101 resultados para High resolution gas chromatography - mass spectrometry


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Este trabalho teve como objetivo identificar e quantificar os constituintes dos óleos essenciais de Illicum verum, Ageratum conyzoides, Piper hispidinervum e Ocotea odorifera, bem como avaliar a toxicidade para o pulgão-verde Schizaphis graminum. A qualificação dos constituintes foi realizada por meio de um cromatógrafo gasoso + espectrômetro de massas, e a quantificação, por um cromatógrafo gasoso + detector de ionização de chama, ambos com uma coluna DB5. O método de hidrodestilação promoveu um rendimento (p/p) de 3,81% para I. verum, 0,46% para A. conyzoides, 2,85% para P. hispidinervum e 0,68% para O. odorífera. Já os componentes majoritários foram: precoceno (87,0%) e (E)-cariofileno (7,1%) para A. conyzoides; (E)-anetol (90,4%), limoneno (2,6%) e metil-chavicol (1,3%) para I. verum; metil-eugenol (81,2%) e safrol (10,6%) para Ocotea odorífera; e safrol (82,5%) e α-terpinoleno (13,4%) para P. hispidinervum. Pelos testes de toxicidade aguda (24 horas) com folhas de sorgo ou papel-filtro contaminados, verificou-se que o óleo de A. conyzoides foi o mais tóxico para o pulgão, com CL50 de 7,13 e 7,08 µL óleo/cm2 respectivamente, seguido por O. odorifera com CL50 de 11,80 e 103,00 µL óleo/cm2 respectivamente; I. verum de 51,80 µL óleo/cm2 em ambos os substratos; e o menos tóxico foi o óleo essencial de P. hispidinervum, com CL50 de 62,50 e 143,00 µL óleo/cm2, respectivamente. Dessa maneira, sugere-se que o uso dos óleos essenciais pode representar uma nova ferramenta em programas de manejo integrado de pragas.

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Os sanitizantes químicos tradicionais utilizados na indústria de alimentos apresentam, como desvantagem, o possível desenvolvimento de resistência e adaptação bacteriana, interferindo na eficiência bactericida mínima destes produtos. Os óleos essenciais com atividade antimicrobiana despertam grande interesse na indústria de alimentos, pela possível utilização como princípios ativos de sanitizantes. Esta pesquisa objetivou determinar a concentração inibitória mínima (CIM) dos óleos essenciais (OEs) de cravo-da-índia e canela contra bactérias Gram positivas (Staphylococcus aureus e Listeriamono cytogenes) e Gram negativas (Escherichia coli e Salmonella sp.) e compará-la com a CIM do hipoclorito de sódio, além de determinar a concentração bactericida mínima (CBM) dos OEs para L. monocytogenes. Foi utilizado o método da microdiluição e os OEs foram caracterizados, quimicamente, por cromatografia gasosa - espectrometria de massa. Os componentes principais dos OEs de canela e cravo-da-índia foram o cinamaldeído (67,58%) e o eugenol (77,58%), respectivamente. A CIM do OE de canela foi de 0,04%, para as bactérias Gram positivas, e < 0,02%, para a bactérias Gram negativas. O OE de cravo-da-índia teve CIM de 0,04% para Salmonella sp., 0,06% para E. coli e S. aureus e 0,08% para L. monocytogenes. Para todas as bactérias testadas, a CIM do hipoclorito de sódio foi > 0,2%. A CBM para L. monocytogenes, no OE de cravo-da-índia, foi de 0,18% e o OE de canela destacou-se por apresentar CBM < 0,02%, demonstrando a possibilidade do uso destes OEs, principalmente o de canela, como princípios ativos de sanitizantes.

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The present study aimed to evaluate the volatiles profile of red mombin (Spondias purpurea) pulp and its powder produced by spray-drying (SD) as an example to show utility of headspace solid-phase microextraction (HS-SPME) in the analysis of parameters such as the quality and stability of fruit products. Volatiles profiles of the pulp were identified by gas chromatography-mass spectrometry (GC-MS), quantified by gas chromatography-flame ionization detector (GC-FID) and compared to the profile of the powder stored at 0, 60 and 120 days in plastic (PP) or laminated packages (LP). The results showed that the technique was able to identify 36 compounds in the red mombin pulp, 17 out of which have been described for the first time in this fruit, showing that red mombin fresh pulp appears to be unique in terms of volatiles composition. However, only 24 compounds were detected in the powder. This decrease is highly correlated (r(2) = 0.99), at least for the majority of compounds, to the degree of volatility of compounds. Furthermore, the powder stored in PP or LP showed no statistical differences in the amounts of its components for a period of 120 days of storage. Finally, this work shows how HS-SPME analysis can be a valuable tool to assess the quality and stability of fruit products.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Pós-graduação em Ciência Florestal - FCA

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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The chloroform extract of bark of the tropical tree Qualea parviflora (Vochysiaceae) was fractionated by column chromatography on silica gel, yielding triterpenes (lupeol, lupenone, betulin, epi-betulinic acid and friedelin) and a steroid (β-sitosterol). β-sitosterol, lupenone and lupeol were also identified in Q. grandiflora and Q. multiflora, while friedelin was detected only in Q. Multiflora, by means of gas chromatography-mass spectrometry. The anti-Mycobacterium tuberculosis activity of the chloroform extract and isolated compounds was assayed by MABA and MIC values ranged from 250.0 to 31.2 µg/mL. This study is the first to investigate the chemistry and antitubercular activity of apolar compounds from Qualea species.

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China is an important center of origin for the genus Citrus L. of the family Rutaceae and is rich in wild Citrus species. The taxonomy of Citrus has been a subject of controversy for more than a half century. We propose that the metabolite profiles of Chinese native Citrus species can be used for classification and understanding of the taxonomic relationships within the Citrus germplasm. In this study, triplicate gas chromatography-mass spectrometry (GC-MS) metabolite profiles of 20 Citrus species/varieties were acquired, including 10 native varieties originating in China. R-(+)-limonene, alpha-pinene, sabinene and alpha-terpinene were found to be major characteristic components of the essential oils analyzed in this study, and these compounds contributed greatly to the metabolic classification. The three basic species of the subgenus Eucitrus (Swingle's system), i.e., C. reticulata Blanco, C. medica L. and C. grandis Osb., were clearly differentiated based upon their metabolite profiles using hierarchical cluster analysis (HCA) and partial least square-discriminant analysis (PLS-DA). All the presumed hybrid genotypes, including sweet orange (C. sinensis Osb.), sour orange (C. aurantium L.), lemon (C. limon Burm.f.), rough lemon (C. jambhiri Lush.), rangpur lime (C. limonia Osb.) and grapefruit (C. paradisi Macf.), were grouped closely together with one of their suggested parent species in the HCA-dendrogram and the PLS-DA score plot. These results clearly demonstrated that the metabolite profiles of Citrus species could be utilized for the taxonomic classification of the genus and are complementary to the existing taxonomic evidence, especially for the identification and differentiation of hybrid species.

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Most advanced eusocial bees recruit their nestmates to food resources. Recently, studies in Meliponini species showed that the cephalic salivary (labial) glands (CSGs) are responsible for the production of scent-trail pheromones. Studies on CSGs have shown changes in glandular cell morphology since the worker emerges from brood combs (newly emerged) till forager phase, which may be correlated to changes in the composition of secretion produced. However, no study has been made till now regarding to the composition of CSGs secretion of Scaptotrigona postica and the chemical changes that occur in this secretion according to the worker's life phase or tasks performed. In this study, the chemical profile of CSG secretion in S. postica workers was studied. Glands were taken from specimens newly emerged (NE), working in the brood combs area (CA) and forager (FO) and were analyzed by gas chromatography-mass spectrometry. The results showed that glandular secretion consists of oxygenated compounds of middle volatility (acids, alcohols, aldehydes, ketones, esters and ether), and their quantity varies among the different phases of life, increasing as the individual undergoes from intra- to extra-colonial activities. The NE phase contained the smallest variety and quantity of compounds. Due to the variability of compounds, the CA workers were separated into 3 groups according to the chemical constitution of their secretion. Forager workers showed the largest quantity and variety of chemical compounds. The major compounds in forager gland secretion are 7-hexadecen-1-yl acetate and 5-tetradecen-1-yl acetate. Statistical analysis indicates that the chemical composition of glandular secretion is task-related.

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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An analytical method for the determination of aldicarb, and its two major metabolites, aldicarb sulfoxide and aldicarb sulfone in fruits and vegetables is described. Briefly the method consisted of the use of a methanolic extraction, liquid-liquid extraction followed by solid-phase extraction clean-up. Afterwards, the final extract is analyzed by liquid chromatography-atmospheric pressure chemical ionization mass spectrometry (LC-APCI-MS). The specific fragment ion corresponding to [M-74](+) and the protonated molecular [M+K](+) ion were used for the unequivocal determination of aldicarb and its two major metabolites. The analytical performance of the proposed method and the results achieved were compared with those obtained using the common analytical method involving LC with post-column fluorescence detection (FL). The limits of detection varied between 0.2 and 1.3 ng but under LC-FL were slightly lower than when using LC-APCI-MS. However both methods permitted one to achieve the desired sensitivity for analyzing aldicarb and its metabolites in vegetables. The method developed in this work was applied to the trace determination of aldicarb and its metabolites in crop and orange extracts. (C) 2000 Elsevier B.V. B.V. All rights reserved.