References of "Servais, Anne-Catherine"
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See detailOn-line coupling of cyclodextrin mediated nonaqueous capillary electrophoresis to mass spectrometry for the determination of salbutamol enantiomers in urine
Servais, Anne-Catherine ULg; Fillet, Marianne ULg; Mol, Roelof et al

in Journal of Pharmaceutical & Biomedical Analysis (2006), 40(3), 752-757

The usefulness of the on-line coupling of nonaqueous capillary electrophoresis (NACE) with electrospray ionization (ESI) mass spectrometry (MS) using heptakis(2,3-di-O-acetyl-6-O-sulfo)-beta-cyclodextrin ... [more ▼]

The usefulness of the on-line coupling of nonaqueous capillary electrophoresis (NACE) with electrospray ionization (ESI) mass spectrometry (MS) using heptakis(2,3-di-O-acetyl-6-O-sulfo)-beta-cyclodextrin (HDAS-beta-CD) was demonstrated for the enantioselective determination of low concentrations of salbutamol in human urine. After optimization of several parameters, such as sheath-liquid composition and flow rate, nebulizing gas pressure, CE counter-pressure and position of the CE capillary outlet, a limit of quantification of 18 and 20 ng/ml was obtained for salbutamol enantiomers. Moreover, the relative standard deviation values for repeatability at a concentration of 30 ng/ml were below 7% for both enantiomers. Typical regression lines obtained after application of a simple linear regression model revealed a pod relationship between peak area and analyte concentration (with 0.9988 and 0.9966 as coefficients of determination). This paper proposes an easy to use and sensitive NACE-MS method to determine enantiomers of a basic chiral drug in biological fluids preceded by solid-phase extraction as sample cleanup. (c) 2005 Elsevier B.V. All rights reserved. [less ▲]

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See detailInterlaboratory study of a NACE method for the determination of R-timolol content in S-timolol maleate: assessment of uncertainty.
Marini Djang'Eing'A, Roland ULg; Groom, Carl; Doucet, Francois R et al

in Electrophoresis (2006), 27(12), 2386-99

Analyses of statistical variance were applied to evaluate the precision and practicality of a CD-based NACE assay for R-timolol after enantiomeric separation of R- and S-timolol. Data were collected in an ... [more ▼]

Analyses of statistical variance were applied to evaluate the precision and practicality of a CD-based NACE assay for R-timolol after enantiomeric separation of R- and S-timolol. Data were collected in an interlaboratory study by 11 participating laboratories located in Europe and North America. General qualitative method performance was examined using suitability descriptors (i.e. resolution, selectivity, migration times and S/N), while precision was determined by quantification of variances in the determination of R-timolol at four different impurity levels in S-timolol maleate samples. The interlaboratory trials were designed in accordance with the ISO guideline 5725-2. This allowed estimating for each sample, the different variances, i.e. between-laboratory (s2(Laboratories)), between-day (s2(Days)) and between-replicate (s2(Replicates)). The variances of repeatability (s2r) and reproducibility (s2R) were then calculated. The estimated uncertainty, derived from the precision estimates, seems to be concentration-dependent above a given threshold. This example of R-timolol illustrates how a laboratory can evaluate uncertainty in general. [less ▲]

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See detailNonaqueous capillary electrophoresis method for the enantiomeric purity determination of S-timolol using heptakis(2,3-di-O-methyl-6-O-sulfo)-beta-cyclodextrin: validation using the accuracy profile strategy and estimation of uncertainty.
Marini Djang'Eing'A, Roland ULg; Servais, Anne-Catherine ULg; Rozet, Eric ULg et al

in Journal of Chromatography. A (2006), 1120(1-2), 102-11

Nonaqueous capillary electrophoresis (NACE) was successfully applied to the enantiomeric purity determination of S-timolol maleate using heptakis(2,3-di-O-methyl-6-O-sulfo)-beta-cyclodextrin (HDMS-beta-CD ... [more ▼]

Nonaqueous capillary electrophoresis (NACE) was successfully applied to the enantiomeric purity determination of S-timolol maleate using heptakis(2,3-di-O-methyl-6-O-sulfo)-beta-cyclodextrin (HDMS-beta-CD) as chiral selector. With a background electrolyte made up of a methanolic solution of 0.75 M formic acid, 30 mM potassium camphorsulfonate and containing 30 mM HDMS-beta-CD, the determination of 0.1% of R-timolol in S-timolol could be performed with an enantiomeric resolution of 8.5. Pyridoxine was selected as internal standard. The NACE method was then fully validated by applying a novel strategy using accuracy profiles. It is based on beta-expectation tolerance intervals for the total measurement error which includes trueness and intermediate precision. The uncertainty of measurements derived from beta-expectation tolerance intervals was estimated at each concentration level of the validation standards. To confirm the suitability of the developed and validated method, several real samples of S-timolol maleate containing R-timolol maleate at different concentrations were analysed and the results were compared to those obtained by liquid chromatography. [less ▲]

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See detailInfluence of the nature of the electrolyte on the chiral separation of basic compounds in nonaqueous capillary electrophoresis using heptakis(2,3-di-O-methyl-6-O-sulfo)-beta-cyclodextrin
Servais, Anne-Catherine ULg; Fillet, Marianne ULg; Chiap, Patrice ULg et al

in Journal of Chromatography. A (2005), 1068(1), 143-150

The influence on the enantiomeric resolution of the nature of the cationic BGE component (sodium, ammonium or potassium) and that of the anionic component (chloride, formate, methanesulfonate or ... [more ▼]

The influence on the enantiomeric resolution of the nature of the cationic BGE component (sodium, ammonium or potassium) and that of the anionic component (chloride, formate, methanesulfonate or camphorsulfonate) as well as the concentration of heptakis(2,3-di-O-methyl-6-O-sulfo)-beta-cyclodextrin (HDMS-beta-CD), the selected chiral selector, was studied in nonaqueous capillary electrophoresis (NACE). For this purpose, two D-optimal designs with 33 and 26 experimental points were applied. Three beta-blockers (atenolol, celiprolol and propranolol) and three local anesthetics (bupivacaine, mepivacaine and prilocaine) were selected as basic model compounds. Both cationic and anionic BGE components were found to have a deep impact on the enantiomeric resolution of the investigated analytes but it is the cationic component that has shown the strongest influence. Indeed, in some cases, the change of the latter led to a complete loss of enantioresolution. Based on the observed results, two NACE systems were recommended, namely ammonium formate and potassium camphorsulfonate in a methanolic solution containing HDMS-beta-CD and acidified with formic acid, in order to separate efficiently the enantiomers of basic drugs. (c) 2004 Elsevier B.V. All rights reserved. [less ▲]

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See detailSéparation et dosage de substances médicamenteuses par électrophorèse capillaire en milieu non aqueux : Influence de l’utilisation simultanée d’une cyclodextrine et d’un agent d’appariement d’ions
Servais, Anne-Catherine ULg

Doctoral thesis (2005)

The use of nonaqueous electrolyte solutions in capillary electrophoresis (CE) has made it possible to open up new horizons in the field of drug analysis. The achiral separation of four beta-blockers was ... [more ▼]

The use of nonaqueous electrolyte solutions in capillary electrophoresis (CE) has made it possible to open up new horizons in the field of drug analysis. The achiral separation of four beta-blockers was first investigated in nonaqueous CE (NACE) using the principle of ion-pair formation. Camphorsulfonate was selected as the counter-ion. The influence on resolution of parameters such as the nature and concentration of the counter-ion and the ionic components of the background electrolyte was studied by means of a univariate approach. Experimental designs were then applied to estimate possible quadratic effects and first-order interactions. Finally, the optimal conditions obtained by the univariate and the multivariate approaches were compared. The enantiomeric separation of basic pharmaceuticals was then investigated using an original combination in NACE, namely an ion-pairing reagent together with a cyclodextrin (CD). The simultaneous addition to the methanolic background electrolyte of (+)-S-camphorsulfonate or an alkanesulfonate and an anionic beta-CD derivative, namely heptakis(2,3-di-O-methyl-6-O-sulfo)-beta-CD (HDMS-beta-CD), led to partial or complete enantioresolution in all cases. The influence on the enantioseparation of the nature and concentration of the counter-ion and the anionic CD derivative was studied by means of a univariate approach. In order to understand the effects on the enantiomeric resolution of the simultaneous use of camphorsulfonate and HDMS-b-CD, experimental designs were applied. A fast method development strategy was finally recommended for the enantioseparation of basic drug compounds. The influence on the enantiomeric resolution of the nature of the cationic and anionic background electrolyte components was also studied in the presence of several HDMS-beta-CD concentrations. Both cationic and anionic background electrolyte components were found to have a deep impact on the enantioseparation but it is the cationic component that seems to have the strongest influence. Finally, NACE was successfully applied to the resolution and the determination of salbutamol enantiomers in urine samples using heptakis(2,3-di-O-acetyl-6-O-sulfo)-beta-CD. Solid phase extraction was used for sample clean-up prior to the CE separation. The method was then fully validated using a new approach based on accuracy profiles over a concentration range from 375 to 7500 ng/ml for each enantiomer. [less ▲]

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See detailEvaluation de liquides ioniques chiraux comme sélecteurs pour des séparations électrocinétiques d'énantiomères en veine liquide capillaire
François, Yannis; Juillerat, E.; Villemin, Didier et al

Poster (2005)

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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 detailDetermination of salbutamol enantiomers in human urine using heptakis(2,3-di-O-acetyl-6-O-sulfo)-beta-cyclodextrin in nonaqueous capillary electrophoresis
Servais, Anne-Catherine ULg; Chiap, Patrice ULg; Hubert, Philippe ULg et al

in Electrophoresis (2004), 25(10-11), 1632-1640

Nonaqueous capillary electrophoresis (NACE) was successfully applied to the resolution and the determination of salbutamol enantiomers in urine samples using heptakis(2,3-di-O-acetyl-6-O-sulfo)-beta ... [more ▼]

Nonaqueous capillary electrophoresis (NACE) was successfully applied to the resolution and the determination of salbutamol enantiomers in urine samples using heptakis(2,3-di-O-acetyl-6-O-sulfo)-beta-cyclodextrin (HDAS-beta-CD). After optimization of the electrophoretic parameters, namely the background electrolyte (BGE) composition and the HDAS-beta-CD concentration, salbutamol enantiomers were completely resolved using a BGE made up of 10 mm ammonium formate and 15 mm HDAS-beta-CD in methanol acidified with 0.75 M formic acid. Isoprenaline was selected as internal standard. Solid-phase extraction (SPE) was used for sample cleanup prior to the CE separation. Different sorbents involving polar, nonpolar interactions or dual retention mechanisms were evaluated and extraction cartridges containing both nonpolar and strong cation-exchange functionalities were finally selected. Salbutamol enantiomers recoveries from urine samples were determined. The method was then successfully validated using a new approach based on accuracy profiles over a concentration range from 375 to 7500 ng/mL for each enantiomer. [less ▲]

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