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See detailEnantiomeric separation of amino acid derivatives by non-aqueous capillary electrophoresis using quinine and related compounds as chiral additives.
Piette, Véronique; Fillet, Marianne ULg; Lindner, W. et al

in Biomedical Chromatography : BMC (2000), 14(1), 19-21

Enantiomeric separation of amino acid derivatives by non-aqueous capillary electrophoresis using quinine and related compounds as chiral additives.

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See detailEnantiomeric separation of aminoglutethimide by capillary electrophoresis using native cyclodextrins in single and dual systems
Abushoffa, A. M.; Fillet, Marianne ULg; Marini Djang'Eing'A, Roland ULg et al

in Journal of Separation Science (2003), 26(6-7), 536-542

Aminoglutethimide (AGT) is one of the few examples of chiral drugs that can be enantioseparated by capillary electrophoresis using any of the three native cyclodextrins: alpha-, beta-, or gamma-CD. A ... [more ▼]

Aminoglutethimide (AGT) is one of the few examples of chiral drugs that can be enantioseparated by capillary electrophoresis using any of the three native cyclodextrins: alpha-, beta-, or gamma-CD. A complete resolution of the enantiomers of this compound in cationic form could be achieved with each of the three CDs, using a pH 3 phosphoric acid-triethanolamine buffer. Affinity constants for AGT enantiomers with the three native CDs were determined, confirming that the highest selectivity was given by gamma-CD while the strongest complexation was obtained with beta-CD. However, an opposite affinity pattern was observed with the latter. Selectivity was lower for AGT enantiomers in dual CD systems, compared to that obtained with a single selector at its optimal concentration, which confirms that dual systems are of more limited interest when the two selectors have a similar effect on the analyte mobility. These results are in good agreement with those predicted using recently developed mathematical models. [less ▲]

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See detailEnantiomeric separation of basic compounds usin heptakis(2,3-di-O-methyl-6-O-sulfo)-beta-cyclodextrin in combination with potassium camphorsulfonate in nonaqueous capillary electrophoresis: Optimization by means of an experimental design
Servais, Anne-Catherine ULg; Fillet, Marianne ULg; Chiap, Patrice ULg et al

in Electrophoresis (2004), 25(16), 2701-2710

The enantiomeric separation of a series of basic pharmaceuticals (beta-blockers, local anesthetics, sympathomimetics) has been investigated in nonaqueous capillary electrophoresis (NACE) systems using ... [more ▼]

The enantiomeric separation of a series of basic pharmaceuticals (beta-blockers, local anesthetics, sympathomimetics) has been investigated in nonaqueous capillary electrophoresis (NACE) systems using heptakis(2,3-di-O-methyl-6-O-sulfo)-beta-cyclodextrin (HDMS-P-CD) in combination with potassium camphorsulfonate (camphorSO(3)(-)). For this purpose, a face-centered central composite design with 11 experimental points was applied. The effect of the concentrations of HDMS-beta-CD and camphorSO(3)(-) on enantioresolution was statistically evaluated and depended largely on the considered analyte. The presence of camphorSO(3)(-) was found to be particularly useful for the enantioseparation of compounds with high affinity for the anionic CD. CamphorSO(3)(-) seems to act as a competitor, reducing the affinity for the CD, probably by ion-pair formation with these analytes. For compounds with lower affinity for HDMS-beta-CD, the combination of camphorSO(3)(-) and the CD appeared to have a favorable effect on enantioresolution only if the optimal CD concentration could be reached. On the other hand, for compounds characterized by a very low affinity for the anionic CD, the association of camphorSO(3)(-) and HDMS-beta-CD is always unfavorable. Finally, experimental conditions were selected by means of the multivariate approach in order to obtain the highest resolution (R-s) value for each studied compound. [less ▲]

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See detailEnantiomeric separation of basic drugs by cyclodextrin modified capillary electrophoresis using poly(vinyl alcohol) coated fused silica capillaries
Fillet, Marianne ULg; Schomburg, G.; Bechet, I. et al

in Journal de Pharmacie de Belgique (1995), 50

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See detailEnantiomeric separation of basic drugs on an ovomucoid column
Ceccato, Attilio ULg; Hubert, Philippe ULg; Bechet, I. et al

in Journal de Pharmacie de Belgique (1992), 47

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See detailEnantiomeric Separation of Clenbuterol by Transient Isotachophoresis-Capillary Zone Electrophoresis-Uv Detection New Optimization Technique for Transient Isotachophoresis
Toussaint, B.; Hubert, Philippe ULg; Tjaden, U. R. et al

in Journal of Chromatography. A (2000), 871(1-2), 173-80

A method for the in-line preconcentration and enantioseparation of clenbuterol by transient isotachophoresis-capillary zone electrophoresis-UV absorbance detection (transient ITP-CZE-UV) has been ... [more ▼]

A method for the in-line preconcentration and enantioseparation of clenbuterol by transient isotachophoresis-capillary zone electrophoresis-UV absorbance detection (transient ITP-CZE-UV) has been developed. It implies the use of dimethyl-beta-cyclodextrin as chiral selector and the application of a hydrodynamic counterflow during the ITP step. ITP is used to focus the sample constituents prior to CE whereas a counterpressure counterbalances the electrophoretic migration of the compounds. The sample is then focused and kept stationary in the proximity of the capillary inlet before CZE separation, leading to an extended-volume ITP-CZE system. A new strategy for the fast optimization of the counterpressure has been developed which implies the measurement of the hydrodynamic and electrophoretic velocities of the analyte during ITP. The in-line preconcentration and enantioseparation of clenbuterol selected as model compound was optimized using this method. Salbutamol was chosen as internal reference in order to check the reproducibility of the method. A 173-nl volume of aqueous ample solution was injected which implies an improvement of the injection volume of about 16 and a resolution of 4.8 was obtained for the clenbuterol enantiomers. A concentration detection limit of 10(-6) mol/l was readily achieved for clenbuterol and salbutamol using only 3 min ITP preconcentration in in-line counterflow transient ITP-CZE-UV. Thanks to its fast optimization, the method is applicable to any enantioseparation by means of only five very short preliminary measurements. [less ▲]

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See detailEnantiomeric separation of clenbuterol by transient ITP-CE-MS
Toussaint, B.; Bergmann, J.; Hubert, Philippe ULg et al

Poster (1999)

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See detailEnantiomeric separation of N-protected amino acids by non-aqueous capillary electrophoresis with dimeric forms of quinine and quinidine derivatives serving as chiral selectors
Piette, Vincent ULg; Lindner, W.; Crommen, Jacques ULg

in Journal of Chromatography. A (2002), 948(1-2), 295-302

A non-aqueous capillary electrophoretic method with quinine and tert.-butyl carbamoylated quinine as chiral selectors was developed previously for the enantioseparation of N-protected amino acids. This ... [more ▼]

A non-aqueous capillary electrophoretic method with quinine and tert.-butyl carbamoylated quinine as chiral selectors was developed previously for the enantioseparation of N-protected amino acids. This system was here applied as a screening tool for a fast evaluation of the chiral discrimination potential of six new dimeric forms of carbamoylated quinine and quinidine derivatives as chiral additives: 1,3-phenylene-bis(carbamoylated quinine), 1,6-hexamethylene-bis(carbamoylated quinine), 1,6-hexamethylene-bis(carbamoylated quinidine), trans-1,4-cyclohexylene-bis(carbamoylated quinine), trans-1,4-cyclohexylene-bis(carbamoylated-11-dodecylthio-dihydroquinine) and trans-1,4-cyclohexylene-bis(carbamoylated-11-dodecylsulfinyl-dihydroquinine). A series of 24 chiral acids, as various benzoyl, 3,5-dinitrobenzoyl (DNB) and 3,5-dinitrobenzyloxycarbonyl amino acid derivatives were investigated with regards to enantioselectivity employing these different dimeric chiral selectors. The composition of the background electrolyte was 12.5 mM ammonia, 100 mM octanoic acid, and 10 mM chiral selector in an ethanol-methanol (60:40, v/v) mixture and the enantioseparations were performed at 15 degreesC and in the reversed polarity mode at -25 kV. With these dimeric chiral selectors, higher enantioselectivity values, compared to those obtained with monomeric derivatives, were usually achieved, especially with the dimers containing dodecyl substituents. For example, an a value of 4 and a resolution value of 78 were obtained for DNB-phenylalanine, using trans-1,4-cyclohexylene-bis(carbamoylated-11-dodecylthio-dihydroquinine) as selector. (C) 2002 Elsevier Science B.V. All rights reserved. [less ▲]

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See detailEnantiomeric Separation of Pirlindole by Liquid Chromatography Using Different Types of Chiral Stationary Phases
Ceccato, Attilio ULg; Hubert, Philippe ULg; De Tullio, Pascal ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (1998), 18(4-5), 605-14

The enantioseparation of pirlindole by liquid chromatography (LC) was investigated using three different chiral stationary phases (CSPs) containing either cellulose tris-(3,5-dimethylphenylcarbamate ... [more ▼]

The enantioseparation of pirlindole by liquid chromatography (LC) was investigated using three different chiral stationary phases (CSPs) containing either cellulose tris-(3,5-dimethylphenylcarbamate) (Chiralcel OD-R), ovomucoid (OVM) or beta-cyclodextrin (beta-CD). The effects of the mobile phase pH on retention, enantioselectivity and resolution were studied. Methanol and acetonitrile were tested as organic modifiers while the influence of the addition to the mobile phase of sodium alkanesulfonates or sodium perchlorate was also investigated. Sodium perchlorate was only used on the Chiralcel OD-R column while sodium alkanesulfonates were tested as mobile phase additives on the three kinds of CSPs. The enantioseparation of pirlindole could be obtained on all CSPs tested, the best results with respect to chiral resolution being achieved on the Chiralcel OD-R and the OVM columns. The use of sodium octanesulfonate (NaOS) was found to improve the enantioseparation of pirlindole on the OVM column while enantioselectivity was considerably enhanced by addition of sodium perchlorate on the Chiralcel OD-R column. [less ▲]

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See detailEnantiomeric separations by capillary electrophoresis applications in pharmaceutical, biomedical and environmental analysis, chapitre #L-7
Crommen, Jacques ULg; Fillet, Marianne ULg; Bechet, Isabelle et al

in Buszewski, B. (Ed.) New analytical methods for environmental control and monitoring (1995)

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