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The contamination of foods with ochratoxin A can be determined very sensitively by high-performance liquid chromatography (HPLC) with fluorescence detection. A novel procedure is described to confirm OA-positive results quantitatively down to the HPLC detection limit of 0.1 ppb. For this, ochratoxin A in the sample extract is converted into its O-methylochratoxin A methyl ester derivative, which is identified subsequently by gas chromatography-mass spectrometry negative-ion chemical ionization and multiple ion detection modes using the hexadeuterated O-methyl-d3-ochratoxin A methyl-d3 ester derivative as internal standard for quantification. In the analysis of more than 60 contaminated samples, the procedure was found to be very accurate. 相似文献
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The liquid Chromatographic separation of 3,3',5-triiodothyronine, 3,3',5'-triiodothyronine, and thyroxine with a nonpolar stationary phase was studied as a function of pH, temperature, organic content of the mobile phase, and ionic strength using aqueous phosphate—acetonitrile, aqueous phosphate—methanol, and aqueous phosphate— n-propanol mobile phase systems. It was demonstrated that the quality of the thyroid hormone separations, as determined by normalized peak capacity values, was unchanged with temperature, remained relatively constant with increasing ionic strength, and was affected to the greatest extent by changes in pH and organic modifier content of the mobile phase. Chromatographic behavior of the compounds studied as a function of these variables was found to be consistent with existing Chromatographic theory and/or empirical observations. Recommended conditions are aqueous phosphate—methanol mobile phase, pH 2–5 (aqueous portion), and high temperature (60–70°C). 相似文献
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We report on collisional depolarization of NO2 fluorescence with use of Hanle effect (zero magnetic field level crossing) experiments. Single fine structure levels of NO2 in several regions of the visible absorption spectrum predominantly near 593 nm and 514 nm are prepared by selective optical excitation and the depolarization of the fluorescence light versus a magnetic field is investigated. We find that the Hanle signal is in general a superposition of two Lorentzian shaped signals, each with a characteristic dependence on light intensity and NO2 pressure. For NO2 pressures >1 µ bar the collisional depolarization follows simple Stern-Volmer kinetics. However, an unusual pressure dependence is observed at NO2 pressures <1 µ bar. In the same pressure range (<1 µ bar) we see also an unexpected resonance with significantly different properties as the Hanle signal. 相似文献
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The separation of racemic benoxaprofen into the two benoxaprofen enantiomers by preparative high-performance liquid chromatography and the application of the activated enantiomers as derivatization reagents for the simultaneous stereoselective determination of chiral amines in biological material is described. Activated (+)- and (-)-benoxaprofen are both shown to be very sensitive and stable chiral fluorescence markers, applicable to thin-layer chromatography as well as to high-performance liquid chromatography. 相似文献
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Fritz Vögtle Edwin Weber 《Journal of inclusion phenomena and macrocyclic chemistry》1992,12(1-4):75-119
We thank the editors of this issue for the opportunity to present the historic development of crown chemistry at the Universities of Wurzburg and Bonn in memory of C. J. Pedersen, the originator of the crown ethers. His legacy of science has tremendously stimulated research at both universities.This paper is dedicated to the memory of the late Dr C. J. Pedersen. 相似文献
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The structures of the inclusion compounds formed by the host 9,9’-(ethyne-1,2-diyl)bis(fluoren-9-01) with pyridine and picolines are similar and display tubular topology. The host discriminates poorly between
these guests. The kinetics of desorption of the pyridine compound is governed by the Avrami-Erofe’ev equation A2, with an
activation energy of 111(7) kJ mol−1. 相似文献