961 resultados para CHROMATOGRAPHY-MASS-SPECTROMETRY
Resumo:
Propolis and plant secretions from three species, most frequently mentioned as botanical sources of the bee glue in Brazil (Baccharis dracunculifolia, Araucaria angustifolia and Eucalyptus citriodora) have been investigated using GC-MS. Based on chemical evidence, B. dracunculifolia was shown to be the main propolis source in Sao Paulo state. The antibacterial and antifungal activities of all four materials were also tested, the most active being propolis and Baccharis leaf exudate.
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Chemical analyses of complete larvae of the first to third instar and cuticle, fat body and salivary glands extracts of fourth instar larvae using gas chromatography and gas chromatography-mass spectrometry, were performed upon Pachycondyla villosa. The results revealed that P. villosa larvae do not produce a pheromone, as only fatty acids and n-alkanes were detected. After quantifying the identified compounds, it was determined that the fat body is the main place of storage and/or production of the cuticular hydrocarbons. It was also observed that the absolute quantity of cuticular hydrocarbons increases progressively during larval development. Inferences about the transport behavior of matured larvae to the pupation place and the colony odor are discussed.
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Termites have become an important pest of Eucalyptus and Pinus reforestations, sugarcane and other cultures. An alternative for the control of this pest would be the use of attractive traps that take in account the social behavior of these insects. Diverse factors are important for the insects in the localization of the habitat and the choice of the food and specific odors can facilitate this. Studies referring to Heterotermes tenuis (Isoptera: Rhinotermitidae) are scarce. The objective of this work was to analyze the tergal cuticular extract of H. tenuis and determine the selectivity and sensitivity of its antennae to the components of this extract by electroantennography (EAG). The composition of the cuticular extract was determined by GC-MS analysis. The hydrocarbons found were restricted to linear alkanes, being most abundant C24 to C27 that comprises ca. 65% of the total. Olefins were not detected. EAG and behavioral test responses to the cuticular hydrocarbons were greater and significantly different from the control and the high selectivity of the antennae to the extract indicates its potential as chemical messenger. Cuticular hydrocarbons mixture is species-specific and can be used to identify a given taxon without the diagnostic castes, soldiers or imagoes. Difference in the composition appears to relate with the type of habitat of specie.
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The mandibular gland secretions of newly emerged, nurse and forager workers, virgin and physogastric queens and males of Melipona bicolor were analyzed by gas chromatography-mass spectrometry. The secretion is composed of a blend of hydrocarbons, alcohols, esters, and acids. The secretion is caste-sex specific and also differs with the tasks performed by the workers and the physiological reproductive condition of the queens.
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The family Verbenaceae comprises about 175 genera and 2300 species, distributed in tropics and subtropics, mainly in temperate zone of southern hemisphere. The lemon verbena (Aloysia triphylla (L'Herit) Britton) is a perennial, bushy plant originally from South America. The essential oil of this plant is used in pharmaceutical, cosmetic and perfumery industry. Therapeutic properties include febrifuge, sedative, stomachical, diuretic, and antispasmodic activities. The present work aimed to identify the chemical composition of essential oil of Aloysia triphylla leaves. The study was done in Lageado Experimental Farm of the Department of Plant Production-Horticulture, Agronomical Sciences College, São Paulo State University Campus of Botucatu. Leaves of lemon verbena from Medicinal and Aromatic Plant Garden, were collected in the end of winter (September/2001). The essential oil was extracted by hydrodistillation, in Clevenger apparatus. 100 g of leaves were used in each extraction. Four extractions were performed during three hours. The essential oils of the leaves were analyzed in Gas Chromatography Mass spectrometry (CG-MS, Shimadzu, QP-5000), equipped with capillary column DB-5 (30 m × 0,25 mm × 0,25 mm), split 1/35, injector for 220 C°, detector for 230 C°, dragged by gas He (1,0 mL/min), with programmed temperature for 60 C° to 240 C°, 3 C°/min. The identification of the substances was held by comparison of their mass spectra with data of the CG-MS (Nist 62 lib), literature references and retention index of Kovats. The main constituents of essential oils were geranial (29.54 %), neral (27.01 %), limonene (15.93 %), geranyl acetate (4.0 %) and geraniol (3.96 %). This species possesses high quantity of monoterpenes and low quantity of sesquiterpenes.
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The hybrid Mentha pulegium x spicata, also well-known as poejo de praia, it is a perennial, low plant, with fields, violet stem and opposite leaves, with lance format and sawed board, presenting characteristic smell. The objective of the present work was accomplish a study of the leaf anatomy, including a biometric study of tissue and quantitative analysis of secretory trichomes/mm2 and of stomata/mm2 in both faces of the epidermis, besides a chemical analysis of the essential oil. Histological permanent laminas were made for anatomical analysis of the leaf surface and also sheets of the impression to foliate for the count of the trichomes number and stomatas. The chemical studies were made through the extraction of the essential oil by hydrodistillation and analyzed in GC-MS. The capitate and peltates trichomes are present on both sides of the leaf, even so they prevail in the abaxial surface. The variance analysis show that there are significant differences for the number of capitate trichomes and tectores between the adaxial and abaxial surfaces, but they are not significant for the peltate trichoma. The analyzed of essential oil shows the presence of a majority component, trans piperitone epoxide, being it responsible for more than 80% of the relative composition in the essential oil.
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The aim of this paper was to apply a multiresidue method using Supercritical Fluid Extraction (SFE) and capillary gas chromatography with electron capture and mass spectrometry detections in the analysis of the levels of pesticide residues in fruits and vegetables. Single laboratory validation of both solid-liquid and supercritical fluid extraction methods was carried out for 32 compounds selected from four pesticide classes (organochlorine, organonitrogen, organophosphorus and pyretroid) in blank and fortified samples of fresh lettuce, potato, apple and tomato. Recoveries for the majority of pesticides from fortified samples at fortification level of 0.04-0.10 mg kg -1 ranged 74-96% for both methods and confirmation of pesticide identity was performed by gas-chromatography-mass spectrometry in a selected-ion monitoring mode. Both methods showed good limits of detection (less 0.01 mg kg-1, depending on the pesticide and matrix) and the SFE method minimized environmental concerns, time, and laboratory work. ©2005 Sociedade Brasileira de Química.
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A rapid and reliable method for the determination of 25 compounds selected from four classes of pesticides in samples of fresh apples, grapes, pears, and strawberries purchased at a local supermarket, is presented. The study describes two different methods of extraction: solid-liquid extraction with acetone and supercritical fluid extraction. Clean-up was based on aminopropyl cartridge extraction followed by gas chromatography with an electron capture detector for simultaneous determinations. Confirmatory analysis was carried out by gas chromatography with mass spectrometry in the selected-ion monitoring (SIM) mode. Extraction efficiencies were directly compared and the methods were applied to the analysis of real samples. Recoveries for a majority of pesticides from standard samples at enrichment levels of 0.04-0.10 mg/ kg ranged from 77 to 96 % for both methods. The supercritical fluid extraction method showed good limits of detection (less than 0.01 mg/kg, depending on the pesticide and matrix) as well as minimizing environmental concerns, time, and laboratory effort. © 2006 Centro de Información Tecnológica.
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Migration of components from plastic packaging into foodstuffs or into medicines is a very important issue, concerning public health. Using experimental techniques, like gas chromatography-mass spectrometry, these essays measure total migration and specific migration of components from plastic packaging. This work presents an explanation and applications of a numerical technique tool for this measurement, allowing the comprehension of the diffusion process and the estimate of component migration in difficult or impractical measurements. As an application example, the non-uniform influence of initial concentration profile on the migration is presented, demonstrating the necessity of this profile determination for high quality considerations on involved metrology.
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In this study, the antiulcerogenic effect of essential oil from Baccharis dracunculifolia was evaluated using the model of acute gastric lesions induced by ethanol. The ulcerative lesion index (ULI) was significantly reduced by oral administration of the essential oil of B. dracunculifolia at doses of 50, 250 and 500 mg/kg which reduced the lesions by 42.79, 45.70 and 61.61%, respectively. The analysis of the chemical composition of the essential oil from B. dracunculifolia by GC showed that this was composed mainly of mono- and sesquiterpenes and the majority compound was nerolidol. Therefore, antiulcerogenic activity of nerolidol (50, 250 and 500 mg/kg) was investigated using ethanol-, indomethacin- and stress-induced ulcer models in rat. In the stress-induced ulcer model, a significant reduction of the ULI in animals treated with nerolidol (50, 250 and 500 mg/kg) and cimetidine (100 mg/kg) was observed, compared to the control group (p < 0.05). The percentage of inhibition of ulcer was 41.22, 51.31, 56.57 and 53.50% in groups treated with 50, 250, 500 mg/kg of nerolidol and 100 mg/kg of cimetidine (positive control), respectively. Regarding ethanol- and indomethacin-induced ulcer models, it was observed that the treatment with nerolidol (250 and 500 mg/kg) significantly reduced the ULI in comparison with the control group (p < 0.05). The dose of 50 mg/kg reduced the parameters analyzed but this was not statistically significant. In the ethanol-induced model percentage of inhibition of ulcer was 34.20, 52.63, 87.63 and 50.87% in groups treated with 50, 250, 500 mg/kg of nerolidol and 30 mg/kg of omeprazol (positive control), respectively. In indomethacin-ulcer the percentage of inhibition of ulcer was 34.69, 40.80, 51.02 and 46.93% in groups treated with 50, 250, 500 mg/kg of nerolidol and 100 mg/kg of cimetidine (positive control), respectively. The results of this study show that nerolidol displays antiulcer activity, as it significantly inhibited the formation of ulcers induced in different animal models. However, further pharmacological and toxicological investigations, to delineate the mechanism(s) of action and the toxic effects, are required to allow the use of nerolidol for the treatment of gastric ulcer. © 2007 Verlag der Zeitschrift für Naturforschung.
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Persistent organic pollutants (POPs), organochlorine pesticides and polychlorinated biphenyls (PCBs), listed as per the Stockholm Convention (α -HCH, β -HCH, γ -HCH, p,p′-DDT, o,p′-DDT, p,p′-DDD, p,p′-DDE, aldrin, endrin, dieldrin, PCBs 28, 52, 118, 138, 153, and 180), were analyzed in municipal solid waste (MSW) compost samples from three different Brazilian composting plants located in three São Paulo State cities: Araras, Araraquara and São Paulo (Vila Leopoldinha). Quantitative and qualitative analyses were carried out using gas chromatography electron capture detection (GC-ECD) and gas chromatography mass spectrometry (GC-MS) (Ion Trap, electron impact ionization), respectively. The samples were analyzed in triplicate and the target POPs were not detected by GC-ECD. Twelve pollutants were identified in two samples when qualitative analysis (GC-MS) was used (β -HCH, γ -HCH, p,p′-DDT, o,p′-DDT, p,p′-DDD, and p,p′-DDE, PCBs 28, 118, 138, 153 and 180). The composting process has advantages such as urban solid waste reduction and landfill life-span increase, however the MSW compost quality, which can be utilized for agricultural purposes, should be evaluated and be controlled. This kind of study is the first step in making available information to answer questions regarding MSW compost for sustainable agricultural use, such as the pollutants accumulation in soil and in groundwater, and plants uptake. Copyright © Taylor & Francis Group, LLC.
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This study describes the chemical and physical-chemical profile of plant drug and ethanolic extract obtained from fruits of Solanum lycocarpum A. St.-Hill. (Solanaceae). The physical and chemical analysis involved the granulometry determination, non-compacted apparent density, loss on drying in oven and in infrared scale, pH, ash values and extractive values. The results determined the physical-chemical characteristics of the drug plant. It was also carried out the microbiological control of the plant drug. The preliminary phytochemical screening featured the presence of tannins, flavonoids and saponins in the plant drug and alkaloids and steroids in the ethanolic exctract. The solamargine and solasonine glycoalkaloids were identified through TLC and GC/ MS. The levels of total phenols and tannins were quantified in the extract (8.90% and 6,85% respectively). Such studies contribute to the chemical identification and quality control of S. lycocarpum fruits. © 2010 Phcog.net.
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Background and Purpose: The circadian rhythm of melatonin in saliva or plasma, or of the melatonin metabolite 6-sulfatoxymelatonin (a6MTs) in urine, is a defining feature of suprachiasmatic nucleus (SCN) function, the body's endogenous oscillatory pacemaker. The primary objective of this review is to ascertain the clinical benefits and limitations of current methodologies employed for detection and quantification of melatonin in biological fluids and tissues. Data Identification: A search of the English-language literature (Medline) and a systematic review of published articles were carried out. Study Selection: Articles that specified both the methodology for quantifying melatonin and indicated the clinical purpose were chosen for inclusion in the review. Data Extraction: The authors critically evaluated the methodological issues associated with various tools and techniques (e.g. standards, protocols, and procedures). Results of Data Synthesis: Melatonin measurements are useful for evaluating problems related to the onset or offset of sleep and for assessing phase delays or advances of rhythms in entrained individuals. They have also become an important tool for psychiatric diagnosis, their use being recommended for phase typing in patients suffering from sleep and mood disorders. Additionally, there has been a continuous interest in the use of melatonin as a marker for neoplasms of the pineal region. Melatonin decreases such as found with aging are or post pinealectomy can cause alterations in the sleep/wake cycle. The development of sensitive and selective methods for the precise detection of melatonin in tissues and fluids has increasingly been shown to have direct relevance for clinical decision making. Conclusions: Due to melatonin's low concentration, as well as the coexistence of numerous other compounds in the blood, the routine determination of melatonin has been an analytical challenge. The available evidence indicates however that these challenges can be overcome and consequently that evaluation of melatonin's presence and activity can be an accessible and useful tool for clinical diagnosis. © Springer-Verlag 2010.
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Objective-To determine the pharmacokinetics of dexmedetomidine administered as a short-duration IV infusion in isoflurane-anesthetized cats. Animals-6 healthy adult domestic female cats. Procedures-Dexmedetomidine hydrochloride was injected IV (10 μg/kg over 5 minutes [rate, 2 μg/kg/min]) in isoflurane-anesthetized cats. Blood samples were obtained immediately prior to and at 1, 2, 5, 6, 7, 10, 15, 30, 60, 90, 120, 240, and 480 minutes following the start of the IV infusion. Collected blood samples were transferred to tubes containing EDTA, immediately placed on ice, and then centrifuged at 3,901 X g for 10 minutes at 4°C. The plasma was harvested and stored at -20°C until analyzed. Plasma dexmedetomidine concentrations were determined by means of liquid chromatography-mass spectrometry. Dexmedetomidine plasma concentration-time data were fitted to compartmental models. Results-A 2-compartment model with input in and elimination from the central compartment best described the disposition of dexmedetomidine administered via short-duration IV infusion in isoflurane-anesthetized cats. Weighted mean ± SEM apparent volume of distribution of the central compartment and apparent volume of distribution at steady-state were 402 ± 47 mL/kg and 1,701 ± 200 mL/kg, respectively; clearance and terminal half-life (harmonic mean ± jackknife pseudo-SD) were 6.3 ± 2.8 mL/min/kg and 198 ± 75 minutes, respectively. The area under the plasma concentration curve and maximal plasma concentration were 1,061 ± 292 min·ng/mL and 17.6 ± 1.8 ng/mL, respectively. Conclusions and Clinical Relevance-Disposition of dexmedetomidine administered via short-duration IV infusion in isoflurane-anesthetized cats was characterized by a moderate clearance and a long terminal half-life.