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121.
Fast gas chromatography/negative-ion chemical ionization mass spectrometric (GC/NICI-MS) assay combined with rapid and nonlaborious sample preparation is presented for the simultaneous determination of benzodiazepines and alpha-hydroxy metabolites, zaleplon and zopiclone in whole blood. The compounds were extracted from 100 microl of whole blood by simultaneous multitube, microscale liquid-liquid extraction (LLE) and derivatized by N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA), without the need for the time-consuming concentration stage. In the analytical separation, various parameters of fast GC/NICI-MS were applied, e.g. the use of hydrogen as a GC carrier gas, a high carrier gas velocity, a small film thickness of the analytical column, fast MS data acquisition, fast temperature ramping, and high initial and final temperatures of GC column. Sensitive identification, screening and quantitation of 18 compounds of interest were achieved in chromatographic separation in only 4.40 min. Accurate and reproducible results were obtained by using five different and carefully selected deuterated analogues on the basis of the chemical properties of the target analytes. Nevertheless, for alpha-OH-midazolam, and for bromazepam and flunitrazepam at low concentrations, the results can be considered only semiquantitative on the basis of the validation data. The extraction efficiencies ranged from 74.3 to 105.7% and the limits of quantitation (LOQ) from 1 to 100 ng ml(-1). Rapid sample preparation and fast chromatographic separation allowed cost-efficient, reliable and high sample-throughput analyses with a low amount of manual work. The method was fully validated and accredited according to EN ISO/IEC 17025 standards and is applicable for sensitive, reliable and quantitative determination of benzodiazepines, zaleplon and zopiclone, e.g. in clinical and forensic toxicology. 相似文献
122.
Annika Pohl Gunnar Westin Kjell Jansson 《Journal of Sol-Gel Science and Technology》2003,26(1-3):257-260
The first purely alkoxide-based sol-gel route to nano-phase powders and thin films of perovskite La0.75Sr0.25MnO3 is described. The phase and microstructure evolution on heat treatment of free gel films to form the target nano-phase oxide were investigated by TGA, IR spectroscopy, powder XRD, SEM and TEM-EDS. The xerogel consisted of a hydrated oxo-carbonate, without remaining alkoxo groups or solvent. Heating at 5°C·min–1 decomposed the carbonate groups and yielded the pure perovskite La0.75Sr0.25MnO3 at 760°C. The cell dimensions were virtually unchanged from the first observation of perovskite at 680°C, to 1000°C, 4 h. The monoclinic cell of La0.75Sr0.25MnO3 obtained at 1000°C, 4 h, had the dimensions a = 5.475(1), b = 5.504(2), c = 7.771(1) Å, = 90.50(2), fitting the literature data quite well. Crack-free, homogenous, 150 nm thick La0.75Sr0.25MnO3 films were prepared by spin-coating Si/SiO2/TiO2/Pt and polycrystalline -Al2O3 substrates with a 0.6 M alkoxide solution, followed by heating at 5°C·min–1 to 800°C, 30 min. 相似文献
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Erik Allard Rikard Åslund Tröger Björn Arvidsson Per Johan Ragnar Sjöberg 《Rapid communications in mass spectrometry : RCM》2010,24(4):429-435
Precision, reproducibility and lower limit of quantitation (LLOQ) are important characteristics of a quantitative method. We have investigated these properties for Ximelagatran (Xi), which has a high tendency to form doubly charged ions in electrospray ionization (ESI), by studying the percentage of doubly charged species formed when varying the formic acid (FA) concentration, analyte concentration, amount of organic modifier and flow rate. It was found that the percentage of [Xi + 2H]2+ can be controlled to be more than 90% or less than 10% by varying the amount of FA present, and that the change between these values is dramatic. Furthermore, the percentage of [Xi + 2H]2+ formed decreases with increased analyte concentration and increased flow rate. No apparent relationship with the amount of organic modifier was found. The results have the implication that, by carefully controlling the selected parameters, the LLOQ, precision and reproducibility can be improved. We have compared the fragmentation of the singly and doubly charged species and concluded that the [Xi + 2H]2+ ion is more inclined to undergo fragmentation than [Xi + H]+. As a consequence, unusual instrumental settings had to be used for the experiments. The fragmentation patterns are to a great extent similar, but the doubly charged species is more inclined to generate low‐mass product ions. Copyright © 2010 John Wiley & Sons, Ltd. 相似文献
127.
Estephania Lira Jonas ?. Hansen Peipei Huo Ralf Bechstein Patrick Galliker Erik L?gsgaard Bj?rk Hammer Stefan Wendt Flemming Besenbacher 《Surface science》2010,604(21-22):1945-1960
High-resolution scanning tunneling microscopy (STM) and temperature-programmed desorption (TPD) were used to study the interaction of O2 with reduced TiO2(110)–(1 × 1) crystals. STM is the technique of choice to unravel the relation between vacancy and non-vacancy assisted O2 dissociation channels as a function of temperature. It is revealed that the vacancy-assisted, first O2 dissociation channel is preferred at low temperature (~ 120 K), whereas the non-vacancy assisted, second O2 dissociation channel operates at temperatures higher than 150 K–180 K. Based on the STM results on the two dissociative O2 interaction channels and the TPD data, a new comprehensive model of the O2 chemisorption on reduced TiO2(110) is proposed. The model explains the relations between the two dissociative and the molecular O2 interaction channels. The experimental data are interpreted by considering the available charge in the near-surface region of reduced TiO2(110) crystals, the kinetics of the two O2 dissociation channels as well as the kinetics of the diffusion and reaction of Ti interstitials. 相似文献
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We present experimental evidence that pressure solution creep does not establish a steady-state interface microstructure as previously thought. Conversely, pressure solution controlled strain and the characteristic length scale of interface microstructures grow as the cubic root of time. Transient creep with the same scaling is known in metallurgy (Andrade creep). The apparent universal scaling of pressure solution transient creep is explained using an analogy with spinodal dewetting. 相似文献
130.
Brezger B Hackermüller L Uttenthaler S Petschinka J Arndt M Zeilinger A 《Physical review letters》2002,88(10):100404
We demonstrate a near-field Talbot-Lau interferometer for C70 fullerene molecules. Such interferometers are particularly suitable for larger masses. Using three free-standing gold gratings of 1 microm period and a transversally incoherent but velocity-selected molecular beam, we achieve an interference fringe visibility of 40% with high count rate. Both the high visibility and its velocity dependence are in good agreement with a quantum simulation that takes into account the van der Waals interaction of the molecules with the gratings and are in striking contrast to a classical moiré model. 相似文献