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See detailDetermination of electron and proton auroral energy inputs from FUV-IMAGE
Gérard, Jean-Claude ULg; Hubert, Benoît ULg; Meurant, M. et al

Conference (2001, May 01)

The FUV experiment onboard the IMAGE spacecraft offers the unique possibility to obtain simultaneous snapshots of the global north aurora every 2 minutes in three different spectral channels. The WIC ... [more ▼]

The FUV experiment onboard the IMAGE spacecraft offers the unique possibility to obtain simultaneous snapshots of the global north aurora every 2 minutes in three different spectral channels. The WIC camera has a broadband channel covering the 135-190 nm interval including the N[SUB]2[/SUB] LBH bands, part of which may be absorbed by O[SUB]2[/SUB]. The SI13 channel is centered on the OI 135.6 nm line which is optically thin and includes a ~ 40% LBH contribution. Finally, the SI12 camera images the Doppler-shifted Ly-α emission excited by the proton aurora. This set of instrumentation is combined with auroral models to determine the electron and the proton energy fluxes from the magnetosphere. Examples will be presented and compared with the values deduced from the NOAA satellites. Simultaneous in-situ measurements of the particle characteristic energy have been combined with the data extracted from the FUV images to validate the models and derive empirical relationships between the particle flux measured by the detectors and the brightness observed by FUV-IMAGE at the footprint of the same magnetic field line. Finally, we will assess the ability to deduce the characteristic energy of the auroral particles from the ratio of co-registered images in the WIC and SI13 cameras. This method is based on the difference of vertical distribution of the LBH and the OI 135.6 nm emissions. It offers the potential to globally remotely sense not only the energy flux from the magnetosphere but also the main features of the electron characteristic energy. [less ▲]

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See detailDetermination of Electrostatic Potential Differences Between Coexisting Phases in Aqueous Two-Phase Systems
Bringmann, J; Gaube, J; Keil, B et al

Conference (1993)

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See detailDetermination of enantiomeric purity of S-amlodipine by chiral LC with emphasis on reversal of enantiomer elution order.
Dossou, Katina Sourou Sylvestre ULg; Edorh, P. A.; Chiap, Patrice ULg et al

in Journal of Separation Science (2011), 34

An LC method was developed and prevalidated for the enantiomeric purity determination of S-amlodipine in polar organic solvent chromatography using a chlorine-containing cellulose-based chiral stationary ... [more ▼]

An LC method was developed and prevalidated for the enantiomeric purity determination of S-amlodipine in polar organic solvent chromatography using a chlorine-containing cellulose-based chiral stationary phase (CSP). The concentration of formic acid (FA) (0.01-0.2%) in the mobile phase containing acetonitrile as the main solvent was found to influence the elution order of amlodipine enantiomers as well as the enantioresolution. A reversal of the enantiomer elution order of amlodipine was only observed with chiral stationary phases with both electron-withdrawing (chloro) and electron-donating groups (methyl) on the phenyl moieties of the chiral selector, namely cellulose tris(3-chloro-4-methylphenylcarbamate) and cellulose tris(4-chloro-3-methylphenylcarbamate). The highest enantioresolution (R(s) : 4.1) value was obtained at the lowest FA concentration (0.01%) using cellulose tris(4-chloro-3-methylphenylcarbamate) as the chiral selector and the enantiomeric impurity, R-amlodipine, eluted first under these conditions. Therefore, the mobile phase selected for the prevalidation of the method consisted of ACN/0.1% DEA/0.01% FA and the temperature was set at 25 degrees C. The method was prevalidated by means of the strategy based on the total measurement error and the accuracy profile. The method was found to be selective and the limit of quantification was found to be about 0.05% for R-amlodipine, while the limit of detection was close to 0.02%. [less ▲]

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See detailDetermination of equilibrium association constants of ligand-DNA complexes by electrospray mass spectrometry
Gabelica, Valérie ULg

in Keith R., Fox (Ed.) Drug-DNA Interaction Protocols (2010)

Electrospray mass spectrometry can be used to detect ligand-DNA noncovalent complexes formed in solution. This chapter describes how to determine equilibrium association constants of the complexes ... [more ▼]

Electrospray mass spectrometry can be used to detect ligand-DNA noncovalent complexes formed in solution. This chapter describes how to determine equilibrium association constants of the complexes. Particular attention is devoted to describing how to tune an electrospray mass spectrometer using a 12-mer oligodeoxynucleotides duplex in order to perform these experiments. This protocol can then be applied to any nucleic acid structure that can be ionized with electrospray mass spectrometry. [less ▲]

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See detailDetermination of equivalent material characteristics for parasitic effects in electrical apparatus
Hedia, Hakim; Henrotte, François; Dular, Patrick ULg et al

in IEEE Transactions on Magnetics (1996), 32(5), 4341-4343

For linear systems excited with sinusoidal constraints, an exact dynamical modelling can be performed with a phasor (complex number) approach. For nonlinear systems (exhibiting saturation, hysteresis and ... [more ▼]

For linear systems excited with sinusoidal constraints, an exact dynamical modelling can be performed with a phasor (complex number) approach. For nonlinear systems (exhibiting saturation, hysteresis and higher harmonics), a time stepping model is very time consuming. A method to model such nonlinear systems with an approximated phasor approach is presented. Determination of equivalent material characteristics is discussed and applications are given. [less ▲]

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See detailDetermination of fluorine by proton-induced gamma-ray emission (PIGE) spectrometry in igneous and metamorphic charnockitic rocks from Rogaland (S.W. Norway)
Roelandts, Iwan; Robaye, G; Weber, G et al

in Journal of Radioanalytical & Nuclear Chemistry (1987), 112(2), 453-460

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See detailDetermination of flurbiprofen enantiomers in plasma using a single-isomer amino cyclodextrin derivative in nonaqueous capillary electrophoresis.
Rousseau, Anne ULg; Pedrini, Matteo; Chiap, Patrice ULg et al

in Electrophoresis (2008), 29(17), 3641-8

A nonaqueous capillary electrophoresis (NACE) assay was developed for the separation and determination of flurbiprofen enantiomers in plasma samples using 6-monodeoxy-6-mono(3-hydroxy)propylamino-beta ... [more ▼]

A nonaqueous capillary electrophoresis (NACE) assay was developed for the separation and determination of flurbiprofen enantiomers in plasma samples using 6-monodeoxy-6-mono(3-hydroxy)propylamino-beta-cyclodextrin as chiral selector. The nonaqueous background electrolyte was made up of 40 mM ammonium acetate in methanol (MeOH), and flufenamic acid was employed as internal standard. Solid-phase extraction was used for sample cleanup prior to the NACE separation.The NACE method reproducibility was optimized by evaluating different capillary washing sequences between runs. After having tested various conditions, trifluoroacetic acid (1 M) in MeOH was finally selected. Concerning the solid-phase extraction procedure, good and reproducible analyte recoveries were obtained using MeOH for protein denaturation and a polymeric phase combining hydrophobic interactions with anion exchange properties (Oasis) MAX) was selected as extraction sorbent. The method selectivity was not only demonstrated toward a blank plasma sample but also toward other non-steroidal anti-inflammatory drugs. The method was then successfully validated with respect to response function, trueness, precision, accuracy, linearity and limit of quantification. [less ▲]

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See detailDETERMINATION OF GLUCOSINOLATES IN RAPESEED
Wathelet, Jean-Paul ULg; Mabon, N.; Marlier, M.

Poster (1999)

The official ISO protocol (similar to U.E. recommendations established in 1987 by six european laboratories) for determination of individual glucosinolate content in rapeseed using HPLC was published for ... [more ▼]

The official ISO protocol (similar to U.E. recommendations established in 1987 by six european laboratories) for determination of individual glucosinolate content in rapeseed using HPLC was published for the first time in 1992 (ISO 9167-1). Numerous laboratories, all over the world, use now this method, especially in order to control the 00 varieties. The goals of our research were to considerably reduce the analysis time without loosing precision. A single extraction is now suggested (200 mg of ground seeds stirred in 10 ml of 75°C methanol/water 70/30 with an internal standard for 10 min). Then 1-6 ml of the crude extract is directly put on DEAE A-25 resin prepared according to the ISO method. Glucosinolates are desulfated by addition of 100 µl of concentrated Helix pomatia sulfatase (H1, EC 3.1.6.1) quickly prepared by ethanol precipitation. The desulfatation process can be reduced to 1 hour without any problems with all kind of glucosinolate (alcenyl, benzyl, indolyl, methylthio, methylsulfinyl, methylsulfonyl...). Elution of the desulfo-glucosinolates is realised with 4 x 0.5 ml of distilled water. Desulfo-glucosinolates are separated by HPLC using an Inertsil 3 ODS-3 column (100 x 3 mm, 3 µm) with a water/acetonitrile gradient (from 2 to 25% in 35 min). Resolution is very nice and the limited flow (0.4 ml/min) reduce the solvent costs and the elimination of wastes. The suggested fast method has been compared with the official ISO method analysing the three certified reference materials prepared by BCR (now IRMM) and recommended by U.E. and ISO (CRMs 366, 190 and 367). The recovery of indolyl desulfo-glucosinolates, specially 4-OH glucobrassicin, is higher with the quicker method. Results obtained with the two methods are very close for other desulfo-glucosinolates. [less ▲]

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See detailDetermination of inhibitory potency of argatroban toward thrombin by electrophoretically mediated microanalysis
Pochet, Lionel; Servais, Anne-Catherine ULg; Farcas, Elena ULg et al

in Talanta (2013), 116

Developing an EMMA method for enzymatic assay remains a challenge, particularly using UV detection. Indeed, it is necessary to optimize the separation conditions while allowing the enzymatic reaction to ... [more ▼]

Developing an EMMA method for enzymatic assay remains a challenge, particularly using UV detection. Indeed, it is necessary to optimize the separation conditions while allowing the enzymatic reaction to occur within the capillary respecting kinetic constraints and achieving enough sensitivity. In this work, such EMMA methodology was set up to evaluate the inhibitory potency of drugs toward thrombin, a serine protease implicated in the coagulation cascade. To achieve our goal, the separation buffer, the injection sequence, the internal standard and the chromogenic substrate were investigated. The newly developed system was then assessed determining the kinetic Km constant for the selected substrate and compared with the results obtained with a continuous spectrophotometer cell assay. Secondly, the Ki inhibitory constant of the thrombin inhibitor argatroban was determined and found in agreement with the published value. [less ▲]

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See detailDetermination of iohexol and iothalamate in serum and urine by capillary electrophoresis.
Van Houcke, Sofie K.; Seaux, Liesbeth; Cavalier, Etienne ULg et al

in Electrophoresis (2016)

Estimation of glomerular filtration rate (eGFR) is essential to assess kidney function. Iodine containing contrast agents detection by HPLC has been proposed as a safe alternative for inulin or ... [more ▼]

Estimation of glomerular filtration rate (eGFR) is essential to assess kidney function. Iodine containing contrast agents detection by HPLC has been proposed as a safe alternative for inulin or radioactive compounds. However, HPLC is a time-consuming and labour-intensive method. The aim of this study was to develop an assay for iohexol and iothalamate using capillary electrophoresis (CE). Iohexol and iothalamate were directly analysed by CE in serum and urine, using photometric detection (246 nm). Serum peak height was proportional to iohexol and iothalamate concentrations. Detection limits for iohexol and iothalamate were 10 mg/L and 5 mg/L. Limits of quantification were 13.0 mg/L and 15.0 mg/L. Within-run CVs were 4.9% and 6.5%; between-run CVs 3.1-9.9% and 3.8-13.7%. A good correlation was observed between CE and HPLC: y = 1.1703 x + 5.017 (iohexol) and y = 0.7807 x + 11.01 (iothalamate) [y = concentration obtained by CE (mg/L), x = concentration obtained by HPLC (mg/L)]. In addition, CE allowed to determine urinary iohexol concentration. Although the detection limit for CE was higher than for HPLC, CE can still be used for eGFR determination. Advantages of this high throughput method are the absence of sample pretreatment and a minimal sample volume requirement. This article is protected by copyright. All rights reserved. [less ▲]

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See detailDetermination of isotopic fractionation delta13C of methane from ground-based FTIR observations performed at the Jungfraujoch
Duchatelet, Pierre ULg; Mahieu, Emmanuel ULg; Sussmann, Ralf et al

Poster (2009, April)

Atmospheric methane (CH4) is a strong greenhouse gas that has important chemical impacts on both the troposphere and the stratosphere. In the troposphere, oxidation of methane is a major regulator of OH ... [more ▼]

Atmospheric methane (CH4) is a strong greenhouse gas that has important chemical impacts on both the troposphere and the stratosphere. In the troposphere, oxidation of methane is a major regulator of OH and is a source of formaldehyde, carbon monoxide and hydrogen. In the stratosphere, CH4 plays a central role (i), due to its contribution to the stratospheric water vapor budget, and (ii), as a sink for chlorine atoms which reduces the rate of stratospheric ozone depletion. Because the different sources of methane (natural and anthropogenic like wetlands, rice paddies, termites, natural gas escape, biomass burning, etc) have distinct 13C/12C ratios (usually reported in “delta” notation δ13C), measurements of atmospheric 13CH4 content, in addition to those of the main isotopologue (12CH4), can be used to investigate individual source strengths as well as their spatial and temporal distributions. Characterization of the isotopic fractionation of methane is therefore important, for example, to help models constrain estimates of the global methane budget. However, experimental data for the 13C/12C isotope ratio are sparse. The currently accepted average value of δ13C in atmospheric methane is about -47‰ (Platt et al., 2004). The first goal of this work is to develop and to characterize (in terms of information content and error budget) an original retrieval approach to derive 13CH4 columns from ground-based Fourier transform infrared (FTIR) spectra recorded at the International Scientific Station of the Jungfraujoch (ISSJ; 46.5°N, 8.0°E, 3580m a.s.l., Swiss Alps). The retrieval strategy is based on a Tikhonov L1 approach which has been originally developed for 12CH4 by Sussmann et al. (2008) [see also contributions by Sussmann et al. to this conference (EGU2009-7869)]. In order to validate our 13CH4 products, comparisons with satellite ACE-FTS (Atmospheric Chemistry Experiment - Fourier Transform Spectrometer) measurements are performed. Then, atmospheric δ13C ratios derived from the FTIR measurements will be compared to values published in the literature and critically discussed. References: Platt, U., W. Allan and D. Lowe, Hemispheric average Cl atom concentration from 13C/12C ratios in atmospheric methane, Atmos. Chem. Phys., 4, 2393-2399, 2004. Sussmann, R., Forster, F., Borsdorff, T., et al.: Satellite validation of column-averaged methane on global scale: ground-based data from 15 FTIR stations versus last generation ENVISAT/SCIAMACHY retrievals, IGAC 10th International Conference, Annecy, France, 7-12 Sep 2008. [less ▲]

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See detailDetermination of ITM Key Parameters By the Ionospheric Connection Explorer (ICON)
Immel, T. J.; England, S.; Mende, S. B. et al

Conference (2014)

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See detailDetermination of kinetics and the crystal structure of a novel type 2 isopentenyl diphosphate: dimethylallyl diphosphate isomerase from Streptococcus pneumoniae.
de Ruyck, Jerome; Janczak, Matthew W.; Neti, Syam Sundar et al

in Chembiochem : a European journal of chemical biology (2014), 15(10), 1452-1458

Isopentenyl diphosphate isomerase (IDI) is a key enzyme in the isoprenoid biosynthetic pathway and is required for all organisms that synthesize isoprenoid metabolites from mevalonate. Type 1 IDI (IDI-1 ... [more ▼]

Isopentenyl diphosphate isomerase (IDI) is a key enzyme in the isoprenoid biosynthetic pathway and is required for all organisms that synthesize isoprenoid metabolites from mevalonate. Type 1 IDI (IDI-1) is a metalloprotein that is found in eukaryotes, whereas the type 2 isoform (IDI-2) is a flavoenzyme found in bacteria that is completely absent from human. IDI-2 from the pathogenic bacterium Streptococcus pneumoniae was recombinantly expressed in Escherichia coli. Steady-state kinetic studies of the enzyme indicated that FMNH2 (KM =0.3 muM) bound before isopentenyl diphosphate (KM =40 muM) in an ordered binding mechanism. An X-ray crystal structure at 1.4 A resolution was obtained for the holoenzyme in the closed conformation with a reduced flavin cofactor and two sulfate ions in the active site. These results helped to further approach the enzymatic mechanism of IDI-2 and, thus, open new possibilities for the rational design of antibacterial compounds against sequence-similar and structure-related pathogens such as Enterococcus faecalis or Staphylococcus aureus. [less ▲]

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See detailDetermination of lidocaine and its two N-desethylated metabolites in dog and horse plasma by high-performance liquid chromatography combined with electrospray ionization tandem mass spectrometry
Maes, A.; Weiland, L.; Sandersen, Charlotte ULg et al

in Journal of Chromatography. B : Analytical Technologies in the Biomedical & Life Sciences (2007), 852(1-2), 180-187

A sensitive method for the quantification of lidocaine and its metabolites, monoethylglycinexylidide (MEGX) and glycinexylidide (GX), in animal plasma using high-performance liquid chromatography combined ... [more ▼]

A sensitive method for the quantification of lidocaine and its metabolites, monoethylglycinexylidide (MEGX) and glycinexylidide (GX), in animal plasma using high-performance liquid chromatography combined with electrospray ionization mass spectrometry is described. The sample preparation includes a liquid-liquid extraction with methyl tert-butylmethyl ether after addition of 2 M sodium hydroxide. Ethyl methylglycinexylidide (EMGX) is used as an internal standard. For chromatographic separation, an ODS Hypersil column was used. Isocratic elution was achieved with 0.0 1 M ammonium acetate and acetonitrile as mobile phases. Good linearity was observed in the range of 2.5-1000 ng ml(-1) for lidocame in both dog and horse plasma. For MEGX, linear calibration curves were obtained in the range of 5-1000 ng ml(-1) and 20-1000 ng ml(-1) for dog and horse plasma, respectively. In dog and horse plasma good linearity was observed in the range of 200-1500 ng ml(-1) for GX. The limit of quantification (LOQ) in dog plasma for lidocaine, MEGX and GX was set at 2.5 ng ml(-1), 20 ng ml(-1) and 200 ng ml(-1), respectively. For horse plasma a limit of quantification of 2.5 ng ml(-1), 5 ng ml(-1) and 200 ng ml(-1) was achieved for lidocaine, MEGX and GX, respectively. In dog plasma, the limit of detection (LOD) was found to be 0.8 ng ml(-1), 2.3 ng ml(-1) and 55 ng ml(-1) for lidocaine, MEGX and GX, respectively. In horse plasma the LOD's found for lidocame, MEGX and GX, were 1.1 ng ml(-1), 0.5 ng ml(-1) and 13 ng ml(-1), respectively. The method was shown to be of use in pharmacokinetic studies after application of a transdermal patch in dogs and after an intravenous infusion in horses. (c) 2007 Elsevier B.V. All rights reserved. [less ▲]

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