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Ibon Odriozola Nerea Ormategui Iraida Loinaz José A. Pomposo Hans J. Grande 《Macromolecular Symposia》2008,266(1):96-100
Summary: Coinage metal salts (e.g. AuIII, AgI and CuII salts) readily react with thiols to give the corresponding metal(I) thiolates. These thiolate species are known to either self-assemble into insoluble polymeric species or to form soluble oligomers, depending on the nature of the thiol ligand. Here we demonstrate that this self-assembling ability can be applied to create supramolecular hydrogels. Glutathione (GSH), a naturally occurring tripeptide, has been used in combination with AuIII, AgI and CuII salts to obtain pH responsive hydrogels that are able to gelate 100 times their weight in water. 相似文献
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Ruiz N Reyes E Vicario JL Badía D Carrillo L Uria U 《Chemistry (Weinheim an der Bergstrasse, Germany)》2008,14(30):9357-9367
The organocatalytic conjugate addition of different aldehydes to beta-nitroacrolein dimethyl acetal, generating the corresponding highly functionalized nitroaldehydes in high yields and with high stereoselectivities, has been studied in detail. These transformations have been achieved by using both readily available starting materials in a 1:1 ratio as well as commercially available catalysts at a 10 mol % catalyst loading. Furthermore, a very short and efficient protocol has been devised for the preparation of highly enantioenriched pyrrolidines containing two or three contiguous stereocenters starting from the obtained Michael adducts. 3,4-Disubstituted pyrrolidines have been obtained in a single step by Zn-mediated chemoselective reduction of the nitro group followed by intramolecular reductive amination, and trisubstituted homoproline derivatives have been prepared by means of an olefination reaction and a cascade process involving chemoselective reduction of the nitro group followed by a fully diastereoselective intramolecular aza- Michael reaction. 相似文献
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Antonio Martín Agurtzane Martínez Rosario Pereiro Nerea Bordel Alfredo Sanz-Medel 《Spectrochimica Acta Part B: Atomic Spectroscopy》2007
The determination of sputtering rates is, commonly, an important parameter in glow discharge analyses. In particular, in those quantification procedures where the emission yield plays an important role in calibrations, the correct calculation of such value becomes crucial. The volumetric methods to calculate the sputtering rates (they offer a higher accuracy than the gravimetric ones) aim to measure the crater volume created in the sample during the analysis. The standard approximation assumes the crater as a cylinder and so it is mandatory to achieve crater shapes with a flat bottom and walls perpendicular to it. But in practice, craters show many times a convex (or concave) bottom which depends on the measurement conditions. 相似文献
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J. A. Gallastegui C. L. Folcia J. Etxebarria J. Ortega I. De Francisco M. B. Ros 《Liquid crystals》2002,29(10):1329-1333
Optical second harmonic generation (SHG) measurements have been carried out on the B2 phases of three liquid crystal materials composed of conventional banana-shaped molecules (P-10-O-PIMB, P-8-O-PIMB and P-8-PIMB). Quantitative values of the second order susceptibilities dij have been deduced from SHG measurements at oblique incidences on polydomain racemic samples under an electric field. The dij coefficients are in the range 1-10 pm V-1. 相似文献
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Ferreirós N Iriarte G Alonso RM Jiménez RM Ortíz E 《Journal of separation science》2008,31(4):667-676
In this work, an SPE-HPLC method coupled to photodiode array detection was validated in human urine matrix, in order to monitor four antihypertensive angiotensin II receptor antagonist drugs in patients under cardiovascular treatment. For that purpose, experimental design was used. Quantitation was accomplished by the internal standard method. The obtained LOQs were 95, 113, 125, and 85 ng/mL for eprosartan, telmisartan, irbesartan, and valsartan, respectively. The intraday and interday precision and accuracy at four concentration levels in the working range (LOQ-15 microg/mL) were always lower than 11% RSD and 8% relative error. The urine samples proved to be stable during 4 h at room temperature, after three thaw-freeze cycles, and for 2 months at -20 degrees C. No interferences from other endogenous compounds or co-administered drugs were found. The method has been successfully applied to monitor the renal elimination of eprosartan and valsartan during 24 h. 相似文献
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Viñas P Aguinaga N Campillo N Hernández-Córdoba M 《Journal of chromatography. A》2008,1194(2):178-183
The present study compares two new sample preparation methods, stir bar sorptive extraction (SBSE) and membrane-assisted solvent extraction (MASE) coupled to the novel technique of ultra-performance liquid chromatography (UPLC) for the sensitive, selective and solvent-free determination of six oxazole fungicide residues (hymexazol, drazoxolon, vinclozolin, chlozolinate, oxadixyl and famoxadone) in wine and juices. The analytes were separated on a rapid resolution C(18) column (50 mm x 4.6 mm, I.D., 1.8 microm) thermostated at 50 degrees C with isocratic elution using a 50/50 (v/v) water/acetonitrile (ACN) mobile phase at a flow-rate of 1 mL min(-1) and detected by diode-array detection (DAD). The UPLC method rapidly separates the fungicides (7 min). The best results as regards sensitivity, repeatability and analyte recovery were obtained using SBSE with a polydimethylsiloxane (PDMS) twister, at 60 degrees C for 30 min with stirring at 1700 rpm in the presence of a 0.1M acetate/acetic acid buffer (pH 5) and 20% (m/v) sodium chloride. Liquid desorption was performed with 100 microL of a 80/20 (v/v) ACN/water solution in a desorption time of 15 min. With the PDMS polymer, an apolar phase, hymexazol and oxadixyl were not extracted. Consequently, the SBSE procedure can only be applied to the other four fungicides. Detection limits ranged from 0.05 to 2.5 microgL(-1) at a signal to noise ratio of 3, depending on the compound. Recoveries obtained for spiked samples were satisfactory (83-113%) for all compounds. The proposed method was successfully applied to the analysis of different samples, residues of chlozolinate and drazoxolon being found in samples of red wine and grape juice, respectively. 相似文献
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Solà Vázquez A Martín A Costa-Fernandez JM Ruiz Encinar J Bordel N Pereiro R Sanz-Medel A 《Analytical and bioanalytical chemistry》2007,389(3):683-690
There is an increasing concern regarding the toxicity and environmental distribution and impact of brominated organic compounds
employed as flame retardants. Thus, present interest in searching for new analytical techniques and methods allowing a rapid,
simple and reliable detection of those compounds in materials and wastes potentially containing such flame retardants is not
surprising. The feasibility of using radiofrequency glow discharge plasma spectrometry coupled with optical emission spectrometry
(rf-GD-OES) as a rapid and simple tool to directly analyse bromine-containing flame-retardant polymeric layers is investigated
here. Polymeric layers for calibration were made by mixing appropriate amounts of tetrabromobisphenol A, bisphenol A, phloroglucinol
and diphenylmethane-4,4′-diisocyanate in tetrahydrofuran. The corresponding blanks (polymers without tetrabromobisphenol A)
were also prepared. Detection of bromine was investigated both in the visible (at 470.48 nm) and in the near-infrared (at
827.24 nm) regions, using a charge-coupled device for detection. Discharge parameters affecting the emission intensity of
bromine were first optimized (in argon and helium as possible plasma gases) and the analytical performance characteristics
were then evaluated. The best detection limit (0.044% Br) was achieved measuring Br I 827.24 nm in a He discharge, using a
forward power of 70 W and a pressure of 45 Torr. The linearity range extended up to 27% Br. Finally, the applicability of
the rf-GD-OES method proposed to the quantitative analysis of bromine in solid materials coated with flame-retardant commercial
paints was successfully demonstrated.
Figure Flame Retardants 相似文献