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51.
The potential of capillary electrophoresis combined with mass spectrometry for the simultaneous determination of two herbicides (glyphosate and glufosinate) and their metabolites (aminomethylphosphonic acid and methylphosphinicopropionic acid) as the native species is demonstrated utilising a simple microelectrospray interface. The interface uses the voltage applied to the CE capillary to drive separation and generate the electrospray, avoiding sample dilution associated with the use of a sheath liquid interface. The chemistry of the internal walls of the capillary has a marked influence on peak shape, and appropriate choice is essential to successful operation of the interface. A linear polyacrylamide coated capillary, which has no electroosmotic flow, gave best reproducibility, with precision of migration time and peak area in the range 1-2 and 7-12% RSD, respectively, for the four analytes. Limits of detection, low-pg on-column, are substantially better than for previous methods and calibration curves over the range 1-100 microM have R2 values greater than 0.97. The observed concentration limit of detection for glyphosate in water is 1 microM and for a water-acetone extract of wheat is 2.5 microM, allowing the underivatised herbicide to be detected at 10% of the maximum residue limit in wheat. 相似文献
52.
Alexander Goodwin Craig E. Banks Dario Omanovi? Richard G. Compton 《Analytica chimica acta》2005,533(2):141-145
Cathodic stripping voltammetry at a boron-doped diamond electrode utilising an insonated accumulation protocol is shown to be possible for the on-site trace detection of free manganese in seawater samples. No sample pre-treatment is required with the application of ultrasound providing a sensitive and selective protocol for the analysis of manganese. The protocol is used in the evaluation of manganese in seawater samples taken near the site of a former ferromanganese factory in the town Šibenik, Croatia. 相似文献
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The voltammetric response of nitrogen dioxide in aqueous sulfuric acid using an edge plane pyrolytic graphite electrode has been explored and contrasted with that from basal plane pyrolytic graphite, glassy carbon or boron-doped diamond electrodes. Edge plane graphite electrode is found to produce an excellent voltammetric signal in comparison with other carbon-based electrodes exhibiting a well-defined analytically useful voltammetric redox couple in 2.5 M sulfuric acid which is absent on the alternative electrodes. 相似文献
56.
R. J. Gehrke E. W. Killian L. V. East J. M. Hoggan S. G. Goodwin G. D. McLaughlin 《Journal of Radioanalytical and Nuclear Chemistry》1998,233(1-2):225-231
A portable, battery-powered, multichannel analyzer (MCA) for use with Ge spectrometers has been developed for in-field use
for the assay of x-and γ-ray emitting radionuclides. The spectrometer is capable of operating to rates greater than 150,000
counts per second. The analyzer is a Canberra InSpector MCA, that is equipped with the INEEL ultra-stable dual-energy pulser,
and pulse injection with subsequent removal (PISR) circuitry. PCGAP, a set of MCA control and spectral analysis programs,
was developed for use on a PC with a Windows NT Operating System. It includes an interactive peak analysis program as well
as automatic spectral analysis programs for the X- and γ-ray regions, and a number of utility programs. The pulser peaks are
calibrated with radioactive sources in terms of energy (i.e., their energy equivalents are measured) using the PCGAP spectral
analysis package so that energy shifts, including those due to changes in temperature or count rate, do not cause a loss of
energy calibration. The number of injected low- and high-energy-equivalent pulses is known so the stored pulser pulses can
be used for a dead-time and random summing correction. The pulser peaks are also used to monitor any deterioration in spectral
quality caused by noise, ground loops, etc. The results of performance tests to demonstrate the capabilities of this pulser-equipped
InSpector are reported. 相似文献
57.
Summary It is shown that the retention indices of polar solutes are affected by the amount of stationary phase in the column. The retention indices increase with decreasing stationary phase loadings. The reasons for this behavior are most likely due to the existence of mixed retention mechanisms. At low amounts of stationary phases, adsorption on the support or column walls can take place. Studies were made using four supports, two of which were Chromosorb W and the other two Chromosorb P. The effects of changing the liquid phase loadings are more pronounced when using Chromosorb P. 相似文献
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Abstract A facile procedure is presented for the synthesis of (E)-1-(3′-hydroxy-2′-furanyl)-3-(3″-hydroxy-4″-methoxyphenyl)-2- propen-1-one (6). Galactosylisomaltol (1) was condensed with isovanillin (2) under strong alkaline conditions at 25 [ddot]C to form (E)-1-(3′-O-β-D-galactopyranosyloxy-2′-furanyl)-3-(3″- hydroxy-4″-methoxyphenyl)-2-propen-1-one (4). (E)-1-(3′-hydroxy-2′-furanyl)-3-(3″-hydroxy-4″-methoxyphenyl)-2-propen-1-one (6) was obtained by acid hydrolysis of 4 in a 53.9% yield. This hetero-cyclic 2-propen-1-one was characterized on the basis of spectral data (IR and 1H NMR), physicochemical properties, and conversion to a mono-O-acetyl derivative. 相似文献
60.
Harvey SD Mong GM Ozanich RM McLean JS Goodwin SM Valentine NB Fredrickson JK 《Analytical and bioanalytical chemistry》2006,386(2):211-219
A novel, affinity-augmented, bacterial spore-imprinted, bead material was synthesized, based on a procedure developed for
vegetative bacteria. The imprinted beads were intended as a front-end spore capture/concentration stage of an integrated biological
detection system. Our approach involved embedding bead surfaces with Bacillus thuringiensis kurstaki (Bt) spores (as a surrogate for Bacillus anthracis) during synthesis. Subsequent steps involved lithographic deactivation using a perfluoroether; spore removal to create imprint
sites; and coating imprints with the lectin, concanavalin A, to provide general affinity. The synthesis of the intended material
with the desired imprints was verified by scanning electron and confocal laser-scanning microscopy. The material was evaluated
using spore-binding assays with either Bt or Bacillus subtilis (Bs) spores. The binding assays indicated strong spore-binding capability and a robust imprinting effect that accounted for 25%
additional binding over non-imprinted controls. The binding assay results also indicated that further refinement of the surface
deactivation procedure would enhance the performance of the imprinted substrate. 相似文献