References of "Servais, Anne-Catherine"
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See detailCE-MS method development for peptides analysis, especially hepcidin, an iron metabolism marker.
Martin, Gaëlle ULg; Mansion, François ULg; Servais, Anne-Catherine ULg et al

in Electrophoresis (2009), 30(15), 2624-31

A method for the resolution of a peptides mixture including hepcidin-25, an iron metabolism marker, was developed by CE-ESI-MS. Several strategies were tested to optimize peptide separation, such as the ... [more ▼]

A method for the resolution of a peptides mixture including hepcidin-25, an iron metabolism marker, was developed by CE-ESI-MS. Several strategies were tested to optimize peptide separation, such as the addition of cyclodextrins or organic solvents in the BGE or the use of coated capillaries. Best results in terms of resolution, symmetry and efficiency were obtained with a BGE made of 500 mM ammonium acetate pH 4.5/ACN 70:30 v/v. Using the methodology of experimental design, BGE concentration, sheath liquid composition and MS-coupling parameters were then optimized in order to obtain the best signal intensity for hepcidin. Finally, a 225 mM BGE and a sheath liquid composed of isopropanol/water 80:20 v/v containing 0.5% v/v formic acid were selected as it constitutes the best compromise for selectivity, peak shape and sensitivity. [less ▲]

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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 detailValidation of a nonaqueous capillary electrophoretic method for the enantiomeric purity determination of R-flurbiprofen using a single-isomer amino cyclodextrin derivative
Rousseau, Anne ULg; Chiap, Patrice ULg; Ivanyi, Robert et al

in Journal of Chromatography. A (2008), 1204(2), 219-225

Nonaqueous capillary electrophoresis (NACE) was successfully applied to the enantiomeric purity determination of R-flurbiprofen using 6-monodeoxy-6-mono(2-hydroxy)propylamino-beta-cyclodextrin (IPA-beta ... [more ▼]

Nonaqueous capillary electrophoresis (NACE) was successfully applied to the enantiomeric purity determination of R-flurbiprofen using 6-monodeoxy-6-mono(2-hydroxy)propylamino-beta-cyclodextrin (IPA-beta-CD) as chiral selector. The nonaqueous BGE was made up of 20 mM IPA-beta-CD, 20 mM ammonium camphorsulfortate and 40 mM ammonium acetate in methanol. Flufenamic acid was selected as internal standard. The CE method was carefully optimized in order to prevent the adsorption of the cationic CD onto the capillary wall, and therefore, to avoid loss of peak efficiency and enantioresolution. To achieve this goal, the addition of ammonium camphorsulfonate was found to be necessary. In the selected conditions, the determination of 0.1% of S-flurbiprofen in R-flurbiprofen could be performed using the method of standard additions. The NACE method was then fully validated by applying a novel strategy using accuracy profiles. (c) 2008 Elsevier B.V. All rights reserved. [less ▲]

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See detailNonaqueous electrokinetic chromatography-electrospray ionization mass spectrometry using anionic cyclodextrins
Mol, Roelof; Servais, Anne-Catherine ULg; Fillet, Marianne ULg et al

in Journal of Chromatography. A (2007), 1159(1-2), 51-57

The set-up of an on-line method for coupling nonaqueous electrokinetic chromatography (NAEKC) and electrospray ionization mass spectrometry (ESI-MS) is presented. It allows the use of the single-isomer ... [more ▼]

The set-up of an on-line method for coupling nonaqueous electrokinetic chromatography (NAEKC) and electrospray ionization mass spectrometry (ESI-MS) is presented. It allows the use of the single-isomer derivative anionic cyclodextrins heptakis(2,3-di-O-methyl-6-O-sulfo)-beta-cyclodextrin (HDMS-beta-CD) and heptakis(2.3-di-O-acetyl-6-O-sulfo)-beta-cyclodextrin (HDAS-beta-CD) for chiral and achiral separations of positively charged analytes. The effect of the cyclodextrins (CDs) on the MS signal intensities of model compounds was studied. When a voltage is applied over the CE capillary, the overall mobility of the CDs is towards the inlet vial preventing CDs from entering the ion source. However, the sodium counter ions of the CDs still enter the ion source and appeared to cause ionization suppression. Nevertheless, significant analyte signals could still be detected with detection limits in the sub-mu g/ml. System parameters such as sheath liquid composition and flow rate, nebulizing gas pressure, capillary position in the sprayer and the drying gas flow and temperature were studied and optimized. The selection of a relatively low nebulizing gas pressure appeared to be important to achieve optimum sensitivity. The chiral selectivity of the NAEKC-ESI-MS system could be improved by addition of camphorsulfonate to the background electrolyte. Using mixtures of drugs and drug-related compounds, the NAEKC-ESI-MS system is shown to offer potential for (chiral) drug profiling. (c) 2007 Elsevier B.V. All rights reserved. [less ▲]

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See detailNonaqueous capillary electrophoretic behavior of 2-aryl propionic acids in the presence of an achiral ionic liquid - A chemometric approach
Francois, Yannis; Varenne, Anne; Juillerat, Emilie et al

in Journal of Chromatography. A (2007), 1138(1-2), 268-275

Ionic liquids (ILs) appear really attractive as electrolyte additives in nonaqueous capillary electrophoresis (NACE). These salts may offer new possibilities of interactions to modulate analyte effective ... [more ▼]

Ionic liquids (ILs) appear really attractive as electrolyte additives in nonaqueous capillary electrophoresis (NACE). These salts may offer new possibilities of interactions to modulate analyte effective mobilities. The presence of 1-n-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide (BMIM NTf2) in acetonitrile/alcohol background electrolytes (BGEs) was investigated in this work. The aim of this study was to elucidate the influence of the IL concentration on the electrophoretic behavior of four arylpropionic acids and to identify the interactions between the analytes and the 1L cation. The influence on mobility of the IL concentration, the nature and the proportion of the organic solvents, and the concentration of the ionic components of the BGE was first studied by a univariate approach. A four-factor D-optimal experimental design was then applied to provide a deeper insight into analyte interaction with IL cation present both free in BGE and adsorbed onto the capillary wall. (c) 2006 Elsevier B.V. All rights reserved. [less ▲]

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See detailRobustness testing of a chiral NACE method for R-timolol determination in S-timolol maleate and uncertainty assessment from quantitative data.
Marini Djang'Eing'A, Roland ULg; Rozet, Eric ULg; Vanderheyden, Yvan et al

in Journal of Pharmaceutical & Biomedical Analysis (2007), 44(3), 640-51

A robustness test of a capillary electrophoresis method for the chiral separation of timolol in nonaqueous acidified media was performed. A two-level Plackett-Burman design was applied in which one ... [more ▼]

A robustness test of a capillary electrophoresis method for the chiral separation of timolol in nonaqueous acidified media was performed. A two-level Plackett-Burman design was applied in which one qualitative and six quantitative factors were examined. Resolution, migration times and relative migration times to pyridoxine (selected as internal standard) were examined as qualitative responses to evaluate electrophoretic performance. A quantitative response, the content of R-timolol in S-timolol maleate sample, was also considered. Even though some significant factor effects were observed on the qualitative responses, it was still possible to quantify the R-timolol in the S-timolol maleate samples properly. The quantitative response was not significantly affected by the selected factors, demonstrating the robustness of the procedure. However, the use of different HDMS-beta-CD batches seemed to affect both types of responses necessitating to introduce a warning in the procedure. Since the experiments of the Plackett-Burman design can be assimilated to laboratories in an interlaboratory study, uncertainty can be evaluated using the robustness test data. The robustness test was set-up in such a way that the required variances could be estimated. [less ▲]

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See detailEnantiomeric separation of acidic compounds using single-isomer amino cyclodextrin derivatives in nonaqueous capillary electrophoresis
Fradi, Inès; Servais, Anne-Catherine ULg; Pedrini, Matteo et al

in Electrophoresis (2006), 27(17), 3434-3442

The enantiomeric separation of a series of acidic pharmaceuticals (mostly nonsteroidal anti-inflammatory drugs) has been investigated in NACE systems using single-isomer amino beta-CD derivatives. The ... [more ▼]

The enantiomeric separation of a series of acidic pharmaceuticals (mostly nonsteroidal anti-inflammatory drugs) has been investigated in NACE systems using single-isomer amino beta-CD derivatives. The first part of this study consisted of the selection of the basic experimental conditions to separate efficiently the enantiomers of acidic drugs. Several parameters, such as the nature of the ionic BGE components, were studied and a methanolic solution of ammonium acetate containing the cationic CD was selected as BGE. A D-optimal design with 20 experimental points was then applied and the nature and concentration of the CD were found to have a significant effect on the enantiomeric resolution for all studied compounds. Resolution (R(s)) values were always higher with 6-monodeoxy-6-mono(3-hydroxy)propylamino-beta-CD (PA-beta-CD) compared to those obtained with 6-monodeoxy-6-mono(2-hydroxy)propylamino-beta-CD (IPA-beta-CD). However, the latter led to shorter migration times. Generic NACE conditions were then selected by means of the multivariate approach in order to obtain the highest R(s) values in a minimum amount of time. Finally, dependence of separation selectivity, resolution, as well as mobility difference on chiral selector concentration was discussed and binding constants with PA-beta-CD were estimated for the two enantiomers of one of the model compounds, suprofen in these NACE systems. [less ▲]

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See detailCapillary electrophoresis-mass spectrometry, an attractive tool for drug bioanalysis and biomarker discovery
Servais, Anne-Catherine ULg; Crommen, Jacques ULg; Fillet, Marianne ULg

in Electrophoresis (2006), 27(13), 2616-2629

The coupling of CE with MS detection, a relatively recent hyphenated technique, has gained increasing respect in the field of bioanalytical applications over the past few years. The first part of this ... [more ▼]

The coupling of CE with MS detection, a relatively recent hyphenated technique, has gained increasing respect in the field of bioanalytical applications over the past few years. The first part of this review presents CE-MS applications dealing with drug bioanalysis, including forensic analysis and metabolism studies. Practical considerations to achieve a robust and sensitive CE-MS coupling are also presented. It is indeed essential to strictly control some critical electrospray parameters, such as the sheath liquid composition and flow rate, the nebulizing gas pressure as well as the capillary outlet position. The second part of the review critically describes the applications of CE coupled on-line to MS for the identification of biomarkers in body fluids for diagnostic purposes. Since the sample preparation procedures strongly differ according to the intended use (drug bioanalysis or biomarker discovery), they are discussed separately, taking into account the particular properties of plasma and urine matrices. [less ▲]

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