Determinação de benzeno, tolueno, etilbenzeno e xilenos em gasolina comercializada nos postos do estado do Piauí

Automotive gasoline consists of a complex mixture of flammable and volatile hydrocarbons derived from crude oil with carbon numbers within the range of 4-12 and boiling points range of 30-225 ºC. Its composition varies with the kind of crude oil and the type of refinery process that they undergone. Aromatics hydrocarbons, in particular benzene, toluene, ethylbenzene and isomeric xylenes (BTEX) are the toxic group constituents presents. GC-FID was employed to quantify these hydrocarbons in 50 commercial gasoline samples from Piauí state. Statistical analysis techniques, such as PCA and HCA were used to analyze the data. Moreover, several validation parameters were evaluated.

Ácidos ciclopentênicos do óleo da sapucainha (Carpotroche brasiliensis Endl, Flacourtiaceae): o primeiro antileprótico usado no Brasil

The chaoolmugra oil is one of the oldest medicines used for leprosy until the development of sulfas. In Brazil, it is known as sapucainha oil that is obtained from Carpotroche brasilienesis seeds (Flacourtiaceae). Chemical and medicinal studies of sapucainha oil were introduced in Brazil by Peckolt, Cole and Cardoso which showed that major ciclopentenyl fatty acids as chaulmoogric, hydnocarpic and gorlic were responsible for its bactericidal activity. In this work, a method for quantification of sapucainha oil acidic fraction by HRGC was established using methyl n-heptadecanoate as internal standard. The oil chemical stability was investigated by the use of GC-MS, IR, ¹H and 13C NMR and showed that the main degradation products belong to the cyclopentenyl moiety oxidation.

Constituintes químicos voláteis das folhas e galhos de Zanthoxylum syncarpum Tull.

The essential oils of the leaves and twigs from Zanthoxylum syncarpum Tull. were examined by GC/MS and GC-FID. Variation in the oil composition relative to the harvesting time was also described. The major components in the leaves oils were limonene (23.1-47.3%) and myrcene (4.8-10.8%). In the oils of twigs, the main components were ar-curcumene (12.8-18.1%), E-β-farnesene (9.1-9.7%) and β-caryophyllene (9.2-9.3%). This paper describes for the first time the composition of the essential oil of the twigs from Z. syncarpum.

Volatile compounds of Nectandra salicina (lauraceae) from Costa Rica and their cytotoxic activity on cell lines

The chemical composition of the volatiles of Nectandra salicina growing wild in Costa Rica was determined by capillary GC/FID and GC/MS. Thirty-seven and forty-two compounds were identified in the leaf and branch oils respectively corresponding to about 92.6 and 86.2% of the total amount of the oils. The major components of the leaf oil were: atractylone (14.6%), viridiflorene (10.1%), α-pinene (9.4%), β-caryophyllene (7.2%), α-humulene (7.0%), δ-cadinene (6.1%), β-pinene (6.0%) and germacrene D (5.8%). The major components of the branch oil were: atractylone (21.1%), germacrene D (10.7%), viridiflorene (7.9%) and 7-epi-α-selinene (5.0%). When the oils were tested on different cell lines, all the LD50 values were higher than 150 µg/mL, with values very similar for the leaf and branch oils. Low toxicity could be explained by antagonistic effects among the main compounds present in the oils.

Variação sazonal da composição do óleo essencial de Myrcia salzmannii Berg. (Myrtaceae)

This work report the seasonal variation of composition of the volatile oils from leaves and from flowers of Myrcia salzmannii harvested in the sand dunes of Salvador, Bahia, northeastern region of Brazil in the years 2001 and 2003. The oils were analyzed by GC-FID and GC-MS being identified 49 components. Nine essential oil samples of leaves collected on different months and years and one sample of flowers were analyzed. β-Caryophyllene and α-humulene were the only compounds present in all of the samples being the first the majority compound.

Comparação de técnicas de determinação de ésteres em cachaça

An analytical comparison of three different techniques for quantitative profile of esters in cachaça is reported. The Ministério da Agricultura Pecuária e Abastecimento (MAPA) recommends the use of GC/FID or volumetry. Despite being laborious and lacking in chemical speciation, the volumetric technique for total ester content shows to be appropriate, reproducible, and accurate for the analysis of cachaça. However, the GC/FID suggested by MAPA, considering only ethyl acetate, shows inaccuracy, underestimating the total ester content by a median factor of 72%, mainly due to the absence of ethyl lactate analysis. On the other hand, the GC/MS technique that comprises the analysis and speciation of nine esters, including ethyl lactate, proved to be reproducible, simple, fast and accurate for the analysis of total ester content in cachaça. Thus, the total ester content results obtained using GC/FID must be considered with precaution.

Composição química volátil, em diferentes estádios de maturação, de manga 'Tommy Atkins' produzida no Vale do São Francisco

The effect of the maturation stages on the volatile chemical composition of mango fruit cv. Tommy Atkins, cultivated in São Francisco Valley, was investigated using SPME. GC/MS and GC-FID analysis allowed the identification of 32 compounds, consisting mainly of monoterpenes. δ-3-Carene was the major component in all the stages, while α-terpinolene, trans-β-caryophyllene e α-pinene succeded each other as the second most abundant constituent, during the ripening. The aroma of the ripe fruit was characterized by presence of short-chain ethyl esters (C2-C6), whereas the green mango contained the highest concentration of δ-3-carene. Furthermore, some terpenes were detected exclusively at one of the stages.

Determinação de etanol e voláteis relacionados em sangue e fluido oral por microextração em fase sólida em headspace associada à cromatografia gasosa com detector de ionização em chama

The aim of this study was to validate a method for the determination of acethaldehyde, methanol, ethanol, acetone and isopropanol employing solid-phase microextraction associated to gas chromatography with flame ionization detection. The operational conditions of SPME were optimized by response surface analysis. The calibration curves for all compounds were linear with r² > 0.9973. Accuracy (89.1-109.0%), intra-assay precision (1.8-8.5%) and inter-assay precision (2.2-8.2%) were acceptable. The quantification limit was 50 µg/mL. The method was applied to the meaurement of ethanol in blood and oral fluid of a group of volunteers. Oral fluid ethanol concentrations were not directly correlated with blood concentrations.

Comparison of gas chromatographic and gravimetric methods for quantization of total fat and fatty acids in foodstuffs

Different methods to determine total fat (TF) and fatty acids (FA), including trans fatty acids (TFA), in diverse foodstuffs were evaluated, incorporating gravimetric methods and gas chromatography with flame ionization detector (GC/FID), in accordance with a modified AOAC 996.06 method. Concentrations of TF and FA obtained through these different procedures diverged (p< 0.05) and TFA concentrations varied beyond 20 % of the reference values. The modified AOAC 996.06 method satisfied both accuracy and precision, was fast and employed small amounts of low toxicity solvents. Therefore, the results showed that this methodology is viable to be adopted in Brazil for nutritional labeling purposes.

Composição química de óleos essenciais de espécies de Aniba e Licaria e suas atividades antioxidante e antiagregante plaquetária

Leaves and stems from Aniba panurensis (Meisn.) Mez, Aniba rosaeodora Ducke and Licaria martiniana (Mez) Kosterm. were collected in the Reserva Florestal Adolpho Ducke-AM and their essential oils were obtained by hydrodistillation procedures. The oils were analyzed by GC-FID and GC-MS resulting on fifty and six compounds being identified. The major components were linalool in A. rosaeodora, and β-caryophyllene in A. panurensis and L. martiniana. At qualitative assays the oils showed antioxidant and antiplatelet activities, but only weak activities were found at quantitative spectrometric assays.

Hidrólise do óleo de Azadirachta indica em água subcrítica e determinação da composição dos triacilglicerídeos e ácidos graxos por cromatografia gasosa de alta resolução a alta temperatura e cromatografia gasosa de alta resolução acoplada à espectrometria de massas

The development of modern analytical tools plays an important role in quality control. The main purpose of this study was to explore the use of subcritical water as a versatile analytical tool, employed simultaneously as a reagent and solvent, as well as the application of high temperature-high resolution gas chromatography (HT-HRGC) to develop a procedure for the analysis of triacylglycerides and fatty acids in Azadirachta indica A. Juss. (Neem) oil without the need for solvents, chemical reagents, or catalytic agents. The developed method presented satisfactory results and is in agreement with the concepts of Green Analytical Chemistry (GAC).

Estudo da eficiência de degradação de tetracloreto de carbono por plasma térmico e caracterização dos produtos formados

Decomposition of carbon tetrachloride in a DC thermal plasma reactor was investigated in argon atmosphere. The operational parameters such as plasma torch power and argon flow rate versus CCl4 conversion were examined. The CCl4 net degradation was determined by GC-FID, the chlorine produced was quantified by iodometric titration, the solid carbon was characterised by Raman spectroscopy and by BET analysis. The solid carbon collected inside de plasma reactor was submitted to solid/liquid extraction and the desorbed species were identified by GC-MS.

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.

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.

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.