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61.
Kucera R Zizkovský V Sochor J Klimes J Dohnal J 《Journal of separation science》2005,28(12):1307-1314
Zirconia-based stationary phases represent an interesting alternative to silica-based materials. Two zirconia-based stationary phases were studied as an option for use in drug analysis. The different properties of zirconia material, distinct from RP silica-columns, were employed for the development of a novel and rapid stability monitoring HPLC method. This method enables simultaneous control of possible degradation processes of active substance (ibuprofen) as well as antimicrobial excipients (methyl-and propylparaben). The separation of ibuprofen, its two main degradation products 2-(4-isobutyrylphenyl)propionic acid and 4-isobutylacetophenone, parabens, and 4-hydroxybenzoic acid as their degradation product was successfully accomplished on a Zr-CarbonC18 column using a mobile phase consisting of acetonitrile-phosphate buffer (pH 4.8)-propan-2-ol (27:56:17, v/v/v). Detection was performed at 258 nm and the analysis was completed within 17 minutes. 相似文献
62.
Wallace WT Wyrwas RB Whetten RL Mitrić R Bonacić-Koutecký V 《Journal of the American Chemical Society》2003,125(27):8408-8414
The discovery that supported gold clusters act as highly efficient catalysts for low-temperature oxidation reactions has led to a great deal of work aimed at understanding the origins of the catalytic activity. Several studies have shown that the presence of trace moisture is required for the catalysts to function. Using near-atmospheric pressure flow reactor techniques, we have studied humidity and temperature effects on the reactivity of gas-phase gold cluster anions with O2. Near room temperature, the humid source produces abundant gold-hydroxy cluster anions, Au(N)OH(-), and these have a reversed O2 adsorption activity: Nonreactive bare gold clusters become active when in the form Au(N)OH(-), while active bare clusters are inactive when -OH is bound. The binding energies for the stable structures obtained from density functional calculations confirm fully these findings. Moreover, the theory provides evidence that electron-transfer induced by the binding of a OH group enhances the reactivity toward molecular oxygen for odd anionic gold clusters and suppresses the reactivity for the even ones. The temperature dependence of O2 addition to Au(3)OH(-) and Au(4)(-) indicates deviations from equilibrium control at temperatures below room temperature. The effects of humidity on gold cluster adsorption activity support the conclusion drawn for the mechanism of O2 adsorption on "dry" gold cluster anions and provides insight into the possible role of water in the enhanced activity of supported gold cluster catalysts. 相似文献
63.
A potentiometric reductimetric method for the determination of platinum (Pt(IV)Pt(II)) with a standard Fe(II) solution in an alkaline medium of mannitol is described. The method, the error of which does not exceed 2%, can be used in the presence of palladium, iridium, and rhodium. 相似文献
64.
P. Vaňura V. Jedináková-Křížová M. Vobecký 《Journal of Radioanalytical and Nuclear Chemistry》2006,267(2):501-503
Summary An extraction technique for the separation of 90Sr from a high excess of90Y has been developed. This procedure can be used for the determination of trace amounts of90Sr in90Y prepared by a radiochemical90Y/90Sr generator by liquid scintillation. 相似文献
65.
Zusammenfassung Die bei 1850, 2000 bzw. 2300°C durch die Reduktion von Scandiumoxid mittels Kohlenstoff in dem der Scandiumdicarbidbildung entsprechenden Molverhältnis hergestellten Produkte wurden mit Wasser zersetzt und mit Hilfe der gleichzeitigen gaschromatographischen und massenspektrometrischen Analyse untersucht. Aus den Ergebnissen geht hervor, daß bei der Scandiumdicarbidbildung gleichzeitig ein weiteres Scandiumcarbid, höchstwahrscheinlich ein Sesquicarbid, entsteht.
Herrn Prof. Dr.H. Nowotny gewidmet.
7. Mitt.: Coll. Czech. Chem. Commun., im Druck. 相似文献
Scandium(III) dicarbide problem. Further experimental results
Products obtained by the reduction of Sc2O3 with carbon at 1850, 2000 and 2300°C, resp., in the molar ratio corresponding to the scandium dicarbide were hydrolysed with water. Gaseous reaction products were analysed using gas chromatography combined with mass spectrometry. Results show, that during dicarbide formation another scandium carbide, probably sesquicarbide, is also formed.
Herrn Prof. Dr.H. Nowotny gewidmet.
7. Mitt.: Coll. Czech. Chem. Commun., im Druck. 相似文献
66.
Thorsteinn Loftsson Dagný Hreinsdóttir Már Másson 《Journal of inclusion phenomena and macrocyclic chemistry》2007,57(1-4):545-552
Studies have shown that cyclodextrins form both inclusion and non-inclusion complexes and that several different types of
complexes can coexist in aqueous solutions. In addition, both cyclodextrins and cyclodextrin complexes are known to form aggregates
and it is thought that these aggregates are able to solubilize drugs through micellar-type mechanism. Thus, stability constants
determined from phase-solubility profiles are rarely true stability constants for of some specific drug/cyclodextrin complexes.
A more precise method for evaluation of the solubilizing effects of cyclodextrins is to determine their complexation efficiency
(CE). CE can be determined by measuring the solubility of a given drug at 2–3 cyclodextrin concentrations in pure water or
a medium constituting the pharmaceutical formulation such as parenteral solution or aqueous eye drop formulation. Based on
the CE value the drug:cyclodextrin ratio in the complexation medium can be determined as well as the increase in the formulation
bulk in a solid dosage form. Determination of CE is a simple method for quick evaluating the solubilizing effects of different
cyclodextrins and/or the effects of excipients on the solubilization. Here we report the CE of 43 different drugs with mainly
2-hydroxypropyl-β-cyclodextrin but also with randomly methylated β-cyclodextrin as well as few other cyclodextrins. Calculation of CE, drug:cyclodextrin molar ratio and the increase in the
formulation bulk is discussed, as well as the influence of the intrinsic solubility and drug lipophilicity on the CE. 相似文献
67.
P. Fantucci S. Polezzo V. Bonačić-Koutecký J. Koutecký 《Zeitschrift für Physik D Atoms, Molecules and Clusters》1989,13(4):355-361
The core-valence correlation potential has been derived for Na and K employing atomic calculations which make use of the density functional formula worked out by Lee, Yang and Parr based on Colle-Salvetti approach. The numerical potential is fitted with a small number of Gaussians leading to a very simple expression for an one-electron corevalence correlation operator? cv . The core-valence correlation corrections can be computed by applying? cv on a quite general class of wavefunctions. Applications of the? cv operator within the framework of valence-electron-only calculations using effective Hamiltonians are presented for Na and K atoms, for Na2, K2, NaK and their cations. Almost all the corrections calculated for the physical properties due to the core-valence correlation lead to results which are in good agreement with those obtained from much more sophisticated treatments and experimental data. 相似文献
68.
Stationary phase containing quinolin-8-ol immobilized on macroporous methacrylate support for the affinity chromatography of porcine pepsin A is described. Optimized chromatographic conditions for separation of porcine pepsin A on this stationary phase were found investigating the influence of pH, concentration, ionic strength and chemical composition of the used mobile phases. The stationary phase shows a good reproducibility of chromatographic analyses (relative standard deviation, +/-2%), a high recovery (ca. 93%) and a satisfactory capacity (13 mg pepsin A/1 mL stationary phase) for porcine pepsin A. The obtained findings confirm the applicability of affinity chromatography on the stationary phase with immobilized quinolin-8-ol to the isolation and determination of porcine pepsin A. 相似文献
69.
70.