Distribuição espacial de compostos orgânicos de estanho em sedimentos costeiros e em Phallusia nigra da Baía de Todos os Santos e litoral norte da Bahia - Brasil

Organic tin compounds were investigated in the sediment of twenty-four stations located in the Todos os Santos Bay and the north coast of Bahia - Brazil. The concentration of these organic tin was also determined in a ascidium species of Phallusia nigra. The speciation and quantification was performed by GC-MS/MS. The highest concentrations were: tributyltin (TBT) 438 ng g-1, dibutyltin (DBT) 207 ng g-1, monobutyltin (MBT) 423 ng g-1, diphenyltin (DPT) 25.8 ng g-1 and monophenyltin (MPT) 55.0 ng g-1. DBT and MBT were found in Phallusia nigra, with highest concentrations of 294.1 and 148.5 ng g-1, respectively.

Óleos essenciais das folhas de Vernonia Remotiflora e Vernonia Brasiliana: composição química e atividade biológica

The chemical composition of the essential oils, obtained by hidrodistillation, from leaves of two Vernonia species (V. remotiflora and V. brasiliana), was determined by GC-FID and GC-MS. Both essential oils were predominantly constituted by sesquiterpenes (92.0 - 93.4%). The main constituents of the oil from V. brasilana were (E)-caryophyllene (36.7%), germacrene D (35.5%), and α-humulene (11.7%), while (E)-caryophyllene (42.2%) and bicyclogermacrene (20.0%) were the major ones in the oil from V. remotiflora. Although with moderate activity both oils showed acetylcholinesterase and antibacterial activities.

Desenvolvimento de métodos analíticos para determinação de agrotóxicos em sedimentos por cromatografia gasosa monodimensional e bidimensional abrangente com micro detector de captura de elétrons

The development of analytical methods for determination of eight pesticides of different chemical classes (trichlorfon, propanil, fipronil, propiconazole, trifloxystrobin, permethrin, difenoconazole and azoxystrobin) in sediments with gas chromatography-micro-electron capture detector (GC/µECD) and comprehensive two-dimensional gas chromatography with micro-electron capture detector (GCxGC/µECD) is described. These methods were applied to real sediment samples, and the best results were obtained using a 5% diphenyl-methylpolysiloxane column for 1D-GC. For GCxGC the same column was employed in the first dimension and a 50%-phenyl-methylpolysiloxane stationary phase was placed in the second dimension. Due to the superior peak capacity and selectivity of GCxGC, interfering matrix peaks were separated from analytes, showing a better performance of GCxGC.

Uma métrica gráfica para avaliação holística da verdura de reacções laboratoriais - "Estrela Verde"

A new semi-quantitative metrics, Green Star (GS), for evaluation of the global greenishness of chemical reactions used in teaching laboratories has been developed. Its aim is to help choosing the more acceptable reactions for implementing Green Chemistry (GC) and to identify suitable modifications of reaction protocols to improve the greenishness of chemistry. GS considers globally all the Twelve Principles of GC. To illustrate its construction, the tetraamminecopper(II) sulfate monohydrate laboratory synthesis, performed under several sets of conditions to pursue greenishness, is presented. A comparative study with other GC metrics showed the advantages of GS and that it accomplishes its purpose.

Influência dos constituintes químicos dos extratos de diferentes matrizes na resposta cromatográfica de agrotóxicos

Multiresidue methods for pesticides monitoring by GC are commonly employed, however, it is well known that the presence of compounds of the matrix introduces errors during the quantiûcation. The main consequence of matrix effect is an increasing or decreasing analyte signal after the GC saturation with extracts of matrix. In this paper, the influence of constituents of nine matrices on the quantification of the four pesticides by GC-ECD was studied. Variation of signal was evaluated by PCA and HCA, and results showed that the constituents of tomato increased the signal (until 300%), while extracts of apple decreased (until -20%). Variation the analyte signal in the presence of the matrix in respect to the same analyte in solvent (standard solution) also was observed, mainly for liver extract (until 270%).

Chemical constituents of the wood from Zanthoxylum quinduense Tul. (Rutaceae)

Phytochemical investigation of the wood from Zanthoxylum quinduense Tul. allowed the isolation and identification of norchelerythrine, decarine, 6-acetonyldihydrochelerythrine, syringaresinol, evofilin C, p-hydroxybenzaldehyde, vanillic acid, a mixture of β-sitosterol, stigmasterol and campesterol and a mixture of saturated and unsaturated fatty acids, and their esters derivatives. The structures of the isolated compounds were elucidated by spectroscopic techniques and comparison with literature data and the mixture of sterols and fatty acids were identified by GC/MS. The antifungal activity of the ethanolic extract, fractions and pure compounds against Fusarium oxysporum f. sp. lycopersici was determined by bioautography. Evofilin C and nochelerytrine were the only substances that present antifungal activity.

Variabilidade química de compostos orgânicos voláteis e semivoláteis de populações nativas de Maytenus ilicifolia

This work is focused on the chemical distribution of volatile and semi-volatile compounds of 18 native populations of Maytenus ilicifolia collected all over Brazil. The extracts of bulk samples (30 plants) of each population were obtained by supercritical CO2 extraction technique, and analyzed by GC/MS. The quantification of compounds (phytol, squalene, vitamin E, limonene, stigmasterol, friedelan-3-ol, friedelin, fridelan-3-one, palmitic acid and geranyl acetate) showed significant variations within the different populations, which could be related tom microclimate characteristics.

Chemical composition of volatile oils from leaves of Nectandra megapotamica Spreng. (Lauraceae)

The volatile oils from Nectandra megapotamica Spreng. leaves, collected in February and August of 2007 and at 7:00 and 12:00 h (samples A - D), were extracted by hydrodistillation and the chemical composition was analyzed by GC-FID and GC/MS. A total of nineteen compounds were identified with predominance of oxygenated sesquiterpenes, among them, α-bisabolol, was the main constituent (62.3-69.4 %). After chromatographic separation procedures, this compound was purified from crude oil and its structure was confirmed by analysis of NMR data. This paper describes for the first time the composition of the leaves volatile oil from N. megapotamica.

Interespecific variation in the composition of volatile oils from the leaves of Swietenia macrophylla King (Meliaceae)

The volatile oils from leaves of five Brazilian specimens of Swietenia macrophylla King (Meliaceae) collected in three different Amazon Rainforest Conservation Areas in the States of Mato Grosso, Pará, and Rondônia were extracted and analyzed by GC and GC/MS. The oils showed to be composed by terpenoids, majority hydrocarbon sesquiterpenes, being germacrene D (20.5-46.8%) and bicyclogermacrene (8.3-11.1%) the main components. Besides these derivatives, only α-cubebene, β-caryophyllene, β-gurjunene and γ-cadinene were detected in all of the analyzed samples. This analysis indicated a great diversity of constituents in the oils obtained from specimens collected in these regions, which could be associated to the different susceptibility in the attack of H. grandella in S. macrophylla cultures.

Variação anual do rendimento e composição química dos componentes voláteis da Siparuna guianensis Aublet

This work describes the volatile composition obtained by hidrodistillation of fresh leaves of Siparuna guianensis Aublet collected from Cuiabá (MT), Brazil. The composition of DCM extract of hydrolate was determined by GC-MS analysis and the results showed that the specie present a range of components according to their phenology and period of the leaves were collects. The highest volatile components yield was obtained during the reproductive period and the principal compound was the siparunone.

Constituintes químicos e efeito ecotoxicológico do óleo volátil de folhas de Eucalyptus urograndis (Mirtaceae)

The volatile oil from the leaves of E. urograndis was analyzed by GC and GC-MS. It was identified 10 compounds in which, orto-cimene (41.4%) and 1,8-cineol (25.8%) were the main constituents. The induction of deleterious effect to aquatic organisms due to the presence of volatile oil lixiviated from E. urograndis leaves was studied using Daphnia laevis and D. similis as bioindicators. Through the results of toxicological tests it was possible to show that the litterbag of E. urograndis represents a risk factor for the aquatic ecosystem of lakes and rivers that are in the surrounding area of large scale Eucalyptus plantations. The method can be used for monitor the quality of these types of aquatic environments.

Avaliação do uso de inibidores de etileno sobre a produção de compostos voláteis e de mangiferina em manga

Effects of two ethylene inhibitors, 1-methylcylopropene (1-MCP) and aminoethoxyvinylglycine (AVG), on production of volatile compounds and mangiferin (a bioactive xanthone) in 'Tommy Atkins' mango fruit were investigated. Volatile composition and mangiferin content, in treated and untreated fruits at three maturity, stages were determined by SPME-GC-MS and HPLC, respectively. These chromatographical analysis revealed that the volatile profiles and mangiferin concentrations were not significantly different, suggesting that the use of ethylene inhibitors does not affect the mango aroma and functional properties relative to this xanthone. Moreover, a simple, precise and accurate HPLC method was developed for quantifying mangiferin in mango pulp.

Análise comparativa entre vários métodos de quantificação de hemiceluloses da madeira de eucalipto

Pulp hemicelluloses can be extracted with NaOH and quantified by colorimetric and gravimetric techniques. However the most usual methods to measure eucalyptus pulp hemicelluloses have been through the pentosan method or through xylan analyses by GC or HPLC techniques. In this study a comparison was made between the more traditional methods and indirect method of NaOH 5% extraction followed by colorimetric analyses. It was observed that the content of NaOH 5% extract correlates very well with pulp xylan content and reasonably well with the pentosan content. It is concluded that the 5% NaOH solubility method can be used in replacement of the other two, since it is faster, simpler and less costly to carry out than the others.

Estimativa da incerteza de medição em análise cromatográfica: abordagem sobre a quantificação de carbamato de etila em cachaça

The measurement uncertainty is useful to estimate the confidence of analytical results. Nowadays, a result without the uncertainty statement cannot be considered reliable, but the scientific literature still lacks examples of the estimate of the measurement uncertainty. This paper presents a practical and reliable description of the measurement uncertainty estimation of the analytical determination of ethyl carbamate in cachaça by GC-IDMS. The isotope dilution technique (ID) associated with GC-MS was used to improve the accuracy. The uncertainty estimated corresponds to 10% of the mass fraction of ethyl carbamate (115 ± 11) ng/g, which is in agreement with ppb level.

Benzo(a)pireno, carbamato de etila e metanol em cachaças

The objective of this work was to evaluate the presence of benzo(a)pyrene (BaP), ethyl carbamate (EC) and methanol in 61 samples of cachaça. The quantification of BaP was carried out using HPLC with fluorescence detection, EC concentrations was determined by GC/MS and that of methanol, by GC/FID. In all samples, the concentration of methanol remained below 5 mg 100 mL-1 absolute alcohol. The results of BaP varied from <0.03 to 0.86 μg L-1; the values of EC exceeded the limit established by Brazilian legislation (150 μg L-1) in 53% of the samples.