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111.
Damián Pérez-Quintanilla Alfredo Sánchez Isabel del Hierro Mariano Fajardo Isabel Sierra 《Mikrochimica acta》2009,165(3-4):291-298
A mesoporous silica has been chemically modified with 5-mercapto-1-methyltetrazole. The newly synthesized material was characterized by powder X-ray diffraction, N2 adsorption, FT-IR, 13C-NMR spectroscopy and elemental analysis, and used to preconcentrate Pb(II) from aqueous solutions. The effect of several variables on the adsorption capacity (i.e. stirring time, pH, interfering ions, presence of other heavy metals in the medium, etc.) has been studied using batch and column techniques. The adsorption capacity of the material followed the order: Pb(II) >> Cu(II) > Cd(II) >>Mn(II) > Ni(II) > Co(II). In column experiments a pre-concentration factor of 200 was obtained for Pb(II). Spiked tap water, mineral water and river water were used for the preconcentration and determination of Pb(II) by flame atomic absorption spectrometry, and a 101–103% recovery was obtained. The limit of detection and quantification values of the method were found to be 2.22·10?6 mM and 8.20·10?6 mM, respectively. The relative standard deviation for four preconcentration experiments was found to be ≤9% in all cases. 相似文献
112.
Isidro S. Marcos Rosalina F. Moro Isabel Costales Miguel A. Escola Pilar Basabe David Díez Julio G. Urones 《Tetrahedron》2009,65(49):10235-1011
A new cyclisation of 3-(but-3-enyl) indole derivatives that produces policyclic compounds with a hexahydrocarbazole structure is described. In this reaction three stereogenic centres are generated in one step, and this process can be considered as evidence of the biogenetic relationship between anominine and tubingensin A. 相似文献
113.
Carolina Moltó-Puigmartí Ana Isabel Castellote M. Carmen López-Sabater 《Journal of chromatography. A》2009,1216(20):4388-4394
A rapid, highly sensitive and direct Ultra-High-Pressure Liquid Chromatographic method was developed and validated for quantifying δ-, β + γ-, and α-tocopherol in human colostrum and milk. Two reversed-phase chromatographic columns and two detectors (Fluorescence Detector or FD and Photodiode Detector Array or PDA) were used and both methods were independently validated. Two internal standards were selected according to the detector used. Recoveries ranged from 96.71% to 103.55% and the relative standard deviations for the within-day precision were below 6% (PDA) and 3% (FD). Both approaches enabled to achieve low detection limits, on the order of ng (PDA) or pg (FD). Only 300 μL of sample and a chromatographic run of less than 1.6 min were enough to efficiently quantify the isomers in the colostrum and milk of Spanish women. 相似文献
114.
Carla Patrícia Coutinho Isabel Sá-Correia Jo?o Almeida Lopes 《Analytical and bioanalytical chemistry》2009,394(8):2161-2171
A methodology for the discrimination of Burkholderia cepacia complex (Bcc) clinical isolates at the species level and at the ribopattern level using Fourier transform infrared (FTIR)
spectroscopy and chemometrics analysis was assessed in this study. Different Bcc sequential isolates collected at the Santa
Maria Hospital (HSM), in Portugal, from clinically infected cystic fibrosis (CF) patients were previously classified by established
molecular methods at the species level and differentiated at the strain level, based on their ribopatterns. A set of 185 of
these isolates, representing four different Bcc species (Burkholderia cepacia, Burkholderia cenocepacia (recA lineages III-A and III-B), Burkholderia multivorans and Burkholderia stabilis), was analyzed by FTIR and results were processed with chemometric methods. Ten reference strains of these species were used
to test the FTIR method. The discrimination at the species level led to misclassification error rates of 10% and 32% for the
HSM isolates and reference strains, respectively, clearly indicating that the FTIR classification method was unable to generalize
results for the reference strains. Infrared spectra of HSM isolates were further analyzed in terms of the discrimination according
to the ribopattern. Results showed misclassification error rates of 4%, 2%, and 8% for B. cepacia, B. cenocepacia III-A, and B. cenocepacia III-B ribopatterns, respectively. These results demonstrated good FTIR spectroscopy discrimination capacity at the ribopattern
level, for the HSM isolates but showed difficulty at the species level, especially when the reference strains were included.
Remarkably, this methodology was found to discriminate isolates belonging to the same species and ribopattern that were collected
from the same patient during prolonged colonization, opening the door to the identification of chemical modifications resulting
from adaptation strategies to the CF lung stressing environment, in particular to aggressive and prolonged antibiotic therapy.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
115.
Isabel Izquierdo-Barba Edesia Sousa Juan Carlos Doadrio Antonio Luis Doadrio Joaquín Pérez Pariente Africa Martínez Florence Babonneau María Vallet-Regí 《Journal of Sol-Gel Science and Technology》2009,50(3):421-429
Ordered mesoporous materials exhibit potential features to be used as controlled drug delivery systems, including their wide
range of chemical compositions and their outstanding textural and structural properties. Therefore, it is possible to control
the drug release kinetics by tailoring such parameters. In this paper, mesoporous materials such as MCM-48 and SBA-15, which
present different pore sizes (3.7 and 8.8 nm) and structural characteristics (3D-bicontinuous cubic and 2D-hexagonal, respectively)
have been synthesized to evaluate their application as drug delivery system and to determine their influence on release kinetic
of ibuprofen. Moreover, a chemical modification of the SBA-15 mesoporous material with octadecyltrimethoxysilane has also
been performed to study its influence on the release rate of ibuprofen. The structural characteristics (3D cubic and 2D hexagonal
pore system) do not affect the release kinetic profiles of ibuprofen. On the contrary, the pore size affects highly to the
release kinetic profiles from first-order kinetic to zero-order kinetic for MCM-48 and SBA-15, respectively. Moreover, the
importance of surface functionalization was demonstrate through the very fast delivery of ibuprofen from SBA-15 mesoporous
materials functionalized with octadecyl chains. 相似文献
116.
Manuel A.V. Ribeiro da Silva Ana I.M.C. Lobo Ferreira Joana I.T.A. Cabral Ana Filipa L.O.M. Santos Ana Rita G. Moreno Tiago L.P. Galvão Inês M. Rocha Paula M.V. Fernandes Sílvia Q. Salgueiro Vanessa A.F. de Moura Isabel M.S.C. Oliveira Paula C. Cotelo Mariana R.A. Ribeiro 《The Journal of chemical thermodynamics》2009,41(9):984-991
117.
Maria Paula Campello Marina Balbina Isabel Santos Přemysl Lubal Radek Ševčík Romana Ševčíková 《Helvetica chimica acta》2009,92(11):2398-2413
The protonation constants of 2‐[4,7,10‐tris(phosphonomethyl)‐1,4,7,10‐tetraazacyclododecan‐1‐yl]acetic acid (H7DOA3P) and of the complexes [Ln(DOA3P)]4? (Ln=Ce, Pr, Sm, Eu, and Yb) have been determined by multinuclear NMR spectroscopy in the range pD 2–13.8, without control of ionic strength. Seven out of eleven protonation steps were detected (pK =13.66, 12.11, 7.19, 6.15, 5.77, 2.99, and 1.99), and the values found compare well with the ones recently determined by potentiometry for H7DOA3P, and for other related ligands. The overall basicity of H7DOA3P is higher than that of H4DOTA and trans‐H6DO2A2P but lower than that of H8DOTP. Based on multinuclear‐NMR spectroscopy, the protonation sequence for H7DOA3P was also tentatively assigned. Three protonation constants (pKMHL, pKMH2L, and pKMH3L) were determined for the lanthanide complexes, and the values found are relatively high, although lower than the protonation constants of the related ligand (pK , pK , and pK ), indicating that the coordinated phosphonate groups in these complexes are protonated. The acid‐assisted dissociation of [Ln(DOA3P)]4? (Ln=Ce, Eu), in the region cH+=0.05–3.00 mol dm?3 and at different temperatures (25–60°), indicated that they have slightly the same kinetic inertness, being the [Eu(H2O)9]3+ aqua ion the final product for europium. The rates of complex formation for [Ln(DOA3P)]4? (Ln=Ce, Eu) were studied by UV/VIS spectroscopy in the pH range 5.6–6.8. The reaction intermediate [Eu(DOA3P)]* as ‘out‐of‐cage’ complex contains four H2O molecules, while the final product, [Eu(DOA3P)]4?, does not contain any H2O molecule, as proved by steady‐state/time‐resolved luminescence spectroscopy. 相似文献
118.
Silva MM Vale MG Damin IC Welz B Mandaji M Fett JP 《Analytical and bioanalytical chemistry》2003,377(1):165-172
The amount of sample that is available for analysis in laboratory plant cultivation experiments is usually very limited. Highly sensitive analytical techniques are therefore required, even for elements that are present in the plants at mg g–1 concentrations, and graphite furnace atomic absorption spectrometry (GFAAS) was chosen in this work because of its micro-sampling capability, and its relatively simple operation. Four micro-methods were investigated for the determination of iron in roots and leaves of rice plants: i) a micro-digestion with nitric and hydrochloric acids, ii) a slurry procedure using tetramethylammonium hydroxide (TMAH) tissue solubilizer, iii) a slurry prepared in 1.4 mol L–1 nitric acid, and treated in an ultrasonic bath, and iv) the direct analysis of solid samples. The micro-digestion was suffering from high blank values and contamination problems, so that it could not be recommended for routine purposes. The TMAH method exhibited poor precision and occasional low recoveries, particularly for real samples. Direct solid sampling analysis gave results similar to those obtained with the slurry technique with ultrasonic agitation for the determination of iron in certified reference materials with iron content up to about 100 g g–1, but was too sensitive for the investigated rice plants, which had an iron content up to several mg g–1. The slurry technique with ultrasonic treatment of the samples, suspended in dilute nitric acid, was finally adopted as the method of choice.The method was then applied for the determination of iron in the leaves and in different compartments of the roots of two rice cultivars, one sensitive to iron toxicity, an important nutritional disorder, and the other one resistant to iron toxicity. The results suggest that the higher resistance to iron toxicity of the second cultivar is due to a smaller uptake of iron from the soil, resulting in lower iron levels in all compartments of the plant. 相似文献
119.
The elution behaviour of different polymer-solvent systems in three types of organic columns for SEC has been compared and interpreted. The experimental data show that the classical universal calibration is not accomplished. Deviations from a unique curve are observed due to the binary and ternary interactions between the components of the system (solvent, polymer and gel) which results on secondary mechanisms accompanying the main pure or "ideal" SEC separation mechanism. Both, enthalpic and entropic effects are interpreted in terms of the swelling and crosslinking degrees of the gel packings, and are also related with the fractal characteristics of their surfaces, such as the fractal dimension and the available pore size. Moreover, a relationship between the fractal dimension of the pore surface and the chromatographic distribution coefficient is proposed. 相似文献
120.
Bernd Schröder Luís M.N.B.F. Santos Isabel M. Marrucho João A.P. Coutinho 《Fluid Phase Equilibria》2010
The methodology for the prediction of aqueous solubilities of solid organic compounds, and their temperature dependence, based on the Conductor-like Screening Model for Real Solvents (COSMO-RS/COSMOtherm) procedure, is presented and evaluated. The predictive capability of the quantum chemistry based program and the applied methodology was tested on the most common solid carboxylic acids. From the temperature dependence of the solubilities, the mean apparent enthalpies of solution were derived. The results obtained for a set of 27 carboxylic acids, consisting of aromatic carboxylic acids, dicarboxylic acids, as well as hydroxycarboxylic acids, are in good agreement with the experimental solubility data and their dependence with the temperature. The mean apparent enthalpies of solution, although of the same order of magnitude of the experimentally values, seem to be systematically underestimated. 相似文献