Cafeína: revisão sobre métodos de análise

Gravimetric and Bailey-Andrew methods are tedious and provide inflated results. Spectrofotometry is adequate for caffeine analysis but is lengthy. Gas chromatography also is applied to the caffeine analysis but derivatization is needed. High performance liquid chromatography with ultraviolet detection (HPLC-UV) and reversed phase is simple and rapid for xanthine multianalysis. In HPLC-UV-gel permeation, organic solvents are not used. HPLC-mass spectrometry provides an unequivocal structural identification of xanthines. Capillary electrophoresis is fast and the solvent consumption is smaller than in HPLC. Chemometric methods offer an effective means for chemical data handling in multivariate analysis. Infrared spectroscopy alone or associated with chemometries could predict the caffeine content in a very accurate form. Electroanalytical methods are considered of low cost and easy application in caffeine analysis.

Photomultiplier nonlinear response in time-domain laser-induced luminescence spectroscopy

A new procedure to find the limiting range of the photomultiplier linear response of a low-cost, digital oscilloscope-based time-resolved laser-induced luminescence spectrometer (TRLS), is presented. A systematic investigation on the instrument response function with different signal input terminations, and the relationship between the luminescence intensity reaching the photomultiplier and the measured decay time are described. These investigations establish that setting the maximum intensity of the luminescence signal below 0.3V guarantees, for signal input terminations equal or higher than 99.7 ohm, a linear photomultiplier response.

Influência de desproteinizantes ácidos na quantificação da glutationa reduzida eritrocitária por CLAE-UV

Large differences in reduced glutathione (GSH) levels have been found in different investigations, also in healthy people. GSH oxidation in vitro has been associated with sample acidification in the presence of oxihemoglobin. In this work, the influence of different acids on GSH determination utilizing HPLC with UV detection was evaluated. The results showed that metaphosphoric acid and sulfosalicylic acid were inadequate for analysis, because metaphosphoric acid showed to be inefficient for deproteinization and with sulfosalicylic acid loss of GSH was observed. Trichloroacetic acid did not effect GSH quantification, since the deproteinized form was immediately derivatized with 5, 5´-dithio-bis (2-nitrobenzoic) acid. Methods with TCA deproteinization presented linear results from 0.5 to 3.0 mM. The correlation coefficient between aqueous curves and GSH spiked RBC exceeded 0.99. Precision calculations showed CV lower than 10% and bias within ± 10% for concentrations of 0.5; 1.5 and 3.0 mM GSH. The recovery was higher than 94%. Moreover, GSH blood concentrations were independent of hemoglobin concentrations.

Aplicação de radiação UV artificial e solar no tratamento fotocatalítico de efluentes de curtume

Tannery effluents are very dangerous for the environment since they contain large amounts of dangerous and biorecalcitrant contaminants (organic matter and Cr(VI)). This paper reports the efficiency of heterogeneous photocatalysis, based on the application of solar and artificial radiation, furnished by UV lamps, using TiO2 fixed on a flat plate, in the treatment of synthetic effluents. The results of COD and Cr(VI) demonstrate that the use of solar radiation is the most efficient way to perform the photocatalytic treatment of these effluents since a minimum removal of 62 and 61% was observed for Cr(VI) and organic matter, respectively.

Análise química de pigmento vermelho em osso humano

This work presents a chemical study of human bones painted red located at the Morro dos Ossos site, Piauí State, Brazil. The pigment was studied using X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), scanning electron microscopy (SEM), complexation reactions with thiocyanate and UV-Vis absorption spectroscopy. The results confirmed the presence of ochre and that the pigment layer is essentially composed of a mixture of clay and hematite, α-Fe2O3.

Extração de β-caroteno de cenouras: uma proposta para disciplinas experimentais de química

This paper reports on the development of a simple and fast procedure for β-carotene extraction from carrots and its quantification by UV/Vis spectroscopy. Carotenoids extracted from carrots may also be used as alternative reagents for TLC (thin layer chromatography) detection of natural compounds with antioxidant properties, replacing the commercial p.a. grade β-carotene. Although this reagent had around 10% b-carotene, it proved to be as efficient for TLC analysis as the commercial p.a. grade β-carotene. This practice is a useful alternative for teaching undergraduate organic chemistry laboratory classes.

Materiais à base de óxido de ferro para oxidação de compostos presentes no efluente da despolpa do café

Materials based on pure iron oxide and impregnated with niobia (Nb2O5) were prepared. Their catalytic activities were tested on the oxidation of compounds present in the wastewater from the processing of coffee berries. Particularly caffeine and catechol were tested. The oxidation reactions were carried out with the following systems (i) UV/H2O2, (ii) photo-Fenton and (iii) heterogeneous Fenton. All materials were characterized with X-ray diffraction, Mössbauer and infrared spectroscopy. Iron was mainly in the forms of goethite and maghemite. The oxidation kinetics were monitored by UV-vis and the oxidation products were monitored by mass spectrometry. The photo-Fenton reaction presented highest oxidation efficiency, removing 98% of all caffeine and catechol contents.

Performance characteristics of bioassay UV-spectrophotometry and high perfomance liquid chromatographic determination of gatifloxacin in tablets

The microbiological bioassay, UV-spectrophotometry and HPLC methods for assaying gatifloxacin in tablets were compared. Validation parameters such as linearity, precision, accuracy, limit of detection and limit of quantitation were determined. Beer's law was obeyed in the ranges 4.0-14.0 μg/mL for HPLC and UV-spectrophotometric method, and 4.0-16.0 μg/mL for bioassay. All methods were reliable within acceptable limits for antibiotic pharmaceutical preparations being accurate, precise and reproducible. The bioassay and HPLC are more specific than UV-spectrophotometric analysis. The application of each method as a routine analysis should be investigated considering cost, simplicity, equipment, solvents, speed, and application to large or small workloads.

Quantitation of genistein and genistin in soy dry extracts by UV-Visible spectrophotometric method

This paper describes the development and validation of an UV-Visible spectrophotometric method for quantitation of genistein and genistin in soy dry extracts, after reaction with aluminum chloride. The method showed to be linear (r²= 0.9999), precise (R.S.D. < 2%), accurate (recovery of 101.56%) and robust. Seven samples of soy dry extracts were analyzed by the spectrophotometric validated method and by RP-HPLC. Genistein concentrations determined by spectrophotometry (0.63% - 16.05%) were slightly higher than values obtained by HPLC analysis (0.40% - 12.79%); however, the results of both methods showed a strong correlation.

Efeito do intemperismo artificial em quatro madeiras tropicais monitorado por espectroscopia de infravermelho (DRIFT)

Four tropical woods, were investigated to compare their performance and natural resistances to artificial weathering using the diffuse reflectance infrared Fourier transform spectroscopy (DRIFT). The species were garapeira (Apuleia leiocarpa), itaúba (Mezilaurus itauba) and tauari (Couratari sp.), woods traditionally indicated for exterior uses, and marupá (Simarouba amara), that served as reference. The samples were submitted to cycles of UV radiation (350 nm) and water until 2,000 h. The photodegradation processes of woods surfaces were accomplished monitoring the changes in the intensities associated to lignin (1508 cm-1) and carbonyl group (1736 cm-1) absorptions. The results have shown that lignin was the first component to be photodegradated, resulting in surfaces mainly composed by cellulose, after 2,000 h of UV irradiation. The processes of formation and lixiviation of carbonyl compounds were different for each species. The experimental conditions used in this work were too severe to evaluate the wood density and extractives content influences during the treatment.

Vanadium-modified molecular sieves: preparation, characterization and catalysis

Vanadium-containing molecular sieves are redox catalysts and are good candidates as substitutes for oxide-supported V2O5 in a number of reactions. These materials have the advantage of presenting better dispersion of vanadium species, as well as shape-selective properties and controllable acidities. They may be prepared by one-pot synthesis or by post-synthesis methods and a number of techniques such as diffuse reflectance UV-visible spectroscopy, 51V nuclear magnetic resonance and electron paramagnetic resonance, to name but a few, have been used to characterize these materials. In this review, methods of preparation of vanadium-modified molecular sieves, their characterization and applications in catalysis are discussed.

Validation of a simple and rapid UV spectrophotometric method for dexamethasone assay in tablets

This work reports the validation of an analytical UV spectrophotometric method to assay dexamethasone in tablets (assay and dissolution studies). The method was linear in the range between 1 and 30 µg mL-1 presenting a good correlation coefficient (r = 0.9998, n = 7). Precision and accuracy analysis showed low relative standard deviation (< 2.00%) and good percentual recoveries (95-105%). The procedure was linear, accurate, precise, and robust. The method is simple, and it has low cost. It does not use polluting reagents and can be applied in dissolution studies, being an adequate alternative to assay dexamethasone in tablets.

Validação de metodologia para a determinação simultânea dos antioxidantes sintéticos em óleos vegetais, margarinas e gorduras hidrogenadas por CLAE/UV

The use of antioxidants either to prevent or retard food's lipids oxidation was approved after inquires that verified their security within a daily intake limit. In this study, the methodology was developed and validated for the analysis of synthetic antioxidants: propylgallate (PG), tert-butylhydroquinone (TBHQ), butylhydroxyanisole (BHA), octylgallate (OG) and butylhydroxytoluene (BHT) in vegetables oils, margarine and hydrogenated fats by high performance liquid chromatographic. The methodology revealed itself efficient, with recovery rates above 90% for all antioxidant substances, besides good linearity in concentration range of 40-240 mg kg-1 (r = 0,999), repeatability with CV < 3,7% and limit of quantification 16.55, 10.32, 1.40, 3.76 and 9.30 mg/kg for BHT, BHA, PG, OG and TBHQ, respectively.

UVA I-protection effectiveness of bioactive compound and organic UV filters: an in vitro assessment

This research work aimed at determining the UVA effectiveness (UVA I/UV ratio), by diffuse transmittance analysis, of sunscreens developed with a bioactive substance, the rutin, associating or not with organic UVB-UVA filters incorporated at a phosphate-base O/W emulsion. Sunscreens provided conflicting and unpredictable results concerning the anti-UVA protection, specially, at the UVA I region. Possible interactions among the organic UV filters and the polyphenolic bioactive substance may have accounted with improvement or reduction of UV protection by a complex and not yet elucidated mechanism, probably regarding wavelength delocalization to superior or inferior values, by resonant molecule stabilization or destabilization.

Síntese e estudo de ortossilicatos de zinco luminescentes com aplicação da técnica sol-gel

Usually, the concepts of the Sol-Gel technique are not applied in experimental chemistry courses. This work presents a feasible experiment for chemistry instruction, which involves the synthesis of luminescent materials - Zn2SiO4, with and without Mn2+ as a dopant - by the Sol-Gel technique. The obtained materials were analyzed by scanning electron microscopy, X-Ray diffraction, IR spectroscopy and luminescence measures by UV-vis spectroscopy. The results allow the students to confirm the luminescent properties of the zinc orthosilicate luminophores as well as the structural features expected from literature data.