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See detailAutomated Determination of Tramadol Enantiomers in Human Plasma Using Solid-Phase Extraction in Combination with Chiral Liquid Chromatography
Ceccato, Attilio ULg; Chiap, Patrice ULg; Hubert, Philippe ULg et al

in Journal of Chromatography. B : Biomedical Sciences and Applications (1997), 698(1-2), 161-70

A sensitive and automated method for the separation and individual determination of tramadol enantiomers in plasma has been developed using solid-phase extraction (SPE) on disposable extraction cartridges ... [more ▼]

A sensitive and automated method for the separation and individual determination of tramadol enantiomers in plasma has been developed using solid-phase extraction (SPE) on disposable extraction cartridges (DECs) in combination with chiral liquid chromatography (LC). The SPE operations were performed automatically by means of a sample processor equipped with a robotic arm (ASPEC system). The DEC filled with ethyl silica (50 mg) was first conditioned with methanol and phosphate buffer, pH 7.4. A 1.0-ml volume of plasma was then applied on the DEC. The washing step was performed with the same buffer. The analytes were eluted with 0.15 ml of methanol, and 0.35 ml of phosphate buffer, pH 6.0, containing sodium perchlorate (0.2 M) were added to the extract before injection into the LC system. The enantiomeric separation of tramadol was achieved using a Chiralcel OD-R column containing cellulose tris-(3,5-dimethylphenylcarbamate) as chiral stationary phase. The mobile phase was a mixture of phosphate buffer, pH 6.0, containing sodium perchlorate (0.2 M) and acetonitrile (75:25). The mobile-phase pH and the NaClO4 concentration were optimized with respect to enantiomeric resolution. The method developed was validated. Recoveries for both enantiomers of tramadol were about 100%. The method was found to be linear in the 2.5-150 ng/ml concentration range [r2=0.999 for (+)- and (-)-tramadol]. The repeatability and intermediate precision at a concentration of 50 ng/ml were 6.5 and 8.7% for (+)-tramadol and 6.1 and 7.6% for (-)-tramadol, respectively. [less ▲]

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See detailEnantioselective Determination of Oxprenolol in Human Plasma Using Dialysis Coupled on-Line to Reversed-Phase Chiral Liquid Chromatography
Ceccato, Attilio ULg; Toussaint, B.; Chiap, Patrice ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (1997), 15(9-10), 1365-74

A fully automated method for the determination of the enantiomers of oxprenolol in human plasma was developed, involving dialysis through a cellulose acetate membrane, clean-up and enrichment of the ... [more ▼]

A fully automated method for the determination of the enantiomers of oxprenolol in human plasma was developed, involving dialysis through a cellulose acetate membrane, clean-up and enrichment of the dialysate on a short precolumn and subsequent chiral liquid chromatographic (LC) analysis. All sample handling operations were executed automatically by a sample processor equipped with a robotic arm (ASTED system). The trace enrichment column (TEC) was packed with octadecylsilica. After conditioning of the TEC with the LC mobile phase and pH 3.0 acetate buffer. After the enrichment step, the analyte was transferred by the LC mobile phase to the analytical column by means of a switching valve. The influence of different parameters of the dialysis process on the recovery of oxprenolol was first investigated using achiral LC conditions. The volume as well as the aspirating and dispensing flow rates of the acceptor solution were the main parameters studied. Oxprenolol was separated on a C18 stationary phase used for the enantioseparation of oxprenolol was a Chiralcel OD-R column which contained cellulose tris (3,5-dimethylphenylcarbamate) coated on silica as chiral selector. The corresponding mobile phase consisted of a mixture of pH 6.0 phosphate buffer containing NaClO4 at 0.45 M concentration and acetonitrile (70:30 v/v). UV detection was performed at 273 nm. The method developed was validated. Recoveries for each enantiomer of oxprenolol were about 80%. The method was found to be linear in the 50-2500 ng ml-1 concentration range (r2 = 0.999 for both enantiomers) and good results with respect to intra- and inter-day reproducibility as well as accuracy were obtained. [less ▲]

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See detailDetermination of Six Water-Soluble Vitamins in a Pharmaceutical Formulation by Capillary Electrophoresis
Fotsing, Lucas ULg; Fillet, Marianne ULg; Bechet, I. et al

in Journal of Pharmaceutical & Biomedical Analysis (1997), 15(8), 1113-23

A method was developed for the quantitative analysis of six water-soluble vitamins (thiamine, nicotinamide, riboflavine, pyridoxine, ascorbic acid and pantothenic acid) in a pharmaceutical formulation ... [more ▼]

A method was developed for the quantitative analysis of six water-soluble vitamins (thiamine, nicotinamide, riboflavine, pyridoxine, ascorbic acid and pantothenic acid) in a pharmaceutical formulation, using free solution capillary zone electrophoresis (CZE) in uncoated fused silica capillaries and UV detection. The influence of different parameters, such as the nature of the buffer anionic component and buffer concentration on the CZE separation of vitamins was investigated using four vitamins of the B group as model compounds. A good compromise between resolution, analysis time and analyte stability was obtained by use of a 50 mM borax buffer of pH 8.5. This CZE method was found to be very useful for the separation of more complex samples, a mixture of ten water-soluble vitamins being completely resolved in about 10 min. However, cyanocobalamine could not be separated from nicotinamide in this CZE system, the two compounds being in uncharged form at the pH used. These two compounds could easily be resolved by micellar electrokinetic chromatography (MEKC), the anionic surfactant dodecylsulfate being added to the running buffer at 25 mM concentration. In the pharmaceutical formulation, some excipients were found to be adsorbed to the capillary surface, giving rise to a progressive decrease of the electroosmotic flow and consequently to a simultaneous increase of analyte migration times. A capillary wash with sodium hydroxide had to be made between successive runs in order to minimize these effects. Good results with respect to linearity, precision and accuracy were obtained in the concentration range studied for the six vitamins, using nicotinic acid as internal standard. [less ▲]

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See detailRésolution préparative du pirlindole
De Tullio, Pascal ULg; Felekidis, Apostolos ULg; Liégeois, Jean-François ULg et al

Poster (1997, May)

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See detailTentatives de synthèse énantiosélective des isomères R et S du pirlindole
Pirotte, Bernard ULg; De Tullio, Pascal ULg; Stachow, M. et al

Poster (1997, May)

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See detailDetermination of N-acetylcysteine and its potential degradation products by LC/APCI+/MS/MS
Toussaint, B.; Ceccato, Attilio ULg; Maes, P. et al

Conference (1997)

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