Fullerene Separation And Identification By Traveling Wave Ion Mobility Mass Spectrometry In Laser Desorption Processes During Asphaltene Analysis

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Sample preparation focusing on plant proteomics: extraction, evaluation and identification of proteins from sunflower seeds

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)In the present work 17 different procedures for extraction of proteins from sunflower (Helianthus annuus L.) seeds in natura were evaluated regarding extraction time and temperature, type of solvent, and analytical procedure. After each extraction procedure, total protein was determined, ranging from 260 +/- 5 to 2727 +/- 11 mu g g(-1). Then, a 2-D PAGE was used for P4, P5, P13 and P17, which were considered the most efficient extraction protocols, to calculate the match between them. The highest (77 +/- 3%) and the lowest (48 +/- 1%) values were achieved when P13 mu P17 and P4 mu P17 protocols were compared, respectively. Additionally, the P4 and P5 protocols presented the highest number of spots (196 +/- 11 and 194 +/- 20) after 2-D PAGE protein separation. From both protocols (P4 and P5), 66 protein spots were visualized in both extraction protocols and also analyzed by the 2-D PAGE technique for verifying possible changes in protein expression. Thirty-six spots were differentially found at 90% (or 1.8 times) and related to their relative volume and/or intensity. From these protein spots, 24 (ca. 67%) were successfully identified, 17 being proteins from sunflower seeds. The others are homologous proteins from other plant organisms. All of these analyses contributed to choosing the protocol P4 as the best for protein extraction from sunflower seeds.51116123Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES

Antioxidant, antimicrobial activities and characterization of phenolic compounds from buriti (Mauritia flexuosa L. f.) by UPLC-ESI-MS/MS

Mauritia flexuosa L. f. is a native palm tree from the South American Amazon rainforest commercialized in food, cosmetics and medicine. This paper reported the antioxidant, antimicrobial activities and characterization of phenolics from buriti leafs, trunk and fruit extracts. The total phenolics of the buriti extracts ranged from 378.07 +/- 3.12 to 86.89 +/- 3.15 mg GAEq/100 g and flavonoid content ranged from 567.16 +/- 1.15 to 246.84 +/- 1.11 mg QUEREq/100 g. The antioxidant activity assays with EC50, of 12.28 +/- 0.022 to 19.58 +/- 0.064 mg/mL revealed the antioxidant capacity of M. flexuosa extracts. Results of the antimicrobial tests against some pathogenic bacteria revealed its strong ability to inhibit the growth of pathogen with low MIC values, where the best results were found with the leaf extract against the pathogen Pseudomonas aeruginosa (MIC 50 mu g/mL). The characterization of the phenolic compounds using Ultra Performance Liquid Chromatography coupled to Electrospray Ionization Tandem Mass Spectrometry (UPLC-ESI-MS/MS) was based on CID experiments of the observed precursors, thus 13 compounds were tentatively identified ((+)-catechin, caffeic acid hexoside, chlorogenic acid, quercetin, narigenin, myricetin, vitexin, scoparin, rutin, cyanidin-3-rutinoside, cyanidin-3-glucoside, (-)-epicatechin and kaempferol). These results indicate that antioxidant and antimicrobial activities in buriti phenolic extracts are quite potent and implicate the presence of compounds with potent free-radical-scavenging activity. (C) 2013 Elsevier Ltd. All rights reserved.51246747

Phytochemical Study of the Alkaloidal Fractions of Unonopsis duckei R. E. Fr. Guided by Electrospray Ionisation Ion-trap Tandem Mass Spectrometry

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)IntroductionThe Unonopsis genus is a promising source of aporphinoid alkaloids, substances with great biological potential. These alkaloids have a well-defined mass spectrometry fragmentation pattern that, together with previous phytochemical knowledge, can guide the isolation of alkaloids not yet described for the genus. ObjectiveIsolate substances not yet described in the Unonopsis genus, guided by alkaloidal profile analyses of stem barks, twigs and leaves of Unonopsis duckei using electrospray ionisation ion-trap tandem mass spectrometry (ESI-IT/MSn). MethodsMethanolic extracts from stem barks, twigs and leaves were submitted to a liquid-liquid, acid-base partitioning treatment to obtain the alkaloidal fractions. These fractions were analysed by direct infusion into an ESI-IT/MSn system. The major alkaloids observed for each fraction were submitted to fragmentation analysis. ResultsThe MS fragmentation patterns revealed the presence of alkaloids previously reported for Annonaceae, including nornuciferine, anonaine, asimilobine, liriodenine and lysicamine, known for the Unonopsis genus, as well as others that were not yet described for this genus. In this way, the proaporphine alkaloid glaziovine was isolated, as well as a mixture of the aporphine alkaloids glaucine and norglaucine, all described for the first time in the Unonopsis genus. ConclusionMass spectrometry monitoring was fundamental to prioritise the isolation of substances not yet identified for the Unonopsis genus, dismissing known compounds and simplifying the phytochemical study. Copyright (c) 2013 John Wiley & Sons, Ltd. The MS monitoring of the alkaloidal fractions of the Unonopsis duckei was fundamental to prioritise the isolation of substances not yet identified for the Unonopsis genus, dismissing known compounds and simplifying the phytochemical study. The presence of alkaloids previously reported for Annonaceae family, nornuciferine (3), anonaine (4), asimilobine (5), lysicamine (6) and liriodenine (7) was detected. The proaporphine alkaloid glaziovine (1) and the aporphine alkaloids glaucine (2a) and norglaucine (2b) are described for the first time in the Unonopsis genus.2514549Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)FINEPFAPEAMCoordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq

Mauritic acid: a new dammarane triterpene from the roots of Mauritia flexuosa L.f. (Arecaceae)

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)A new dammarane triterpene named mauritic acid (1) was isolated from the roots of Mauritia flexuosa L.f. The complete structural assignment of this new compound was elucidated from spectroscopic methods. Moreover, this compound was evaluated for its cytotoxicity against human cancer cell lines (OVCAR-8, PCM3, NCIH358M and different leukaemia cell strains). The mauritic acid presented significant cytotoxicity against OVCAR-8, PCM3 and NCIH358M cell lines with IC50 3.02, 2.39 and 6.19M, respectively. The triterpenes 1 and 2 were also tested for their antimicrobial activity against 15 strains of microorganisms, including fungi and bacteria, with the best minimal inhibitory concentration values ranging from 50.8 to 203.5M.272221182125Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Fundacao de Amparo a Pesquisa do Estado do Amazonas (FAPEAM)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP