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81.
Birgit Langenbach-Kuttert Ronald Roß Reginald Gruehn 《Monatshefte für Chemie / Chemical Monthly》1985,116(11):1275-1289
Niobiumoxidefluorides Nb59O147F, Nb31O77F, Nb65O161F3 and Nb34O84F2 were prepared by reaction of Nb2O5 and Nb3O7F at 1 270°C. These niobiumoxidefluorides have blockstructures which were examined by high resolution electron microscopy. The observed images of the crystal structures were compared with computer simulated images. 相似文献
82.
Alessandra Gentili Fulvia Caretti Giuseppe D’Ascenzo Lucia Mainero Rocca Stefano Marchese Stefano Materazzi Daniela Perret 《Chromatographia》2007,66(9-10):669-676
Two new methods of analysis, based on liquid chromatography–tandem mass spectrometry, for simultaneous determination of trichothecenes A, B, and D in maize flour and oil have been developed and validated in accordance with European Commission decision 2002/657/EC (recovery, CCα, CCβ, and precision). The trichothecenes were extracted from maize flour by matrix solid-phase dispersion, with recoveries ≥79%, and from maize oil by liquid–liquid extraction, with recoveries ≥78%. Limits of quantitation ranged between 0.03 and 50 μg kg?1, depending on the electrospray response to each analyte and on the matrix. Monitoring of flour and oil samples with this HPLC–MS–MS method revealed the presence of deoxynivalenol, T-2 toxin, and diacetoxyscirpenol at very low concentrations. 相似文献
83.
Daniela Walterová Zdeně;K Stránský Vladimír Preininger Prof. Dr. Vilím Šimánek 《Electrophoresis》1985,6(3):128-132
The isotachophoretic behavior of quaternary benzo/c/phenanthridine, protoberberine and aporphine alkaloids in different electrolyte systems is described. The concentration of the leading ion and the pH value of the leading electrolyte affect the relative effective mobilities of the alkaloids. The system of pH 4.7, containing the leading ion K+ (0.005 M) counter ion acetate, and the terminating ion β-alanine (0.02 M), has been selected for the quantitative determination of the studied alkaloids in model mixtures and plant extracts. 相似文献
84.
Microwave-assisted acid hydrolysis of proteins combined with liquid chromatography MALDI MS/MS for protein identification 总被引:4,自引:0,他引:4
Simple and efficient digestion of proteins, particularly hydrophobic membrane proteins, is of significance for comprehensive proteome analysis using the bottom-up approach. We report a microwave-assisted acid hydrolysis (MAAH) method for rapid protein degradation for peptide mass mapping and tandem mass spectrometric analysis of peptides for protein identification. It uses 25% trifluoroacetic acid (TFA) aqueous solution to dissolve or suspend proteins, followed by microwave irradiation for 10 min. This detergent-free method generates peptide mixtures that can be directly analyzed by liquid chromatography (LC) matrix-assisted laser desorption ionization (MALDI) mass spectrometry (MS) without the need of extensive sample cleanup. LC-MALDI MS/MS analysis of the hydrolysate from 5 microg of a model transmembrane protein, bacteriorhodopsin, resulted in almost complete sequence coverage by the peptides detected, including the identification of two posttranslational modification sites. Cleavage of peptide bonds inside all seven transmembrane domains took place, generating peptides of sizes amenable to MS/MS to determine possible sequence errors or modifications within these domains. Cleavage specificity, such as glycine residue cleavage, was observed. Terminal peptides were found to be present in relatively high abundance in the hydrolysate, particularly when low concentrations of proteins were used for MAAH. It was shown that these peptides could still be detected from MAAH of bacteriorhodopsin at a protein concentration of 1 ng/microl or 37 fmol/microl. To evaluate the general applicability of this method, it was applied to identify proteins from a membrane protein enriched fraction of cell lysates of human breast cancer cell line MCF7. With one-dimensional LC-MALDI MS/MS, a total of 119 proteins, including 41 membrane-associated or membrane proteins containing one to 12 transmembrane domains, were identified by MS/MS database searching based on matches of at least two peptides to a protein. 相似文献
85.
Marchese S Curini R Gentili A Perret D Rocca LM 《Rapid communications in mass spectrometry : RCM》2004,18(3):265-272
A simple and rapid method using reversed-phase liquid chromatography/tandem mass spectrometry (LC/MS/MS) for the simultaneous determination of the urinary metabolites of benzene, toluene, xylene and styrene in human urine specimens and standard solutions is described. A hybrid quadrupole/time-of-flight (QqTOF) mass spectrometer was compared for the determination of metabolite of aromatic solvents in urine samples. The metabolites selected were: trans,trans-muconic acid, hippuric acid, o-, m- and p-methylhippuric acid and phenylglyoxylic acid. The compounds were well separated from each other on narrow-bore 1-mm i.d. reversed-phase LC C-18 columns. Average recoveries for loading 100 microL of urine samples varied from 88-110% and the quantification limits were less than 30 ng/mL for each analyte (3 ng/mL for trans,trans-muconic acid). The qualitative information obtained (mass accuracy, resolution and full-scan spectra) with the QqTOF mass spectrometer allows a secure identification of analytes in biological matrices. 相似文献
86.
The 1,10-phenanthroline (phen) complexes of Co(II), Ni(II), Cu(II) and
Cd(II) orotates were synthesized and characterized by elemental analysis,
magnetic susceptibility, spectral methods (UV-vis and FTIR) and thermal analysis
techniques (TG, DTG and DTA). The Co(II), Ni(II), Cu(II) and Cd(II) ions in
diaquabis(1,10-phenanthroline)metal(II) diorotate octahedral complexes [M(H2O)2(phen)2](H2Or)2·nH2O
(M=Co(II), n=2.25; Ni(II), n=3;
Cu(II) and Cd(II), n=2) are coordinated
by two aqua ligands and two moles of phen molecules as chelating ligands through
their two nitrogen atoms. The monoanionic orotate behaves as a counter ion
in the complexes. On the basis of the first DTGmax,
the thermal stability of the hydrated complexes follows the order: Cd(II),
68°C 68°C 相似文献
87.
Cocchi M Faeti V Manfredini M Manzini D Marchetti A Sighinolfi S 《Journal of AOAC International》2005,88(2):393-398
The presence of some essential and toxic metals in fat supplements for swine diet was investigated. Collected samples represented a relevant production of the Italian industry. In particular, some samples were enriched with antioxidants or waste cooking oils. The method for the determination of Ca, Cu, Cd, Fe, Mg, Mn, Ni, Pb, and Zn in fat samples was developed by means of a certified reference material (CRM 186) and a representative fatty sample (RFS). All samples were digested in closed vessels in a microwave oven and then analyzed by flame atomic absorption or graphite furnace atomic absorption spectrometry. The entire analytical method provided a satisfactory repeatability and reproducibility confirmed by agreement between the experimental recovery data obtained for the CRM 186 sample and, with the method of standard additions, for the RFS material. The samples generally showed a small amount of metals compared with the recommended daily intake for the essential elements. On the other hand, some samples contained a significant concentration, from an analytical point of view, of Cd, Ni, and Pb. Principal component analysis (PCA) was applied to inspect the experimental data obtained from samples analysis. Basically no differences were detected in terms of metal concentration among the fat supplements analyzed. 相似文献
88.
N. K. Tunali H. N. Erten S. Kinikoğlu Ş. Gümüş 《Journal of Radioanalytical and Nuclear Chemistry》1979,49(2):225-237
The extraction of iodine and bromine under various conditions from their saturated aqueous solutions by CCl4, C6H6 and o-xylene has been studied. The data obtained from the experiments carried out at various temperatures, for H2O(I2)−CCl4 and H2O(I2)−C6H6 systems, exhibit an Arrhenius behaviour. The overall activation energy calculated for the extraction in the H2O(I2)−CCl4 system, 650±50 cal·mol−1 is lower than that of H2O(I2)−C6H6, 3600±300 cal·mol−1. The use of the solubility parameter for the interpretation of the data in the extraction of iodine is investigated. The
data obtained in multiple extractions are treated by using the analogy between extraction and radioactive decay. The half
number of extraction for each system is determined. The complex curves obtained in the H2O(I2)−CCl4 and H2O(I2) −Br2)−CCl4 systems are resolved into two components. 相似文献
89.
M.?Prasad S.?P.?MoulikEmail author A. Al.?Wardian S.?Moore A.?van?Bommel R.?PalepuEmail author 《Colloid and polymer science》2005,283(8):887-897
The clouding points (CP) of the nonionic surfactants p-tert-octyl phenyl polyoxyethylene ether (Triton X 100), Brij-56 and Brij-97, and the water soluble polymer polyvinylmethylether (PVME) have been measured in the presence of the ionic surfactants alkyl (C10, C12, C14 and C16) triphenyl phosphonium bromides (ATPBs). The threshold additive concentrations required for efficient CP enhancement of the systems that were studied have been determined. Considering CP as the threshold state of phase separation, the energetics of the process at different additive concentrations has been evaluated. The spontaneity of free energy of the clouding process (G
c
0
) at the transition concentrations followed the order PVME > TX 100 Bj 56 > Bj 97. The clouding process has been found to be energetically endothermic with fairly large enthalpy and entropy changes that nicely compensate each other. The compensation temperature has been evaluated and compared with different types of the clouding agents.This revised version was published online in January 2005 with corrections to the names of the authors. 相似文献
90.
Ewa?Cholewa Ian?Burgess Julia?Kunze Jacek?LipkowskiEmail author 《Journal of Solid State Electrochemistry》2004,8(10):693-705
Electrochemical measurements including cyclic voltammetry, differential capacity, and chronocoulometry have been used to characterize the adsorption behaviors of the zwitterionic surfactant
N-dodecyl-N,N-dimethyl-3-ammonio-1-propanesulfonate (DDAPS) on the Au(111) electrode surface. The thermodynamics of the ideally polarized electrode have been employed to determine the Gibbs excess and the Gibbs energy of adsorption. The results show that the adsorption of DDAPS has a multistate character. The first two states are observed at potentials close to zero charge. At low bulk DDAPS concentrations, it corresponds to the formation of a film of nearly flat adsorbed molecules. At higher concentrations it is converted into a hemimicellar state. The second state is formed at negative potentials and charge densities close to 0 C cm–2. It corresponds to a film of tilted molecules oriented with the hydrocarbon tail towards the metal and the polar head toward the solution.Dedicated to Professor Zbigniew Galus on the occasion of his 70th birthday and in recognition of his many contributions to electrochemistry. 相似文献