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See detailSimultaneous Determination of Methylphenobarbital Enantiomers and Phenobarbital in Human Plasma by on-Line Coupling of an Achiral Precolumn to a Chiral Liquid Chromatographic Column
Ceccato, Attilio ULg; Boulanger, Bruno ULg; Chiap, Patrice ULg et al

in Journal of Chromatography. A (1998), 819(1-2), 143-53

A fully automated liquid chromatographic (LC) method for the simultaneous determination of methylphenobarbital enantiomers and phenobarbital in human plasma has been developed. The method is based on the ... [more ▼]

A fully automated liquid chromatographic (LC) method for the simultaneous determination of methylphenobarbital enantiomers and phenobarbital in human plasma has been developed. The method is based on the use of a precolumn packed with an internal-surface reversed-phase packing material (LiChrospher ADS) for sample clean-up coupled to LC analysis on a cellulose tris(4-methylbenzoate) based chiral stationary phase (Chiralcel OJ-R). A 100-microliter plasma sample was injected directly on the precolumn packed with LiChrospher RP-18 ADS using a mixture of pH 5.0 phosphate buffer-methanol (97:3, v/v) as washing liquid. The analytes were then eluted in the back-flush mode with the LC mobile phase. The enantiomeric separation of methylphenobarbital was achieved on Chiralcel OJ-R). The retention times were modelled using a D-optimal design with ten experimental points in order to optimise the LC mobile phase for the separation of phenobarbital from the enantiomers of mephobarbital. The factors selected were the acetonitrile content, the pH and the sodium perchlorate concentration in the mobile phase. A Derringer's desirability function was used to find an optimal and robust solution within the experimental domain. The mobile phase selected consisted of a mixture of pH 7.0 phosphate buffer-acetonitrile (60:40, v/v). The elution profiles of phenobarbital, methylphenobarbital and blank plasma samples on the precolumn and the time needed for analyte transfer from the precolumn to the analytical column were then determined. Finally, the method developed was validated. [less ▲]

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See detailSimultaneous Determination of Pirlindole Enantiomers and Dehydropirlindole by Chiral Liquid Chromatography
Ceccato, Attilio ULg; Hubert, Philippe ULg; De Tullio, Pascal ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (1998), 17(6-7), 1071-9

Liquid chromatography was employed for the determination of pirlindole enantiomers and its oxidation product dehydropirlindole (DHP). The direct separation of pirlindole enantiomers and DHP was achieved ... [more ▼]

Liquid chromatography was employed for the determination of pirlindole enantiomers and its oxidation product dehydropirlindole (DHP). The direct separation of pirlindole enantiomers and DHP was achieved on a cellulose tris-(3,5-dimethylphenylcarbamate) chiral stationary phase (Chiralcel OD-R). Acetonitrile was used as the organic modifier and sodium perchlorate was used as an ionic additive in the mobile phase. The influence of acetonitrile and sodium perchlorate concentrations on enantioselectivity and achiral selectivity towards DHP was investigated in order to find suitable conditions for the determination of low amounts of each analyte. The mobile phase selected consisted of a mixture of acetonitrile and phosphate buffer (pH 5.0) containing sodium perchlorate (0.05 M) (35:65, v/v) and the UV detector was set at 220 nm. The method developed was validated and was found to be linear in the 0.1-5 microg ml(-1) range (r2 = 0.999 for the three compounds). Repeatability and the intermediate precision for the three analytes at a concentration of 0.1 microg ml(-1) were about 3 and 4%, respectively. This concentration corresponds to the quantification of 0.1% for the minor enantiomer. Actual determinations of enantiomeric purity for single enantiomers of pirlindole were performed. [less ▲]

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See detailSéparation énantiomérique du pirlindole à l’échelle préparative
De Tullio, Pascal ULg; Ceccato, A.; Felekidis, Apostolos ULg et al

Poster (1998, January 16)

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See detailStereoselective determination of s-naproxen in tablets by capillary electrophoresis
Fillet, Marianne ULg; Fotsing, L.; Hubert, Philippe ULg et al

in Journal de Pharmacie de Belgique (1998), 53

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See detailvalidation de méthodes analytiques
Hubert, Philippe ULg; Boulanger, Bruno ULg; Veuthey, J. L.

Conference (1998)

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See detailMethod development strategies for the rapid enantioseparation of drugs by capillary electrophoresis using cyclodextrins as chiral additives
Fillet, Marianne ULg; Fotsing, L.; Piette, V. et al

in Journal de Pharmacie de Belgique (1998), 53

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See detailQuantitative analysis of folic acid in a pharmaceutical formulation by capillary electrophoresis
Fotsing, L.; Fillet, Marianne ULg; Hubert, Philippe ULg et al

in Journal de Pharmacie de Belgique (1998), 53

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See detailValidation of an automated method for the LC determination of atenolol in plasma : application of a new validation strategy
Chiap, Patrice ULg; Boulanger, Bruno ULg; Bimazubute, Marcel et al

in Journal de Pharmacie de Belgique (1998), 53

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See detailFinding rugged pareto optimal solutions in HPLC by means of models : simple is efficient
Boulanger, Bruno ULg; Caliaro, G.; Dewé, Walthère ULg et al

in Journal de Pharmacie de Belgique (1998), 53

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

in Journal de Pharmacie de Belgique (1998), 53

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