Quantitative analysis of phenol and alkylphenols in Brazilian coal tar

The main purpose of this work is the identification and quantification of phenolic compounds in coal tar samples from a ceramics factory in Cocal (SC), Brazil. The samples were subjected to preparative scale liquid chromatography, using Amberlyst A-27TM ion-exchange resin as stationary phase. The fractions obtained were classified as "acids" and "BN" (bases and neutrals). The identification and quantification of phenols, in the acid fraction, was made by gas chromatography coupled to mass spectrometry (GC/MS). Nearly twenty-five phenols were identified in the samples and nine of them were also quantified. The results showed that coal tar has large quantities of phenolic compounds of industrial interest.

Otimização dos parâmetros de extração para determinação multiresíduo de pesticidas em amostras de água empregando microextração em fase sólida

In this study the factors that affect the extraction of pesticide residues from water samples for their determination by solid-phase micro-extraction (SPME) and GC/MS were optimized. The fiber polymer, the extraction mode, the ionic strength, the stirring rate, the pH and the extraction time were the most significant parameters evaluated. The recovery obtained with the proposed method ranged from 94 to 110% and the sensitivity of the method, determined by calculating the detection limit (DL), ranged from 0.004 to 0.1 mug l-1. The results obtained with spiked real samples, at the 0.1 mug l-1 level, showed acceptable conformity with the expected values.

Aplicação da técnica de dispersão da matriz em fase sólida (DMFS) na análise de pesticidas em quiabo por CG-EM

A matrix solid phase dispersion and gas chromatography-mass selective detection method for the simultaneous determination of monocrotophos, methyl parathion, cypermethrin and deltamethrin in okra is described. Analyses of 2 g of fortified okra (0.05-0.75 mg kg-1) showed an average recovery of 96.2% (71.4-128.4%) and average relative standard deviation of 11.7% (1.4-37.1%). The cypermethrin recovery at the lower level was above 130%. The limit of detection ranged from 0.02 to 0.15 mg kg-1. The procedure was applied to the okra samples and has found 0.56 mg kg-1 of cypermethrin-cis, 0.75 mg kg-1 of cypermethrin-trans and 2.71 mg kg-1 of deltamethrin.

Óleos voláteis de espécies de Myrcia nativas do Rio Grande do Sul

Essential oils from M. richardiana, M. arborescens, M. selloi, M. oligantha, M. rostrata, M. lajeana, M. obtecta, M. pubipetala and M. hatschbachii were obtained by hydrodistillation and analyzed by GC and GC/MS. Sixty-seven compounds have been identified ranging from 90-99% of the oil contents. All analyzed species were rich in cyclic sesquiterpenes (66-99%), mainly those from the cadinane, caryophyllane and germacrane cyclization pathway, among them b-caryophyllene, germacrene D, bicyclogermacrene, d-cadinene, spathulenol, caryophyllene oxide, globulol and a-cadinol. The acyclic sesquiterpene series was well represented by M. lajeana (32.1%), with 25,3% of (E)-nerolidyl acetate.

Constituintes químicos voláteis e não-voláteis de Cochlospermum vitifolium (Willdenow) Sprengel

The essential oils from leaves, root bark and root wood of Cochlospermum vitifolium were investigated for the first time. The oils were obtained by hydrodistillation and analyzed by GC/MS. The main volatile constituents were beta-caryophyllene (8.2 - 46.5%), beta-bisabolene (11.5 - 29.3%), gamma-muurolene (28.4%), alpha-humulene (26.0%), 1-hydroxy-3-hexadecanone (16.2 - 19.5%) and beta-pinene (10.6%). Phytochemical analysis of the root bark and root wood extracts yielded excelsin, pinoresinol, narigenin, aromadendrin, galic acid and a triacylbenzene, along with beta-sitosterol and stigmasterol and their D-glucosides. The structures of all compounds were determined by analyses of the spectroscopic data (NMR and MS), and comparison with the literature.

Sesquiterpenos do caule de Pilocarpus riedelianus e atividades sobre microorganismos

Pilocarpus riedelianus was studied in order to obtain compounds with activity against fungi and bacteria. The dichloromethane extract, the most active one, was chromatographed yielding hexane and dichloromethane fractions. Six known sesquiterpenes, alpha-calacorene, beta-calacorene, gamma-calacorene, cadalene, sesquichamaenol and 1-hydroxy-1,3,5-bisabolatrien-10-one were identified in the hexane fractions. The identification of these compound was done by NMR and GC/MS analyses. The hexane fraction from the dichloromethane extract showed activity against several fungi and bacteria.

Caracterização química do "pitch" em indústria de celulose e papel de Eucalyptus

The chemical analysis of the acetone, chloroform, toluene and methanol extracts of a pitch sample was carried out by IR and GC-MS, leading to the identification of sixty nine compounds, including fatty acids, alcohols and hydrocarbons. Analysis of the acetone extractive of a eucalyptus wood used in Brazil for pulp production was also carried out, resulting in identification of fifty nine compounds, including mainly fatty acids, phenolic compounds, beta-sitosterol and other steroids. This analysis showed that pitch formation had a contribution from wood extractives and other sources of contamination. The results obtained and the methodology applied can be used by the pulp industry to develop new methods of pitch control.

Composition and antifungal activity of essential oils from Piper aduncum, Piper arboreum and Piper tuberculatum

The composition of essential oils from leaves, stems and fruits of Piper aduncum, P. arboreum and P. tuberculatum was examined by means of GC-MS and antifungal assay. There was a predominance of monoterpenes in P. aduncum and P. tuberculatum and of sesquiterpenes in P. arboreum. P. aduncum showed the richest essential oil composition, including linalool. The essential oils from fruits of P. aduncum and P. tuberculatum showed the highest antifungal activity with the MIC of 10 µg as determined against Cladosporium cladosporioides and C. sphaerospermum, respectively. This is the first report of the composition of essential oils from P. tuberculatum.

Determinação de hidrocarbonetos voláteis e semi-voláteis na atmosfera

This paper focuses: (i) the development of a measurement technique for the determination of atmospheric C2-C6 hydrocarbons with sampling in canisters and analysis by gas chromatography/flame ionisation detector (GC/FID), (ii) the improvement of an existent adsorption-sampling technique with Tenax TA tubes for the determination of C6-C11 hydrocarbons and analysis by GC/FID after thermal desorption and cryogenic concentration, (iii) the identification of compounds present in ambient air by gas chromatography/mass spectrometry (GC/MS) for both canister and Tenax samples, (iv) a program of interlaboratorial comparison for quality control of C2-C11 analyses, and (v) the seasonal characterisation of ambient air C2-C11 hydrocarbons.

Método multirresíduo para monitoramento de contaminação ambiental de pesticidas na região de Bauru (SP) usando mel como bio-indicador

The presence of residues of the major groups of pesticides (organohalogen, organophosphorous, pyrethroids and organonitrogen) in representative samples of honey produced in Bauru (state of São Paulo, Brazil) was investigated from 1999 through2004. A multiresidue method was applied to honey samples to determine 48 pesticides with recoveries ranging from 76 to 95%. The limits of detection found were lower than 10 µg/kg for GC-MS-SIM. The results indicated that most pesticides found in the samples belonged to the organohalogen and organonitrogen groups. Residues of malathion were detected in almost all of the samples in high concentration.

Óleo essencial de Gochnatia polymorpha (Less) Cabr. ssp floccosa Cabr.

The essential oil isolated by hydrodistillation from flowers and root bark of Gochnatia polymorpha (Less) Cabr. ssp floccosa Cabr. (Asteraceae) was analyzed by capillary GC/MS. Thirty components were identified in oil of flowers. The composition depends on the stage of flowering. At the beginning of flowering, the main components were (E)-nerolidol (20,4%) and eugenol (17,9%) whereas at the end they were phenylacetaldehyde (14,6%) and tricosane (12,0%). In the essential oil of root bark ten sesquiterpenes were identified. The major components were beta-bisabolene (31,0%) and beta-bisabolol (21,5%). This paper describes for the first time the composition of essential oil in the genus Gochnatia.

Variação química do óleo essencial de Hyptis suaveolens (L.) Poit., sob condições de cultivo

This study was performed to establish the correlation between the growth conditions and essential oil composition of Hyptis suaveolens from Alfenas (MG), Brazil. The plants were grown in a greenhouse, four treatments were used and they were harvested at two different periods of time (60 and 135-day-old plants). The essential oil composition was determined by GC-MS analysis. The terpenes spathulenol, globulol, dehydroabietol, a-cadinol and beta-phellandrene were the major constituents found in the essential oil. Oxygenated sesquiterpenes represented the main group of constituents in most of the treatments. The major changes in the essential oil composition were found in 135-day-old plants grown under NPK deficiency. We also identified three groups of volatile components that have not been previously described in H suaveolens.

Influência da temperatura do ar de secagem sobre o teor e a composição química do óleo essencial de Lippia alba (Mill) N. E. Brown

Leaves of Lippia alba were submitted to six different drying treatments, using air at ambient temperature and heated up to 80 °C. The essential oil was extracted by steam distillation and analyzed by GC-MS. For the dried leaves, the oil content was reduced by 12 to 17% when compared with the fresh plant (0.66%). The major oil component was citral, representing 76% for the fresh plant, and varying from 82 to 84% for the dried material. These results showed that L. alba can be submitted to a drying process of up to 80 ºC without degradation and/or loss of the major, [LC1] active component.

Estudo de recuperação de glifosato e AMPA derivados em solo utilizando-se resinas nacionais

In the present paper we studied the recoveries of glyphosate, N-(phosphonomethyl)glycine (GLY) and its major metabolite, (aminomethyl)phosphonic acid (AMPA) in soil using national (Brazilian) ion-exchange resins, derivatization by a mixture of trifluoroacetic anhydride and trifluoroethanol and analyses by GC-MS. The quantification limits were 12 ng.g-1 for both compounds and the methodology showed a range of recuperation from 85 to 94% with coefficients of variation (CV) ranging from 4.07 to 6.91% for GLY. For AMPA, the mean recoveries ranged from 87 to 102% with CVs ranging from 5.81 to 6.99%. Additional studies showed that, due to the instability of the derivatized compounds, they must be analysed keeping constant time between derivatization and analysis, preferably less than 24 h.

Atividade acaricida dos óleos essencias de folhas e frutos de Xylopia sericea sobre o ácaro rajado (Tetranychus urticae Koch)

The essential oils of the leaves and fruits obtained by hydrodistillation of Xylopia sericea, collected in the restinga area of Pernambuco, were analyzed by GC (HP 5890 SERIES II) and GC/MS (HP 5890B SERIES II/ MSD 5971). A major part of the volatile components identified in the oils of fruits and leaves were monoterpenes and sesquiterpenes. Cubenol (57.43%) and alpha-epi-muurolol (26.09%) were the main compounds found in the leaves, whereas beta-pinene (45.59%) and alpha-pinene (17.18%) were the fruits major components. The acaricidal activity of the essential oils was evaluated for Tetranychus urticae. The oil of the leaves was more active than that of the fruits showing an LC50 value of 4.08 µL/L of air for a 72 h period.