924 resultados para HPLC-UV-PAD
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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In 2001, it was estimated that pesticide used worldwide exceeded 2.27 billion kilograms, over 35%, of which, were herbicides. Brazil is considered one of the leaders in the production of sugarcane and mainly ethanol as fuel. The monoculture of sugarcane requires the usage of a range of pesticides, among these, the herbicides diuron and tebuthiuron. The degradation products most studied (DCA and DCPU) are diuron's, especially for toxicological characteristics of this herbicide that is identified as carcinogen and suspected to be endocrine disruptor in mammals. After optimization of the chromatographic separation using HPLC-UV, the analytical curve was constructed in solvent and subsequently in the matrix (surface water). The extraction method contains the usage of SPE (solid phase extraction) (Strata-X, 200 mg/6 mL), applicating 1L of sample and elution with 5 mL of acetonitrile / methanol (50:50, v/v). Analysis by HPLC/UV was performed in gradient mode, acetonitrile/water (70/30-74/26 by 1 min, 74/26 - 78/22 till 3.2 min, returning to initial conditions and remaining this way until 10 min), 018 column (Phenomenex, 4.6 mm diameter, 250 mm long and 5pm particle size) and detection at 254 nm. Tests F and t were performed to verify the presence of the matrix effect. There was matrix effect to all analytes, ranging from -33% (DCA) and 38% (tebuthiuron). Thereby the method was optimized and validated for analysis of diuron, tebuthiuron, and DCPU DCA in surface water using HPLC/UV. The data obtained show that in order to assure the analytical reliability desired the use of the analytical curves in the matrix for the quantification of these analytes in water is required.
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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A stability-indication high performance liquid chromatographic method has been developed for the determination of norfloxacin in tablet dosage forms. Optimum separation was achieved in less than 7 minutes using Eclipse Plus Zorbax C18 Agilent, 150 mm×4.6 mm i.d., 5 μm particle size column. The analyte was resolved by using a mobile phase 5% acetic acid aqueous solution and methanol (80:20, v/v) at a flow rate 1.0 ml/min on an isocratic high performance liquid chromatographic system at a wavelength of 277 nm. Linearity, system suitability, precision, sensitivity, selectivity, specific, and robustness were established by International Conference Harmonization guidelines. For stress studies the drug was subjected to photolysis, oxidation, acid, alkaline and neutral conditions. The analytical conditions and the solvent developed provided good resolution within a short analysis time and economic advantages. The proposed method not required sophisticated and expensive instrumentation.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Species of Microcystis are the most common bloom-forming cyanobacteria in several countries. Despite extensive studies regarding the production of bioactive cyanopeptides in this genus, there are limited data on isolated strains from Brazil. Three Microcystis sp. strains were isolated from the Salto Grande Reservoir (LTPNA01, 08 and 09) and investigated for the presence of mcy genes, microcystins and other cyanopeptides. Microcystin and microginin production was confirmed in two isolates using high-resolution tandem mass spectrometry after electrospray ionization (ESI-Q-TOF), and the structures of two new microginin congeners were proposed (MG756 Ahda-Val-Leu-Hty-Tyr and MG770 MeAhda-Val-Leu-Hty-Tyr). The biosynthesis profile of the identified cyanopeptides was evaluated at different growth phases via a newly developed HPLC-UV method. Results demonstrated no substantial differences in the production of microcystins and microginins after data normalization to cell quota, suggesting a constitutive biosynthesis. This study represents the first confirmed co-production of microginins and microcystins in Brazilian strains of Microcystis sp. and highlights the potential of Brazilian cyanobacteria as a source of natural compounds with pharmaceutical interest.
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Although the occurrence of glandular trichomes is frequently reported for aerial vegetative organs, many questions still remain opened about the presence of such trichomes in underground systems. Here, we present, for the first time, a comparative study concerning the structure, ultrastructure and chemical aspects of both, the aerial and underground glandular trichomes of two different Chrysolaena species, C obovata and C platensis. Glandular trichomes (GTs) were examined using LM, SEM, and TEM and also analyzed by GC-MS and HPLC coupled to UV/DAD and HR-ESI-MS (HPLC-UV-MS). In both aerial (leaf and bud) and underground (rhizophore) organs, the GTs are multicellular, biseriate and formed by five pairs of cells: a pair of support cells, a pair of basal cells, and three pairs of secreting cells. These secreting cells have, at the beginning of secretory process, abundance of smooth ER. The same classes of secondary metabolites are biosynthesized and stored in both aerial and underground GTs of C platensis and C obovata. These GTs from aerial and underground organs have similar cellular and sub-cellular anatomy, however the belowground trichomes show a higher diversity of compounds when compared to those from the leaves. We also demonstrate by means of HPLC-UV-DAD that the sesquiterpene lactones are located inside the trichomes and that hirsutinolides are not artifacts. (C) 2012 Elsevier GmbH. All rights reserved.