Metodologias gerais empregadas no isolamento e identificação estrutural de feromônios de insetos

A selection of common procedures which are used for the identification and analysis of volatile biologically active compounds from insects are described.

Separação e identificação de constituintes químicos polares dos galhos de Porcelia Macrocarpa

This paper describes a methodology to separate and identify polar compounds as flavonoid and lignan glucosides, amino acids, salt of quaternary ammonium amino acid and carbohydrates from branches of Porcelia macrocarpa (Annonaceae).

Sistema em fluxo para determinação espectrofotométrica de uréia em plasma de sangue animal empregando leguminosa como fonte natural da enzima urease

A spectrophotometric flow injection analysis (FIA) procedure employing natural urease enzyme source for the determination of urea in animal blood plasma was developed. Among leguminous plants used in the Brazilian agriculture, the Cajanus cajan specie was selected as urease source considering its efficiency and availability. A minicolumn was filled with leguminous fragments and coupled to the FIA manifold, where urea was on-line converted to ammonium ions and subsequently it was quantified by spectrophotometry. The system was employed to determine urea in animal plasma samples without any prior treatment. Accuracy was assessed by comparison results with those obtained employing the official procedure and no significant difference at 90 % confidence level was observed. Other profitable features such as an analytical throughput of 30 determinations per hour, a reagent consumption of 19.2 mg sodium salicylate, 0.5 mg sodium hipochloride and a relative standard deviation of 1.4 % (n= 12) were also obtained.

Triterpenóides pentacíclicos de Mentha villosa: identificação estrutural e atribuição dos deslocamentos químicos dos átomos de hidrogênio e carbono

The structures of seven oleanene and ursene triterpenoids (1-7) isolated from aerial parts of Mentha villosa were identified. In addition, the complete ¹H and 13C resonance assignments of these triterpenoids were accomplished using 1D and 2D NMR spectroscopic experiments.

Identificação de pigmentos naturais de espécies vegetais utilizando-se cromatografia em papel

The use of natural dyes to demonstrate principles of paper chromatography is proposed. Extraction of the coloring compounds were performed in order to obtain the aglycone form of the anthocyanins present in the crude extracts. Separations were carried out on chromatographic paper with BAW (butanol/acetic acid/water) as mobile phase and the results compared with literature data. The crude extracts were obtained from Tibouchina granulosa, Rododhendron simsii, Impatiens walleriana flowers which are wildely found in Brazil and Phaseolus vulgaris L. grains skin which is the principal ingredient of the world famous "feijoada". Such species were chosen in order to attract the students attention since they are present in their quotidian, in agreement with the new proposals for Brazilian education.

Anestésicos locais: interação com membranas de eritrócitos de sangue humano, estudada por ressonância magnética nuclear de ¹H e 31P

The literature carries many theories about the mechanism of action of local anesthetics (LA). We can highlight those focusing the direct effect of LA on the sodium channel protein and the ones that consider the interaction of anesthetic molecules with the lipid membrane phase. The interaction between local anesthetics and human erythrocyte membranes has been studied by ¹H and 31P nuclear magnetic resonance spectroscopy. It was found that lidocaine (LDC) and benzocaine (BZC) bind to the membranes, increase the mobility of the protons of the phospholipid's acyl chains, and decrease the mobility and/or change the structure of the polar head groups. The results indicate that lidocaine molecules are inserted across the polar and liquid interface of the membrane, establishing both electrostatic (charged form) and hydrophobic (neutral form) interactions. Benzocaine locates itself a little deeper in the bilayer, between the interfacial glycerol region and the hydrophobic core. These changes in mobility or conformation of membrane lipids could affect the Na+-channel protein insertion in the bilayer, stabilizing it in the inactivated state, thus causing anesthesia.

Identificação de resíduos de disparos de armas de fogo por meio da técnica de espectrometria de massas de alta resolução com fonte de plasma indutivo

The violence derived from crimes involving firearms represents one of the main concerns of society. For this reason modern techniques have emerged in forensic science to identify suspects at crime scenes. This work describes a methodology to identify residues present in the hands of suspect by using a high resolution inductively coupled plasma mass spectrometry and collection procedure based on ethylenediaminetetraacetic acid (EDTA) solution as a complexing agent in moistened swabs. In order to distinguish real gunshot residues from others types of residues present in the hand of suspect, ternary ratio per cent diagrams were developed for antimony (Sb), barium (Ba) and lead (Pb) detected on the hands of volunteers, before and immediately after shooting tests, revealing a remarkable difference in both situations.

Análise sistemática de reagentes e resíduos sem identificação

This work presents a detailed routine applied to the identification of unknown chemicals and wastes. 786 specimens were analyzed during 20 months. Unknown materials fell into three basic classes: (i) commercial chemicals without labels or illegible ones; (ii) laboratory synthesis products; (iii) used solvents (including mixtures). Uranium and thorium were recovered form their wastes. Unknown chemicals were mainly inorganic compounds, many of which had never been opened. Alkaline salts were dominant, but also precious metal compounds were identified. Laboratory synthesis products were organic compounds. The final destination depended on the nature of the chemical. Most organic compounds were sent to incineration; inorganic salts were distributed among several public organizations, including secondary and technical schools. The work described in this paper greatly reduced the amount of wastes that had to be sent to disposal.

Imobilização de enzimas a partir de "kit" comercial: determinação de parâmetros metabólicos em sangue animal empregando multicomutação em fluxo

Automatic flow procedures based on the multicommutation concept, dedicated to the determination of 3-hydroxybutyrate, glucose and cholesterol are proposed. The enzymes were immobilized on glass beads and packed into mini-columns that were coupled to a flow system. Sampling throughputs of 55, 40 and 40 determinations per hour, linear response from 10 to 150, 50 to 600, 25 to 125 mg L-1, detection limits of 1.5, 14 and 4 mg L-1 and relative standard deviations of 1, 2 and 2% for 3-hydroxybutyrate, glucose and cholesterol, respectively, were achieved.

Identificação e quantificação do cristal violeta em aguardentes de mandioca (tiquira)

Tiquira is a traditional homemade alcoholic distillate produced in the Maranhão State (Brazil), gotten from cassava (Manihot esculenta, Crantz.). It can be normally found on street markets. Due to the addition of tangerine leaves, the original tiquira has a bluish color. Samples of this beverage were acquired in the local trade and analyzed from the spectroanalytical point of view. The results indicated that these drinks had been adulterated by the addition of crystal violet, a potencialy hazardous compound. The identification and quantification of crystal violet in 10 spiked samples was accomplished by UV-Vis spectrophotometry through the standard addition method. In order to verify the efficiency of the proposed method, experiments on the quantification and recovery were carried out and the results indicated a content of crystal violet in the 10-6 to 10-7 mol L-1 range.

Identificação de substâncias em análise toxicológica sistemática utilizando um sistema informatizado para cálculo de parâmetros cromatográficos e busca em bases de dados

In spite of the availability of large databases of chromatographic data on several standardized systems, one major task in systematic toxicological analysis remains, namely how to handle the experimental data and retrieve data from the large available databases in a meaningful and productive way. To achieve this purpose, our group proposed an Internet-based tool using previously published STA databases, which interlaboratorial reproducibility tests have already evaluated. The developed software has the capability to calculate corrected chromatographic parameters, after the input of data obtained with standard mixtures of calibrators, and search the databases, currently incorporating TLC, color reactions, GC and HPLC data. At the end of the process, a list with candidate substances and their similarity indexes is presented.

Identificação da influência do descarte de lodo de estações de tratamento de água

The growing concern of environmental surveillance of the quality of hydric resources guides the development of research on management of residues generated in water treatment plants (WTP). Approximately 8.000 WTPs in Brazil operate without a treatment program of the residues, disposing these effluents in the environment. This work evaluated WTP discharges into watercourses by collecting superficial waters, sediments and benthic samples at the town of Registro, São Paulo State, Brazil. Even though superficial waters and benthic samples showed no further contamination, sediment analysis pointed out that aluminum deposits detected near sludge discharges may represent a potential risk to the environment.

Espécies reativas de oxigênio e de nitrogênio, antioxidantes e marcadores de dano oxidativo em sangue humano: principais métodos analíticos para sua determinação

We review here the chemistry of reactive oxygen and nitrogen species, their biological sources and targets; particularly, biomolecules implicated in the redox balance of the human blood, and appraise the analytical methods available for their detection and quantification. Those biomolecules are represented by the enzymatic antioxidant defense machinery, whereas coadjutant reducing protection is provided by several low molecular weight molecules. Biomolecules can be injured by RONS yielding a large repertoire of oxidized products, some of which can be taken as biomarkers of oxidative damage. Their reliable determination is of utmost interest for their potentiality in diagnosis, prevention and treatment of maladies.

Procedimentos analíticos para identificação de antocianinas presentes em extratos naturais

Anthocyanins are among the most important plant pigments. Due to their potential benefits for human health, there is considerable interest in these natural pigments. Nonetheless, there is great difficulty in finding a technique that could provide the identification of structurally similar compounds and estimate the number and concentration of the species present. A lot of techniques have been tried to find the best methodology to extract information from these systems. In this paper, a review of the most important procedures is given, from the extraction to the identification of anthocyanins in natural extracts.

Isolamento e identificação da morina em mel brasileiro de Apis mellifera

The flavonoid fraction was purified by a combination of chromatography on Amberlite XAD-2 and preparative silica gel TLC. Morin (3, 5, 7, 2', 4'- pentahydroxyflavone) was the only flavonol found in honey from Brazilian Citrus sp.. The structure of morin was determined on the basis of UV and ¹H and 13C NMR spectral data together with literature references. This is the first report on the isolation of morin from Brazilian Citrus honey.