References of "Chiap, Patrice"
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See detailGESTION DU RISQUE LORS DU TRANSFERT DE METHODES ANALYTIQUES – CAS D’UNE METHODE BIOANALYTIQUE
Rozet, Eric ULg; Dewe, W.; Morello, R. et al

Conference (2007)

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See detailDevelopment of a mass spectrometry method for the determination of a melanoma biomarker, 5-S-cysteinyldopa, in human plasma using solid phase extraction for sample clean-up.
Martin, Gaëlle ULg; Chiap, Patrice ULg; Paquet, Philippe ULg et al

in Journal of Chromatography. A (2007), 1156(1-2), 141-8

5-S-cysteinyldopa is a well-known pigment intermediate and analysis of its plasma concentration is interesting for the early diagnosis, as well as for evaluation of treatment and follow-up of malignant ... [more ▼]

5-S-cysteinyldopa is a well-known pigment intermediate and analysis of its plasma concentration is interesting for the early diagnosis, as well as for evaluation of treatment and follow-up of malignant melanoma. A determination method of 5-SCD in human plasma was developed using solid phase extraction (SPE) on disposable cartridges and liquid chromatography electrospray mass spectrometry (LC-ESI-MS-MS). Compound's sensitivity to light and oxidation requires the addition of anti-oxidative agents (AO), to work in acidic media at 4 degrees C and to avoid light exposure of samples since blood collection. Different solid phases involving covalent binding to phenylboronic groups or dual retention mechanisms were evaluated and extraction cartridges containing both hydrophobic and strong cation exchange functionalities were finally selected. The LC separation of 5-SCD from endogenous catecholamines was achieved by gradient elution on a C18 stationary phase. 5-SCD was detected by multiple reaction monitoring (MRM) performed on ES(+) generated ions. Finally, the method was prevalidated in the lower ng/ml range. Good results with respect to accuracy, trueness and precision were obtained. [less ▲]

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See detailEvaluation of Analytical Method Transfer on a Risk Based Methodology using Total Error
Rozet, Eric ULg; Dewe, W.; Govaerts, B. et al

Conference (2007)

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See detailPerformances of a multidimensional on-line SPE-LC-ECD method for the determination of three major catecholamines in native human urine: Validation, risk and uncertainty assessments
Rozet, Eric ULg; Morello, Rosa; Lecomte, Frédéric ULg et al

in Journal of Chromatography. B : Analytical Technologies in the Biomedical & Life Sciences (2006), 844(2), 251-260

A novel, multidimensional on-line SPE-LC method with electrochemical detection is described for the fully automated and direct analysis of the catecholamines norepinephrine, epinephrine and dopamine in ... [more ▼]

A novel, multidimensional on-line SPE-LC method with electrochemical detection is described for the fully automated and direct analysis of the catecholamines norepinephrine, epinephrine and dopamine in urine. The integrated extractive clean-up of the raw biofluid is based on a SPE-column packed with restricted access material (RAM) which is modified with the affinity ligand nitrophenylboronic acid. The method was fully validated according to a recent approach based on an accuracy profile. The acceptance limits were set at +/- 15% of the nominal concentration values. The method was found accurate over a concentration range from 15 to 500 mu g/l for norepinephrine, from 5 to 500 mu g/l for epinephrine and from 50 to 500 mu g/l for dopamine. The relative risk for the use of the validated method in routine analysis was also assessed based on this validation strategy. It was found that at most 3.5% of future sample measurements will fall outside the acceptance limits. This demonstrates the high reliability of the analytical method described. Moreover, the measurements uncertainties were deduced from the validation experiments without any additional effort. (c) 2006 Elsevier B.V. All rights reserved. [less ▲]

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See detailThe transfer of a LC-UV method for the determination of fenofibrate and fenofibric acid in Lidoses: Use of total error as decision criterion
Rozet, Eric ULg; Mertens, Bénédicte; Dewé, Walthère ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (2006), 42(1), 64-70

Two new statistical approaches to assess the validity of the transfer of a LC-UV method for the determination of fenofibrate and fenofibric acid were investigated and compared to the conventional ... [more ▼]

Two new statistical approaches to assess the validity of the transfer of a LC-UV method for the determination of fenofibrate and fenofibric acid were investigated and compared to the conventional approaches generally used in this domain. These new approaches, namely the Tolerance Interval and the Risk approaches, are based on the simultaneous evaluation of the systematic (or trueness) and random (or precision) errors of the transfer into a single criterion called total error (or accuracy). The results of the transfer showed that only the total error based approaches fulfilled the objective of an analytical method transfer, i.e. to give guarantees that each future measurement made by the receiving laboratory will be close enough to the true value of the analyte in the sample. Furthermore the Risk approach was the most powerful one and allowed the estimation of the risk to have future measurements out of specification in the receiving laboratory, therefore being a risk management tool. (c) 2006 Elsevier B.V. All rights reserved. [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 detailPharmacokinetic study of a new synthetic MMP inhibitor (Ro 28-2653) after IV and oral administration of cyclodextrin solutions
Piette, Marie ULg; Evrard, Brigitte ULg; Frankenne, Francis et al

in European Journal of Pharmaceutical Sciences (2006), 28(3), 189-195

Ro 28-2653 (5-biphenyl-4-yl-5-[4-(4-nitro-phenyl)-piperazin-1-yl]-pyrimidine-2,4,6-trione) is a new synthetic inhibitor of matrix metalloproteinases (MMPs) with a high selectivity towards MMP2, MMP9 and ... [more ▼]

Ro 28-2653 (5-biphenyl-4-yl-5-[4-(4-nitro-phenyl)-piperazin-1-yl]-pyrimidine-2,4,6-trione) is a new synthetic inhibitor of matrix metalloproteinases (MMPs) with a high selectivity towards MMP2, MMP9 and membrane type 1-MMP. It has been shown that cyclodextrins (CDs) are able to form inclusion complexes with Ro 28-2653 and to increase its aqueous solubility. The aim of this study is to demonstrate that an increase in Ro 28-2653 solubility, via ternary complex formation, can lead to an increase in the oral bioavailability of this drug. This study shows that a synergistic effect exists between hydroxypropyl-beta-cyclodextrin (HP-beta-CD) and L-lysine. The use of this multicomponent system enabled the preparation of oral and intravenous solutions of Ro 28-2653. In vivo evaluation of the oral solution of the inclusion complex of Ro 28-2653 in comparison with a suspension of the same uncomplexed drug showed a significant (p < 0.05) increase in absolute bioavailability. The area under curve (AUC) and the peak serum concentration (C-max) were approximately 10 times higher than those obtained with the suspension, while the time (T-max) to reach C-max was reduced. Moreover, in vivo administration of Ro 28-2653 solutions highlighted some information about the pharmacokinetic behavior of Ro 28-2653: a long biologic half-life (about 15.5 h) and a small overall volume of distribution (81). (c) 2006 Elsevier B.V. All rights reserved. [less ▲]

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