corresponding DBDTs.