Influência do horário de colheita sobre o rendimento e composição do óleo essencial de erva-cidreira brasileira [Lippia alba (Mill.) N. E. Br.]

Este trabalho teve como objetivo verificar se o horário de colheita da erva-cidreira brasileira [Lippia alba (Mill.) N. E. Br.], fenotipo carvona-limoneno, tem influência sobre a produção de massa foliar, rendimento e composição do óleo essencial. Foram avaliados cinco horários de colheita quando a cultura estava com 145 dias desde o transplante: 8:00, 10:00, 12:00, 14:00 e 16:00 h com cinco repetições, distribuídos em blocos casualizados. O experimento foi conduzido na Fazenda Experimental Lageado da FCA-UNESP/Botucatu no Setor de Horticultura do Departamento de Produção Vegetal. A colheita foi realizada a 15 cm da superfície do solo e o óleo essencial obtido através de hidrodestilação, em aparelho tipo Clevenger. Levou-se em consideração os fatores agronômicos e o rendimento obtido por hidrodestilação. O óleo essencial foi analisado em cromatógrafo gasoso acoplado a espectrômetro de massas (CG/EM). Os resultados foram submetidos à análise de variância (Teste F) e as médias comparadas pelo teste de Tukey. Não houve diferença estatística para produção de massa foliar, teor de óleo essencial e produtividade de óleo essencial em massa fresca e seca. No entanto, entre os compostos majoritários do óleo essencial das folhas, carvona e limoneno, a melhor produtividade de carvona foi obtida às 10:00 h, em matéria fresca (2,050 L ha-1) e em matéria seca (2,068 L ha-1), e para o limoneno às 16:00 h, em matéria fresca (1,068 L ha-1) e em matéria seca (1,060 L ha-1).

Emprego de nebulizador pneumático de ICP-MS como câmara de diluição em sistemas de injeção em fluxo para determinações multielementares

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Metabolite fingerprint of "capim dourado" (Syngonanthus nitens), a basis of Brazilian handcrafts

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Essential oil of Lithraea molleoides (Vell.): chemical composition and antimicrobial activity

Lithraea molleoides(Vell.) (Anacardiaceae) é uma árvore encontrada no Brasil, Paraguai, Bolívia, Uruguai, Argentina e Chile. É popularmente usada na forma de extrato alcoólico, decocção e infusão para o tratamento de tosse, bronquite, artrite, doenças do sistema digestivo, como diurético, tranqüilizante, hemostático e tônico. O objetivo do presente estudo foi a extração do óleo essencial dos frutos maduros, folhas e outras partes aéreas da planta e o rendimento do mesmo; a identificação e quantificação dos principais componentes e a determinação da atividade antimicrobiana. O rendimento do óleo essencial dos frutos maduros foi de 1%, entretanto, não foi encontrado óleo essencial nas partes aéreas da planta. A análise do óleo essencial por cromatografia gasosa com espectrometria de massa, mostrou a presença de limoneno (89,89%), alfa-pineno (3,48%), beta-pineno (2,63%), alfa-terpineol (1.27%), mirceno (0,64%), sabineno (0,54%), 4-terpineol (0,28%), canfeno (0,22%) e delta-3-careno (0,13%). O óleo essencial foi ativo contra algumas bactérias Gram positivas e leveduras testadas e não apresentou atividade contra bactérias Gram negativas.

Composição química e produtividade dos principais componentes do óleo essencial de Baccharis dracunculifolia DC. em função da adubação orgânica

Objetivou-se avaliar a composição química e produtividade dos principais componentes do óleo essencial de Baccharis dracunculifolia DC. em função de doses de composto orgânico (0, 10, 20, 30, 40 e 50 t ha-1). Foi realizada uma colheita, aos 150 dias após o transplante das mudas. O óleo essencial, da massa seca útil da parte aérea, foi extraído por hidrodestilação e analisado em cromatógrafo a gás acoplado a espectrômetro de massas (Shimadzu, QP-5000). A identificação dos constituintes químicos foi realizada através da análise comparativa dos espectros de massas das substâncias com o banco de dados do sistema CG-EM (Nist 62.lib), literatura e índice de retenção. Os resultados foram submetidos à análise de variância pelo teste F, às médias obtidas foram submetidas à análise de regressão e o teste Tukey para o efeito das doses de composto orgânico. Os três componentes sesquiterpênicos, E-nerolidol, espatulenol e óxido de cariofileno, perfazem 58,44% da média relativa da composição química do óleo essencial de B. dracunculifolia, composto pela presença de 28 substâncias. Na produtividade dos componentes γ-muroleno, valenceno, δ-cadineno e E-nerolidol as dosagens estudadas influenciaram as plantas, que na dosagem 30 t ha-1 obtiveram os melhores resultados. Se o objetivo no cultivo de B. dracunculifolia for o componente espatulenol as dosagens 30 e 40 t ha-1 obtiveram os melhores resultados. Para a produtividade do componente óxido de cariofileno as dosagens estudadas influenciaram as plantas, que na dosagem 40 t ha-1 obtiveram os melhores resultados.

Conteúdo de peptídeos e avaliação morfofisiológica dos espermatozóides do epidídimo e ejaculado de bovinos

Objetivou-se com este estudo a identificação de alguns fatores protéicos envolvidos na qualidade funcional dos espermatozóides epididimais (SPZEP) e ejaculados (SPZEJ) de bovinos. Foram avaliadas as características morfofisiológicas e analisado o conteúdo peptídico destas estruturas de 11 animais mestiços Nelore, de 24 a 30 meses de idade. As avaliações morfofisiológicas foram motilidade progressiva (MOT, %), vigor, patologias espermáticas, integridade acrossômica e da cromatina. Foi observado que, os SPZEJ, na média, apresentaram MOT maior do que os SPZEP, 72,3 e 46,4%, respectivamente. Considerando as patologias espermáticas, taxas de defeitos maiores (DEFMAI), menores (DEFMEN) e totais (DEFTOT), houve diferença significativa entre as taxas dos DEFMEN e DEFTOT dos SPZEP e SPZEJ, sendo, em média, 91,1 e 8,5% e 95,4 e 11,8%, respectivamente. As taxas dos DEFMEN e DEFTOT dos SPZEP foram maiores em função da presença de espermatozóides com gotas citoplasmáticas distais. A análise das protéinas dos SPZEP e SPZEJ foi realizada por espectrometria de massa, método MALDI-TOF (matrix -assisted laser desorption/ionization - time of flight), e revelou presença de peptídeos de massa molecular variando de 1,1 a 26,3 kDa nos SPZEJ e de 1,1 a 11,6 kDa nos SPZEP. Foram identificados peptídeos de 10,6 e 13,4 kDa somente nos SPZEJ e de 6,8 kDa somente nos SPZEP. Foi observada relação do peptídeo de massa molecular de 7,4 kDa dos SPZEP e de 4,7 kDa dos SPZEJ, com a MOT Ê 80%, destas estruturas. Os resultados sugerem o envolvimento destes peptídeos nos processos funcionais das células espermáticas do epidídimo e ejaculado. O estudo utilizou o método MALDI/TOF para espectrômetro de massa, para identificar peptídeos em espermatozóides do epidídimo de bovinos, pela primeira vez no País.

Kinetic evaluation of the pyrolysis of high density polyethylene over H-AlMCM-41 material

The AlMCM-41 material with Si/Al=50 was synthesized by hydrothermal method, using cethyltrimethylammonium as template. The protonic H-AlMCM-41 acid form was obtained by ion exchange with ammonium chloride solution and subsequent calcination. The characterization of the material by several techniques showed that a good-quality MCM-41 material was obtained. High-density polyethylene (HDPE) has been submitted to thermal degradation alone, and in presence of the exchanged H-AlMCM-41 catalyst at a concentration of 1: 1 in mass (H-AlMCM-41/HDPE). The reactor was connected on line to a gas chromatograph connected to a mass spectrometer. This process was evaluated by thermogravimetry (TG), from 350 to 600degreesC, under helium dynamic atmosphere, with heating rates of 5.0; 10.0 and 20.0 degreesC/min. From TG curves, the activation energy, calculated using a multiple heating rate integral kinetic method, decreased from 225.5 KJ.mol(-1), for the pure polymer (HDPE), to 184.7 KJ.mol(-1), in the presence of the catalyst (H-AlMCM-41/HDPE).

Analysis of camphorquinone in composite resins as a function of shade

Objective. To identify and quantify the camphorquinone (CQ) used in different brands of composite resins as a function of the shade analyzed.Materials and methods. Filtek Z250 A3 (FZA3), Filtek Z-250 Incisal (FZI), Pyramid Enamel A1 (PEA1), Pyramid Enamel Translucent (PET), Filtek Supreme A3E (FSA3) and Filtek Supreme GT (FSGT) were used. Five hundred milligrams of each resin were weighed and then dissolved in 1.0 ml of methanol. The samples were centrifuged to accelerate the sedimentation of the inorganic particles. 0.8 ml of the supernatant solution was collected with a pipette and assessed under gas chromatography coupled to the mass spectrometer (GC-MS). The results were compared to pure CQ solutions, used as a standard. Student's t-test, (p = 0.05) significant at the level of 5%, compared the results of each brand shade.Results. A smaller amount of camphorquinone was found in Filtek Z-250 (FZI) resin incisal shade when compared to (FZA3) A3 shade. on the other hand, Filtek Supreme resin featured a statistically larger camphorquinone amount in the incisal shade. in Pyramid Enamel resin camphorquinone was found only in shade Al, while the photoinitiator used in the Translucent shade was not identified.Significance. Based on the data obtained, it is possible to conclude that a single composite resin brand may feature differences in amount and type of photoinitiator used. (C) 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Fast chromatographic determination of polycyclic aromatic hydrocarbons in aerosol samples from sugar cane burning

Sugar cane burning in Brazil causes remarkable amounts of organic compounds to be emitted amongst which the polycyclic aromatic hydrocarbons (PAHs) represent serious health hazards. Therefore, 24-h aerosol samples (< 10 mum aerodynamic diameter) were collected in Araraquara city (São Paulo state) during the harvest season using a Hi-Vol sampler. PAHs were recovered using an Accelerated Solvent Extractor and analyzed by low-pressure gas chromatography-ion trap mass spectrometry (LP-GC-IT-MS). The fully automated extraction process was performed in less than 25 min with a solvent consumption of approximately 20 ml. The use of a deactivated 0.6 m x 0. 10 mm i.d. restrictor coupled to a 10 m wide-bore analytical column allowed most of the 16 PAHs in EPA's priority list to be identified and quantified in only 13 min. Concentrations of PAHs in Nraraquara aerosols ranged between 0.5 and 8.6 ng m(-3). (C) 2003 Elsevier B.V. All rights reserved.

Kinetic parameters of polymer degradation by SAPO-37

High density poly(ethylene) has been submitted to thermal degradation alone, and in the presence of silicoaluminophosphate SAPO-37. The processes were carried out in a reactor connected on line to a gas chromatograph/mass spectrometer in order to analyze the evolved products. Polymer degradation was also evaluated by thermogravimetry, from room temperature until 800 degreesC, under nitrogen dynamic atmosphere, with multiple heating rates. From TG curves, the activation energy related to degradation process was calculated using the Flynn and Wall multiple heating rate kinetic model for pure polymer (PE) and for polymer in the presence of catalyst (PE/S37). SAPO-37 showed good selectivity for low molecular mass hydrocarbons in PE catalytic degradation.

Evaluation of uranium incorporation from contaminated areas using teeth as bioindicators - a case study

The Southwest region of the Bahia state in Brazil hosts the largest uranium reserve of the country (100 kton in uranium, only), plus the cities of Caetite, Lagoa Real and Igapora. In this work, aim was at the investigation of uranium burdens on residents of these cities by using teeth as bioindicators, as a contribution for possible radiation protection measures. Thus, a total of 41 human teeth were collected, plus 50 from an allegedly uranium free area (the control region). Concentrations of uranium in teeth from residents of 5- to 87-y old were determined by means of a high-resolution inductively coupled plasma mass spectrometer (ICP-MS). The highest uranium concentration in teeth was measured from samples belonging to residents of Caetite (median equal to 16 ppb). Assuming that the uranium concentrations in teeth and bones are similar within 10-20% (for children and young adults), it concluded that uranium body levels in residents of Caetite are at least one order of magnitude higher than the worldwide average. This finding led to conclude that daily ingestion of uranium, from food and water, is equally high.

Study of environmental burden of lead in children using teeth as bioindicator

The south region of São Paulo city hosts the Guarapiranga dam, responsible for water supply to 25% of the city population. Their surroundings have been subject to intense and irregular occupation by people from very low socioeconomics classes. Measurements undertaken on sediment and particulate materials in the dam revealed concentrations of lead. copper, zinc and cadmium above internationally accepted limits. Epidemiological and toxicological studies undertaken by the World Health Organization in individuals exhibiting lead concentrations in blood, near or below the maximum recommended (10 mu g dl(-1)), surprisingly revealed that toxic effects are more intense in individuals belonging to low socioeconomics classes. Motivated by these facts, we aimed at the investigation of chronic incorporation of lead. as well as the use of our BIOKINETICS code, which is based on an accepted ICRP biokinetics model for lead, in order to extrapolate the results from teeth to other organs. The focus of our data taking was children from poor families, living in a small, restrict and allegedly contaminated area in São Paulo city. Thus, a total of 74 human teeth were collected. The average concentration of lead in teeth of children 5 to 10 years old was determined by means of a high-resolution inductively coupled plasma mass spectrometer (ICP-MS). For standardization of the measurements, an animal bone certified material (H-Animal Bone), from the International Atomic Energy Agency, was analyzed. The amount of lead in children living in the surroundings of the dam, was approximately 40% higher than those from the control region, and the average lead concentration was equal to 1.3 mu g g(-1) approximately. Grouping the results in terms of gender, tooth type and condition, it was concluded that a carious molar of boys is a much more efficient contamination pathway for lead, resulting in concentrations 70% higher than in the control region. We also inferred the average concentrations of lead in other organs of these children, by making use of our BIOKINETIC code. (C) 2008 Elsevier Ltd. All rights reserved.

Photodesorption and electron trapping in n-type SnO2 thin films grown by dip-coating technique

Thin films of undoped and Sb-doped (2 atg%) SnO2 have been prepared by sol-gel dip-coating technique on borosilicate glasses. Variation of photoconductivity excitation with wavelength and optical absorption indicate indirect bandgap transition with energy of ≅ 3.5 eV. Conductance as function of temperature indicates two levels of capture with 39 and 81 meV as activation energies, which may be related to an Sb donor and oxygen vacancy respectively. Electron trapping by these levels are practically destroyed by UV photoexcitation (305 nm) and heating in vacuum to 200°C. Gas analysis using a mass spectrometer indicates an oxygen related level, which may not be desorbed in the simpler O2 form.

Composição fitoquímica dos óleos essenciais de folhas de Lippia alba (Mill.)N.E.Br. em diferentes épocas de colheita e partes do ramo

This work aimed to determine the best harvest time for biomass production, yield and essential oil composition considering the seasonal variation (spring, summer, autumn and winter) on different plant parts (apical, medial and basal). Essential oils were extracted by hydro-distillation with a Clevenger apparatus for both fresh and dry mass obtained in field and lab conditions respectively. The extracted essential oils were analyzed by GS/MS (Shimadzu, QP-5000). The chemical components were identified by comparing their mass spectrum to the patterns filed in the MS computer memory (Wiley,139,Lib.), to the literature references, and by co-injection with authentic standards. Applying phyto-chemical tests on fresh and dry mass, the chemical component percentages of essential oils were calculated and identified as follows: citral (neral and geranial), myrcene, caryophylene and elemene.

Composition of coriander essential oil from Brazil

Coriander (Coriandrum sativum L.) is an annual and herbaceous plant, belonging to the Apiaceae family. Native of southern Europe and western Mediterranean region, this herb is cultivated world widely. This species, rich in linalool, has potential using as source of essential oil and as a medicinal plant. It has been used as analgesic, carminative, digestive, depurative, anti-rheumatic and antispasmodic agent. Its fruits (commonly called seeds) are used for flavoring candies, in cookery, perfumery, beverage and in tobacco industry. The aim of this study was to analyze the chemical composition of the seed essential oil of this species grown in Botucatu, São Paulo, Brazil. The experiment was carried out in Lageado Experimental Farm, Department of Plant Production, Agronomical Sciences College, São Paulo State University. The fruits were harvest 108 days after sowing. The essential oils were extracted by hydro distillation, in Clevenger apparatus. 50 g of fruits were used in each extraction. Three extractions were performed during three hours. The essential oils were analyzed in Gas Chromatography Mass Spectrometer (CG-MS, Shimadzu, QP-5000), equipped with DB-5 capillary column (30 m × 0,25 mm × 0,25 mm), split 1/20, injector for 240 C°, detector for 230 C°, dragged by gas He (1,7 mL/min), with programmed temperature for 40 C° (5 min)-150 C°, 4 C°/min; 150 C°-280 C°, 8 C°/min. The identification of the compounds was made by comparison of their spectra of masses with data from CG-MS (Nist 62 lib), literature references and retention index of Kovats. The 18 most important components were identified and quantified. The main components of the oil were linalool (77.48 %), γ-terpinene (4.64 %), α-pinene (3.97 %), limonene (1.28 %), geraniol (0.64 %) and 2-decenal (0.16 %).