The analysis of barbiturates in human serum (or plasma) and urine by high-performance capillary electrophoresis-electrokinetic capillary chromatography with on-column fast-scanning multi-wavelength detection is discussed. The use of a buffer of ca. pH 8 and containing sodium dodecyl sulphate provides a medium suitable for fast and high-resolution separations of barbiturates. Seven barbiturates are characterized by their retention and absorption spectra between 195 and 320 nm. Comparison of these computer-stored data with those of unknown samples is shown to allow the identification of barbiturates in samples of patients undergoing pharmacotherapy and in toxicological urine and serum specimens. Three-dimensional electropherograms provide reliable information on the requirement and suitability of sample pretreatment procedures. With urine, extraction of barbiturates prior to analysis is necessary. With human serum several barbiturates, including phenobarbital, are shown to elute in an interference-free window in front of uric acid and the proteins, allowing these substances to be determined by direct sample injection. The need for multi-wavelength detection over a relatively wide wavelength range as a means of peak confirmation in electrokinetic capillary analyses is demonstrated and limitations of this technique for compounds with similar retention behaviour and absorption spectra are discussed. 相似文献
Traditional ensiling of plant material by anaerobic lactic acid fermentation was combined with enzymatic hydrolysis (ENLAC for short) with cell wall degrading enzymes (hemicellulases, cellulases, and pectinases) to increase fiber digestibility or to increase the recovery of cell content from plants. Such findings were made using 0.015% (w/w, wet basis) Phylacell® enzyme preparation by ENLAC of corn and corn-sorghum mixtures, but not of forage grasses. Addition to alfalfa of a mixture of cell wall degrading enzymes, such as NOVO Viscozyme® together with NOVO Celluclast® each at 0.2–1.0% (w/w, wet basis), resulted in more rapid ensiling and improvement of rumen digestibility of silage by 20%. After 20 d of ensiling at 25 °C when the same enzymes were added to alfalfa at the 1.0% level, protein recovery by pressing increased by 35%, β-carotene recovery by 80%, and chlorophyll/xanthophyll recovery by 30%. ENLAC with the same enzymes also increased the recovery of sclareol from muscatel sage by 400%.
An ICP-MS method for the determination of ultra-traces of 24 Elements (Li, Be, Mg, Al, Cr, Mn, Co, Zn, Cu, Ga, As, Se, Rb, Sr, Mo, Ag, Cd, Sn, Sb, Ba, Tl, Pb, Bi, U) at ng/L to μg/L levels in highly saline solutions (up to 30 g/L NaCl) was developed. Calculated to the salt content of the samples, limits of detection at the sub-μg/kg level were obtained. This allows the measurement of samples like sea water, or clinical samples like urine, serum and whole blood, with few or without sample preparation and a drastic improvement to the limits of detection. Compared to the determination in solutions of 1 g/L NaCl the limits of detection in the original sample were improved by one order of magnitude. Improvements in instrumental stability are achieved by the use of an additional gas, that is introduced to the aerosol stream and avoids salt deposition in the aerosol tube of the torch, the use of High Matrix Content (HMC) cones, that show no clogging even at NaCl-concentrations up to 50 g/L. With this setup the long term stability for measurements with changing matrix concentrations is < 10% without and < 5% with use of an internal standard for the individual samples. Cleaning up is necessary after 2 days of operation. The direct analysis of the Nearshore Seawater Reference Material NRC-CNRC CASS3 showed a good agreement with the certified and measured concentrations. Elements, that do not suffer from an isobaric overlap of matrix compounds can be determined clearly at ng/L levels. Measurement of different matrix concentrations showed, that acceptable results can be achieved with a single calibration for concentrations from 5 g/L NaCl to 30 g/L NaCl, though matrix matching shows the best results. 相似文献
The angular dependence of the muon Knight shift,Kμ, and the muon relaxation rate in Bi at 11 K were measured in external magnetic fields up to 1 T. BothKμ and the second moment,M2, are field dependent and involveP40(cos θ) andP43(cos θ) terms in the angular dependence. The Knight shift behaviour is discussed in terms of the dipole-dipole interaction
and the de Haas-van Alphen effect, a consistent interpretation was not achieved in either case. The field dependence ofM2 is in complete contrast to the second moment calculations and points to a field dependent redistribution of the charge distribution
around the interstitial site. 相似文献
Summary The results of local meteorology, solar radiation and ground-level ozone measurements taken in Antarctica during the second
Italian expedition (December 86–February 87) at Terra Nova Bay are presented. During the summer months the site of the Italian
base camp is characterized by a thin strip of deglaciated ground, along which the temperature measurements close to the ground
and up to 6 m high show a strongly superdiabatic profile. This irregular trend of the temperature in the surface layer is
mainly due to the notable incoming amounts of radiation and to the extreme transparency of the atmosphere. This is also shown
by the low values of the ratio between total radiation and diffuse radiation. The ground is thus subjected to intense heating,
especially in the warmer hours of the day, while the surface layer of the atmosphere will be characterized by strong upward
heat fluxes and by turbulent convective movements. Vertical-temperature-profile measurements show an almost forced persistence
in the superdiabatic trend, which tends towards isothermic values only as a resultof rapid variations in the direction and
intensity of the wind, connected to the downward flux of cold air masses, shown also by the simultaneous increases in ground-level
ozone concentrations which would support the presence of dry-deposition processes in the lower layer. However, the complex
local orography and the horizontal discontinuity (sea, deglaciated coast, snow-covered surfaces) do not permit a correct application
of profile flux relations, normally used in studies on groundlevel dry-deposition.
Paper presented at the IV Congresso del Gruppo Nazionale per la Fisica dell'Atmosfera e dell'Oceano, June 22–24, 1987, Rome. 相似文献