Identificação de componentes de óleos voláteis: Análise espectroscópica de misturas de sesquiterpenos

This paper describes a chromatographic method to fractionate volatile oils and to identify their sesquiterpenic constituents. The fractionation process includes flash chromatography over silica gel and chromatography over silica gel/AgNO3, utilising pentane, CH2Cl2 and/or acetone as eluents. GC chromatograms were obtained in order to get the relative percentage of each constituent in the volatile oils, to get the retention time value of them as well as to analyse and combine the fractions eluted from the columns. Such procedure afford mixtures of sesquiterpenes which are analysed by GC/MS, 13C and ¹H NMR.

Redução seletiva aplicada à especiação de mercúrio em peixes: uma adaptação do método de Magos

In the selective reduction procedure proposed by Magos SnCl2 was used as reductant for inorganic mercury while total mercury was determined after reduction with a mixture of SnCl2 and CdCl2. The difference between total mercury and inorganic mercury determines the content of organic mercury. The procedure of the present work differs of Magos in that the mercury vapour is carried to the absorption cell after magnetic stirring of the solution in the reaction flask; in the Magos procedure, mercury vapour is carried by bubbling the gas in to the solution. In contrast to the Magos procedure this slight modification overcame the necessity of at calibration by analyte addition, saving time and gainning accuracy.

Extrações de óleos de sementes de citros e suas atividades sobre a formiga cortadeira Atta sexdens e seu fungo simbionte

Seeds Citrus oils (C. sinensis, C. limon and C. reticulata) extraction with hexane in a soxhlet apparatus and through supercritical fluid (CO2) were done. Besides triglycerides, the oils obtained with hexane comprised volatile compounds such as terpenes and fatty alcohols, esters, and aldehydes. However, the oils obtained by extraction with supercritical fluid presented only triglycerides. These results indicate that the extraction using supercritical fluid presents better selectivity. The activity of the oils on the development of the ant symbiotic fungus, Leucoagaricus gongylophorus, showed week activity and the topic insecticide assay showed better activity for the tangerine seed oil.

Modificação de óleos e gorduras por biotransformação

The oleochemical industry has a permanent interested in controlling the physical, functional and organoleptical properties of their products and in producing useful derivatives from their raw materials. The potential of biotechnology for developing novel or well-known products at more competitive costs meets the need of this industrial segment in expanding their goals. In this work some technical aspects, problems and perspectives related to the production of oil and fat derivatives using biotransformation techniques are discussed. Particular emphasis is given to the description of biotransformation processes using lipase as catalyst, in view of the great versatility of this enzyme class to mediate typical reactions in this technological sector.

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.

Alterações físico-químicas dos óleos de girassol, milho e soja em frituras

The aim of this study is to determine the influence of frying time on the alterations of sunflower, corn and soybean oils during deep fat frying of potato chips. The analytical methods used to evaluate the oil alterations are: free fatty acids, peroxide value, refractive index and total polar compounds. An increase of free fatty acids, refractive index and total polar compounds with frying time were observed. The different behaviors observed for the three vegetables oils can be explained by the differences in the initial composition and quality of them.

Titulação potenciométrica aplicada na determinação de ácidos graxos livres de óleos e gorduras comestíveis

Free fatty acids are a measure of evaluating fats and oils, submitted to abusive conditions, besides being a quality characteristic of edible vegetable oils. The official method of determination (AOCS Ca 5a-40, 2004) is based on titration, using phenolphthalein as an indicator. For crude and degummed oils, the titration end point is difficult to be observed due to the high level of pigments, resulting in dark solutions. In this case and others, such as self-life studies, in which sample quantities are limited, potentiometric titration may be a very good alternative.

Atividade antioxidante de óleos essenciais de espécies de Croton do nordeste do Brasil

Three Croton species, C. zenhtneri, C. nepetaefolius and C. argyrophylloides, were collected at two different times, 6:00 and 13:00 h, their essential oils were extracted by steam distillation and analyzed by gas Chromatography / Mass Spectrometry. The percentage yield of oil constituents changes along the day. The oils were submitted to the antioxidant test thiobarbituric acid reactive species, using BHT and a-tocoferol as the reference compounds. All oils exhibited good antioxidant activities. In general, C. zenhtneri and C. argyrophylloides essential oils showed higher antioxidant activity than C. nepetaefolius.

O emprego da termogravimetria para determinar a energia de ativação do processo de combustão de óleos combustíveis

Activation energy (Ea) is a parameter that can be applied to make predictions about the quality of oils to be used in an ICO engine. In this study, Ea was determined by thermogravimetry following two different procedures: ASTM E 1641 and Model-free kinetics. The energies were calculated in the low temperature oxidation (LTO) region for three Brazilian fuel oils (denominated A, B and C) and the results were equal using both methods: 43 kJ mol-1 (alpha=0.1 to 0.9) for oil A, 48 kJ mol-1 (alpha=0.1 to 0.5) and 65 kJ mol-1 (alpha=0.5 to 0.9) for oil B, and 58 kJ mol-1 (alpha=0.1 to 0.5) and 65 kJ mol-1 (alpha=0.5 to 0.9) for oil C. It was concluded that, among the oils studied, sample A was potentially the best option concerning the behavior in the LTO region.

Determinação de contaminantes em óleos lubrificantes usados e em esgotos contaminados por esses lubrificantes

A simple and reliable ashing procedure is proposed for the preparation of used lubricating oil samples for the determination of Zn, Fe, Pb, Ni and Cu by the flame atomic absorption spectrometry technique. Sulphanilic acid was added to oil samples, the mixture coked and the coke ashed at 550 ºC. The solutions of the ash were analysed by flame AAS for these metals. The quantification limits were 38.250 µg g-1 for Zn, 4.550 µg g-1 for Fe, 1.562 µg g-1 for Pb, 1.450 µg g-1 for Ni, and 0.439 µg g-1 for Cu. The determinations, in lubricating oil, showed good precision and accuracy with recoveries between 90 and 110 %, indicating a negligible matrix effect in the experiments using addition of analyte, with relative standard deviation lower than 5%. The results for analysis of wastewater contamined by theses lubricants showed a very high relative standard deviation.

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.

Transesterificação de óleos vegetais: caracterização por cromatografia em camada delgada e densidade

We studied the transesterification of two vegetable oils: soybean and waste frying oil. The main problem of transesterification is related to the measurement of the ethyl ester content. In this work we used a quick analytical method for assessing the ethyl ester fraction of the purified fuel-grade transesterification products by applying a simple correlation with density. If the ester content is higher than 85% by weight the correlation allows the determination by a single density measurement. This method is suitable for control and determines the ethyl ester quickly and simply.

Composição química dos óleos essenciais das folhas de seis espécies do gênero Baccharis de "Campos de Altitude" da mata atlântica paulista

The essential oils from the leaves of six species of the Baccharis genus (B. dracunculifolia, B. microdonta, B. regnelli, B. schultzii, B. trimera, and B. uncinella), collected in the "Campos de Altitude" of the Atlantic Forest (SP), were extracted using hydrodistillation procedures and analyzed by GC and GC/MS. There was a predominance of sesquiterpenes in all studied oils as b-elemene in B. dracunculifolia and B. regnelli, a-humulene in B. trimera, g-gurjunene in B. schultzii, bicyclogermacrene in B. regnelli, d-cadinene in B. regnelli and B. uncinella, spathulenol in B. schultzii, caryophyllene oxide in B. microdonta and guaiol in B. uncinella. However, a high amount of monoterpenes was also observed in B. uncinella (a-pinene), B. regnelli (d-car-3-ene) and B. schultzii (limonene). The chemical compounds of the essential oils of B. schultzii, B. regnelli and B. microdonta are described for the first time in this work.

Perfil de ácidos graxos e avaliação da alteração em óleos de fritura

The present study had the purpose of evaluating the profile of fatty acids and the total alteration of cottonseed, sunflower and palm oils brought about during discontinued frying processes of cassava frozen chips. An increase in the percentage of saturated fatty acids and a decrease in polyunsaturated fatty acids was observed, regardless of the type of oil used. With regard to the oil's global alteration, the results showed that palm oil, the most saturated one, underwent less alteration. However, none of the oils presented total polar compound values above the limits prescribed.

Quantificação de TBHQ (terc butil hidroquinona) e avaliação da estabilidade oxidativa em óleos de girassol comerciais

Sunflower oil is one of the vegetable oils most susceptible to oxidative reaction. Therefore the presence of natural (tocopherol) and/or synthetic (TBHQ) antioxidants is a prerequisite to secure the stability of this oil during its shelf life, especially with the increased use of PET packaging. On determining the total tocopherol content in 10 samples of deodorized sunflower oils, high losses in total tocopherol during deodorization were identified. In order to facilitate researche involving oxidative stability of vegetable oils, a method for isolated quantification of TBHQ using the isocratic elution system was developed.