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991.
Determination of pesticides in waters by capillary gas chromatography with atomic emission detection 总被引:5,自引:0,他引:5
Viñas P Campillo N López-García I Aguinaga N Hernández-Córdoba M 《Journal of chromatography. A》2002,978(1-2):249-256
Capillary gas chromatography with atomic emission detection (GC-AED) was successfully used to separate and quantify 14 pesticides (organochlorines, organophosphorus compounds and pyrethrins) in water samples after liquid-liquid extraction with ethyl acetate. Monitoring the emission lines for elements such as chlorine, bromine and sulfur ensures nearly specific chromatograms for these elements, and markedly increases selectivity. Calibration curves were obtained by plotting peak area versus concentration and the correlation coefficients relating to linearity were at least 0.999. Each chromatographic separation takes 21 min and, since two injections are necessary, it requires approximately 1 h to analyze one sample. The method shows a precision of 4.3-8.2% (RSD), depending on the compound. The application of liquid-liquid extraction with ethyl acetate led to recoveries from spiked samples ranging from 76 to 113%. The sensitivity and linearity for the elements chlorine, sulfur, nitrogen and phosphorus were checked under the optimized conditions at their customary emission wavelength. The sensitivity and linearity for these compounds decreased in the order (atom and emission wavelength) Cl (479 nm)>S (181 nm)>P (178 nm)>N (174 nm). A study of the GC-AED system's response to chlorine concentration in eight pesticide molecules was performed and a linear relationship was found with a correlation coefficient of 0.987. 相似文献
992.
Jacobi BG Laitar DS Pu L Wargocki MF DiPasquale AG Fortner KC Schuck SM Brown SN 《Inorganic chemistry》2002,41(18):4815-4823
Trimesityliridium(III) (mesityl = 2,4,6-trimethylphenyl) reacts with O(2) to form oxotrimesityliridium(V), (mes)(3)Ir=O, in a reaction that is cleanly second order in iridium. In contrast to initial reports by Wilkinson, there is no evidence for substantial accumulation of an intermediate in this reaction. The oxo complex (mes)(3)Ir=O oxidizes triphenylphosphine to triphenylphosphine oxide in a second-order reaction with DeltaH++ = 10.04 +/- 0.16 kcal/mol and DeltaS++ = -21.6 +/- 0.5 cal/(mol.K) in 1,2-dichloroethane. Triphenylarsine is also oxidized, though over an order of magnitude more slowly. Ir(mes)(3) binds PPh(3) reversibly (K(assoc) = 84 +/- 3 M(-1) in toluene at 20 degrees C) to form an unsymmetrical, sawhorse-shaped four-coordinate complex, whose temperature-dependent NMR spectra reveal a variety of dynamic processes. Oxygen atom transfer from (mes)(3)Ir=O and dioxygen activation by (mes)(3)Ir can be combined to allow catalytic aerobic oxidations of triphenylphosphine at room temperature and atmospheric pressure with overall activity (approximately 60 turnovers/h) comparable to the fastest reported catalysts. A kinetic model that uses the rates measured for dioxygen activation, atom transfer, and phosphine binding describes the observed catalytic behavior well. Oxotrimesityliridium does not react with sulfides, sulfoxides, alcohols, or alkenes, apparently for kinetic reasons. 相似文献
993.
Guillard J Meth-Cohn O Rees CW White AJ Williams DJ 《Chemical communications (Cambridge, England)》2002,(3):232-233
The first calixhetarenes with more than one heteroatom in the constituent rings are prepared in one step by treatment of calix[4]furan 1a and calix[6]furan 1b with ethyl carbamate, thionyl chloride and pyridine to give 2, 3, 4 and 5, 6, 7 respectively; these products have been characterised by X-ray crystallography which reveals that in 2 all eight heteroatoms lie on one face of the macrocyle. 相似文献
994.
Muchová L Jirsa M Kuroki M Dudková L Benes MJ Marecek Z Smíd F 《Biomedical chromatography : BMC》2001,15(6):418-422
Carcinoembryonic cell adhesion molecule 1 (CEACAM1) is a human membrane glycoprotein belonging to the carcinoembryonic antigen (CEA) family and to the immunoglobulin superfamily. It is expressed in apical membranes of many epithelial cells in gastrointestinal and urogenital tract and also in granulocytes and lymphocytes, and its biological effect in human tissues has recently been discussed in literature. The purpose of this study was to isolate CEACAM1 glycoprotein from bile and characterize its purity and recovery which has not been described before. Affinity chromatography of CEACAM1 on hydrazide-activated cellulose with immobilized monoclonal anti-CEA F34-187 antibody is described. The immunoglobulin carbohydrate moiety was oxidized by periodate and then bound to hydrazide-activated matrix. Crude protein fraction from bile was applied on the affinity column and after extensive washing of non-bound proteins CEACAM1 was eluted with 6 M guanidine-HCl. A single immunopositive 85 kDa band was detected on Western blots with anti-CEA antibody after SDS-PAGE. We found out that CEACAM1 was not stainable with any common method of protein staining and the only non-specific method which could detect the 85 kDa band was a lectin staining. 相似文献
995.
Pierre-Anton Aichinger Martin Michel Colin Servais Marie-Lise Dillmann Martine Rouvet Nicola D''Amico Ralf Zink Henning Klostermeyer David S. Horne 《Colloids and surfaces. B, Biointerfaces》2003,31(1-4):243-255
Fermentation of a reconstituted skim milk concentrate (8% protein) was investigated to elucidate the effects of various fermentation parameters on the structural, rheological and visual (wheying-off) properties of the resulting gels (pH 4.60). Fermentation trials were performed with non-exocellular polysaccharide-producing strains of Streptococcus thermophilus at various fermentation temperatures and at various chymosin levels. Oscillatory vane rheometry carried out on the intact gels (at 4 °C) showed that the level of chymosin had a significant impact on the gel strength (storage modulus G′). This can be explained by the arrangement of casein micelles into more compact aggregates and the enhanced fusion of aggregated casein micelles as revealed by transmission electron microscopy for the gels fermented with chymosin. Wheying-off of the stirred gels as measured by a centrifugation test (at 4 °C) and pore size of the intact gel structures investigated by scanning electron microscopy both increased with increasing level of chymosin and increasing fermentation temperature (resulting in an increase in acidification rate). A higher level of syneresis (wheying-off) is explained by the larger pore size, since larger pores present a lower resistance to the outflow of whey from the gel. 相似文献
996.
Patrizia Calaminici Victor D. Domínguez-Soria Gerald Geudtner Elizabeth Hernández-Marín Andreas M. Köster 《Theoretical chemistry accounts》2006,115(4):221-226
The parallelization of the three-center electron repulsion integrals arising from the variational fitting of the Coulomb potential
is presented. A scheme for dynamical load balancing of the corresponding loop structure is discussed. The implementation in
the density functional theory program deMon using the message passing interface is described. The efficiency of the parallelization
is analyzed by selected benchmark calculations 相似文献
997.
998.
An artificial polypeptide scaffold composed of surface anchor and protein capture domains was designed and expressed in vivo. By using a mutant E. coli phenylalanyl-tRNA synthetase, the photoreactive amino acid para-azidophenylalanine was incorporated into the surface anchor domain. Octyltrichlorosilane-treated surfaces were functionalized with this polypeptide by spin coating and photocrosslinking. The resulting protein films were shown to immobilize recombinant proteins through association of coiled coil heterodimer. 相似文献
999.
Stopar D Strancar J Spruijt RB Hemminga MA 《Journal of chemical information and modeling》2005,45(6):1621-1627
Molecular modeling based on a hybrid evolutionary optimization and an information condensation algorithm, called GHOST, of spin label ESR spectra was applied to study the structure and dynamics of membrane proteins. The new method is capable of providing detailed molecular information about the conformational space of the spin-labeled segment of the protein in a membrane system. The method is applied to spin-labeled bacteriophage M13 major coat protein, which is used as a model membrane protein. Single cysteine mutants of the coat protein were labeled with nitroxide spin labels and incorporated in 1,2-dioleoyl-sn-glycero-3-phosphocholine (DOPC) bilayers. The new computational method allows us to monitor distributions of local spatial constraints and molecular mobility, in addition to information about the location of the protein in a membrane. Furthermore, the results suggest that different local conformations may coexist in the membrane protein. The knowledge of different local conformations may help us to better understand the function-structure relationship of membrane proteins. 相似文献
1000.
Marie-Noelle Avettand-Fènoël N. David G. Reumont J. -M. Fiorani M. Vilasi P. Perrot 《Journal of Thermal Analysis and Calorimetry》2007,90(2):329-332
The Fe-Sn-Zn system is of interest because Sn is one element added to the Zn galvanizing bath to overcome the drawbacks due
to the presence of Si in semi-killed steels. This work has been undertaken with the aim to understand the tin effect on the
microstructure and the layers growth in batch galvanized coatings on low alloyed steels.
Various experimental techniques such as metallography, scanning electron microscopy (SEM) coupled with X-ray energy dispersive
spectroscopy (EDX) are used in order to characterize the microstructure and the properties of such coatings elaborated in
a zinc bath enriched with tin.
Solidification phenomena and layers growth mechanisms during galvanization are explained by means of the ternary phase diagram
Fe-Sn-Zn at 450°C. The Calphad method allows to obtain this phase diagram from the three optimized binary phase diagrams Fe-Sn,
Fe-Zn and Sn-Zn and some experimental data inside the ternary Fe-Sn-Zn system. 相似文献