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101.
Carvalho PN Rodrigues PN Alves F Evangelista R Basto MC Vasconcelos MT 《Talanta》2008,76(5):1124-1129
Determination of organochlorine pesticides (OCPs) in sediments implicates extraction of these compounds from the matrix, which is difficult owing to strong interaction among OCPs and different constituents of the sediments, particularly organic content. The method here described is a combination of microwave assisted extraction (MAE), headspace solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS), acting in selected-ion storage mode, or GC-electron capture detector (ECD, for routine analysis). Methanol was used as extracting solvent and aliquots of the MAE extracts (after inclusion of a step for sulfur elimination when required) were used to prepare aqueous solutions for HS-SPME. A complete automation of the SPME procedure increases the sample throughput, including standard addition for calibration purpose. The procedure has the advantage of exclude additional clean-up steps and pre-concentration before SPME. Application to reference sediments of different characteristics revealed absence of significant interferences from the matrix for alpha-lindane, gamma-lindane, aldrin, dieldrin, endrin, 4,4'-DDT, 4,4'-DDD, 4,4'-DDE, heptachlor, heptachlor epoxide and good sensitivity. Detection limits ranged from 0.005 to 0.11 ng of OCP per gram of dried sediment using GC-MS and from 0.01 to 0.26 ngg(-1) using GC-ECD. The linear response ranges embraced 5-6 orders of magnitude (up to 1000 ngg(-1)) in GC-MS, being narrower for GC-ECD. The method was successfully applied to sandy and muddy sediments from Portuguese rivers estuaries, enabling quantification of seven OCPs. The method resulted effective, relatively simple and fast, being suitable for routine monitoring of residues of OCPs from sediments of different grain size and organic matter content, which influence concentration, mobility and availability of contaminants. 相似文献
102.
Mauro Vaccaro Gaetano Mangiapia Antonella Accardo Diego Tesauro Eliana Gianolio Henrich Frielinghaus Giancarlo Morelli Luigi Paduano 《Colloid and polymer science》2008,286(14-15):1643-1652
Two novel amphiphilic unimers containing an aliphatic hydrophobic chain (PDA) with two C≡C triple bonds and hydrophilic heads presenting the chelating agent DTPAGlu and the CCK8 bioactive peptide, respectively, have been prepared by solid phase synthesis. Aggregates obtained by mixing together PDA-DTPAGlu, or its Gd(III) complex, and PDA-L2-CCK8 in 70/30 molar ratio before and after a polymerization process carried out by UV irradiation have been structurally characterized by means of small angle neutron scattering. The relaxivity properties of aggregates containing Gadolinium complexes have also been investigated. Elongated mixed micelles have been observed, in which the relaxivity value r 1p for each Gadolinium complex, measured at 20 MHz and 298 K, is around 12 mM–1 s–1. 相似文献
103.
Rafael M. de Almeida Victoria C. Ferrari Dr. Juliana dos S. Souza Dr. Flavio L. Souza Wendel A. Alves 《Chemphyschem》2020,21(6):476-483
Herein, a detailed investigation of the surface modification of a zinc oxide (ZnO) nanorod electrode with FeOOH nanoparticles dispersed in glycine was conducted to improve the water oxidation reaction assisted by sunlight. The results were systematically analysed in terms of the general parameters (light absorption, charge separation, and surface for catalysis) that govern the photocurrent density response of metal oxide as photoanode in a photoelectrochemical (PEC) cell. ZnO electrodes surface were modified with different concentration of FeOOH nanoparticles using the spin-coating deposition method, and it was found that 6-layer deposition of glycine-FeOOH nanoparticles is the optimum condition. The glycine plays an important role decreasing the agglomeration of FeOOH nanoparticles over the ZnO electrode surface and increasing the overall performance. Comparing bare ZnO electrodes with the ones modified with glycine-FeOOH nanoparticles an enhanced photocurrent density can be observed from 0.27 to 0.57 mA/cm2 at 1.23 VRHE under sunlight irradiation. The impedance spectroscopy data aid us to conclude that the higher photocurrent density is an effect associated with more efficient surface for chemical reaction instead of electronic improvement. Nevertheless, the charge separation efficiency remains low for this system. The present discovery shows that the combination of glycine-FeOOH nanoparticle is suitable and environmentally-friend cocatalyst to enhance the ZnO nanorod electrode activity for the oxygen evolution reaction assisted by sunlight irradiation. 相似文献
104.
Tiago Augusto Donegatti Alnilan Lobato Eliana A. R. Duek Luís Moreira Gonçalves Elisabete Alves Pereira 《Electrophoresis》2020,41(18-19):1576-1583
Aminoglycosides are a relevant class of antibiotics widely used by medics and veterinaries. There are a variety of reasons that make their determination relevant, such as quality control, environment and food contamination assessment, drug-release studies, among others. The lack of a chromophore makes aminoglycoside spectrophotometric detection particularly challenging, often requiring derivatization. In this work, an indirect detection method, making use of imidazole as a probe, applying CZE was successfully tested. It did not require derivatization, which simplified the sample preparation. Suitable figures of merit were obtained; recoveries between 95 and 105%, adequate repeatability and precision, correlation coefficients (r) above 0.998, and limits of detection (LODs) of 3.2 and 11 mg/L for gentamicin and paromomycin, respectively. As a proof-of-concept, it was also applied in a simple controlled release experiment that was well fitted using the Hill equation. 相似文献
105.
Catarina Serafim Maria Elaine Araruna Edvaldo Alves Júnior Margareth Diniz Cllia Hiruma-Lima Lenia Batista 《Molecules (Basel, Switzerland)》2020,25(22)
Peptic ulcers are characterized by erosions on the mucosa of the gastrointestinal tract that may reach the muscle layer. Their etiology is multifactorial and occurs when the balance between offensive and protective factors of the mucosa is disturbed. Peptic ulcers represent a global health problem, affecting millions of people worldwide and showing high rates of recurrence. Helicobacter pylori infection and the use of non-steroidal anti-inflammatory drugs (NSAIDs) are one of the most important predisposing factors for the development of peptic ulcers. Therefore, new approaches to complementary treatments are needed to prevent the development of ulcers and their recurrence. Natural products such as medicinal plants and their isolated compounds have been widely used in experimental models of peptic ulcers. Flavonoids are among the molecules of greatest interest in biological assays due to their anti-inflammatory and antioxidant properties. The present study is a literature review of flavonoids that have been reported to show peptic ulcer activity in experimental models. Studies published from January 2010 to January 2020 were selected from reference databases. This review refers to a collection of flavonoids with antiulcer activity in vivo and in vitro models. 相似文献
106.
A chromotropic acid-functionalized polyurethane foam has been developed for use in an on-line preconcentration system for cobalt and nickel determination. The packing material was prepared by covalent coupling of chromotropic acid with the polyurethane foam through an azo group. Co and Ni ions were sorbed in the mini-column, from which they could be eluted directly to the nebulizer-burner system of a flame atomic absorption spectrometer. Elution of cobalt and nickel from the mini-column can be accomplished with 0.50 and 0.75 M HCl solutions, respectively. The enrichment factors obtained were 22 (Co) and 27 (Ni), for 60 s preconcentration time, and 57 (Co) and 59 (Ni), if a preconcentration time of 180 s was used. Under the optimum conditions, the proposed procedure allowed the determination of metals with detection limits of 0.43 (cobalt) and 0.52 microg/L (nickel), respectively, on using preconcentration periods of 180 s. The accuracy of the developed procedure was evaluated by analysis of the certified reference materials NIST 1515 Apple Leaves and NIST 1570a Spinach Leaves. The method was applied to the analysis of lettuce samples. The contents of cobalt in the samples analyzed varied from 0.75 to 0.98 microg/g. Nickel was not detected in the lettuce samples. 相似文献
107.
Alves Lourdes A. Felipe Maria G. A. Silva JoÃo B. Almeida E. Silva Silvio S. Prata Arnaldo M. R. 《Applied biochemistry and biotechnology》1998,70(1):89-98
Applied Biochemistry and Biotechnology - In order to remove or reduce the concentrations of toxic substances present in the sugarcane bagasse hemicellulose hydrolysate for xyloseto-xylitol... 相似文献
108.
Sofia Nikolaou Sérgio Hiroshi Toma Vagner Roberto de Souza Juliano B. Alves Koiti Araki Henrique Eisi Toma 《Transition Metal Chemistry》2011,36(7):775-783
The triruthenium carboxylate cluster [Ru3O(OAc)6(py)2(bpp)]+ (OAc = acetate) containing the bridging 1,3-bis(4-pyridyl)propane (bpp) ligand, and its dimeric species [{Ru3O(OAc)6(py2)}2(μ-bpp)]2+ were synthesized in order to investigate their inclusion compounds with β-cyclodextrin (β-CD). Characterization of the complexes
was carried out based on spectroscopic, electrochemical and spectroelectrochemical techniques, while the formation of inclusion
complexes was evaluated using 1H NMR/NOESY spectroscopy. Since bpp is a flexible ligand, a DFT study was carried out in order to characterize its conformational
isomers and their possible role in the host–guest chemistry with β-CD. Instead of observing the formation of inclusion compounds
with different stoichiometries, we observed the formation of 1:1 bpp/β-CD compounds in which the bpp ligand assumes different
conformations. The assembly of polymetallic rotaxane species was successfully demonstrated by monitoring the 1H NMR spectra of the monomeric cluster species in the presence of aquapentacyanoferrate(II) ions and β-CD. 相似文献
109.
Solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME) was applied for the extraction of six organophosphorous pesticides (OPPs) in water samples. The analytes considered in this study were determined by gas chromatography with mass spectrometry and included prophos, diazinon, chlorpyrifos methyl, methyl parathion, fenchlorphos and chlorpyrifos. Several extraction conditions (extraction solvent and elution/dispersion solvents nature, extraction solvent volume, elution solvent volume, water volume and sample volume) were tested for SPE-DLLME with these analytes and the best results were obtained using carbon tetrachloride as the extraction solvent and acetone as the elution/dispersion solvent. Calibration curves for the determination of OPPs in water samples were constructed in the concentration range of 10-100 ng/L. Limits of detection (LODs) ranged from 38 to 230 pg/L values that are below the maximum admissible level for drinking water (100 ng/L). Relative standard deviations (RSD) were between 8.6 and 10.4% for a fortification level of 100 ng/L. At the same fortification level, the relative recoveries (R.R.) of tap, well and irrigation water samples were in the range of 30.2-97.1%. 相似文献
110.
Leonardo M. PereiraWagner A. Alves 《Vibrational Spectroscopy》2011,56(2):250-254
Raman experiments of formamide and zinc chloride solutions in a wide concentration range (0.1-5.0 mol kg−1) have been carried out. The spectral changes were interpreted on three different ways: (i) the rupture of the H-bonds of FA was evidenced by the trend observed in the νCO, δHNH and restricted (translation or libration) modes; (ii) the appearance of a new band in the νCN region (∼1338 cm−1) was assigned to FA coordinated to Zn (II) through nitrogen atom; (iii) the electronic delocalization in the FA structure upon complexation provided the appearance of new features in the δCH and νCH regions. The quantitative treatment performed at the νCN region of FA allowed the determination of an average number of 3 FA molecules per Zn (II) in the first solvation shell. This value is supported by the appearance of features assigned to ZnCl+ and ZnCl2 entities that also occupy vertices of the tetrahedron at higher salt concentrations. The present study may be useful for a better understanding on electrochemical processes employed in the production of dendritic zinc films as well as FA hydrolysis catalyzed by this metal. 相似文献