References of "Rozet, Eric"
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See detailTransfert des méthodes analytiques
Rozet, Eric ULg; Hubert, Philippe ULg

Learning material (2010)

Un transfert analytique est un processus complet qui consiste à transférer physiquement une méthode analytique préalablement validée d’un laboratoire émetteur à un laboratoire receveur mais aussi et ... [more ▼]

Un transfert analytique est un processus complet qui consiste à transférer physiquement une méthode analytique préalablement validée d’un laboratoire émetteur à un laboratoire receveur mais aussi et surtout à s’assurer que ce dernier maîtrise cette méthode dans son environnement. Ces transferts de méthodes analytiques sont pleinement inclus dans le développement de nouveaux produits chimiques, pharmaceutiques, cosmétiques, agroalimentaires… En effet, la progression des produits de R&D vers les opérations industrielles et leur commercialisation nécessite le transfert des méthodes de contrôle de production. D’autre part, des contraintes socio-économiques particulières impliques le transfert de méthodes analytiques, telles que la rationalisation des sites de fabrication, la sous-traitance analytique, les achats/ventes de produits en cours de développement et la consolidation/fusion des groupes pharmaceutiques. [less ▲]

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See detailAllocation of ECD Kidneys Based on Donor GFR: The Choice of the Estimating Equation Matters
Delanaye, Pierre ULg; Rozet, Eric ULg; Maillard, N. et al

in American Journal of Transplantation (2010), 10(6), 1493-1494

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See detailAcetaminophen determination in low-dose pharmaceutical syrup by NIR spectroscopy
Ziemons, Eric ULg; Mantanus, Jérôme ULg; Lebrun, Pierre ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (2010), 53

The aim of the present study was first to develop a robust near infrared (NIR) calibration model able to determine the acetaminophen content of a low-dose syrup formulation (2 % (w/v)). Therefore ... [more ▼]

The aim of the present study was first to develop a robust near infrared (NIR) calibration model able to determine the acetaminophen content of a low-dose syrup formulation (2 % (w/v)). Therefore, variability sources such as production campaigns, batches, API concentration, syrup basis, operators and sample temperatures were introduced in the calibration set. A prediction model was then built using Partial Least Square (PLS) regression. First derivative followed by Standard Normal Variate (SNV) were chosen as signal pre-processing. Based on the random subsets cross validation, 4 PLS factors were selected for the prediction model. The method was then validated for an API concentration ranging from 16 to 24 mg/mL (1.6-2.4 % (w/v)) using an external validation set. The 0.26 mg/mL RMSEP suggested the global accuracy of the model. The accuracy profile obtained from the validation results, based on tolerance intervals, confirmed the adequate accuracy of the results generated by the method all over the investigated API concentration range. Finally, the NIR model was used to monitor in real time the API concentration while mixing syrups containing various amounts of API, a good agreement was found between the NIR method and the theoretical concentrations. [less ▲]

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See detailTotal Error Concept in Validation of Viral Activity in Cell Cultures
Gibein, N.; Rozet, Eric ULg

Conference (2010)

Due to the high variability inherent of experimental recipients, validating biological methods is often a complex exercise, and following ICH Q2R1 recommendations is not always feasible and/or meaningful ... [more ▼]

Due to the high variability inherent of experimental recipients, validating biological methods is often a complex exercise, and following ICH Q2R1 recommendations is not always feasible and/or meaningful. Linking systematic error and random error to obtain a unique criterion, as defined in ISO guideline, could be of interest to capture the total variability in biological assays. In this paper, the use of Total Error concept in the validation of biological assays was for the first time investigated and compared to a conventional interpretation of the ICH guideline. Both decision methodologies concluded that the assaywas valid from 2.13 to 5.83 log10(CCID50/ml). However, only the Total Error approach using accuracy profile as decision tool allowed to guarantee that accurate and reliable results will be obtained during the future routine application of the assay. In addition, the risk to obtain out of acceptance limits results was estimated using this approach and was found out to be at the most 3.1% irrespective of the concentration level, thus demonstrating the reliability of the biological assay. [less ▲]

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See detailDevelopment and validation of a sensitive solid phase extraction/hydrophilic interaction liquid chromatography/mass spectrometry method for the accurate determination of glucosamine in dog plasma.
Hubert, Cédric ULg; Houari, Sabah ULg; Lecomte, Frédéric ULg et al

in Journal of Chromatography. A (2010), 1217

A sensitive and accurate LC/MS method was developed for the monitoring of glucosamine (GLcN) dog plasmatic concentration. In this scope, relatively low plasmatic concentrations of GLcN were expected ... [more ▼]

A sensitive and accurate LC/MS method was developed for the monitoring of glucosamine (GLcN) dog plasmatic concentration. In this scope, relatively low plasmatic concentrations of GLcN were expected, ranging from 50 to 1000ng/mL. Liquid chromatography coupled to simple quadrupole mass spectrometry detection (LC/MS) was selected bringing the selectivity and the sensitivity needed for this application. Additionally, a solid phase extraction (SPE) step was performed to reduce matrix and ion suppression effects. Due to the ionisable character of the compound of interest, a mixed-mode strong cation exchange (Plexa PCX) disposable extraction cartridge (DEC) was selected. The separation was carried out on a Zorbax SB-CN column (5mum, 4.6mm i.d.x250mm), considering hydrophilic interaction liquid chromatography (HILIC). Indeed, the mobile phase was made of methanol and 5mM ammonium hydrogen carbonate buffer at pH 7.5 (95/5, v/v). The detection was led at m/z ratios of 180.0 and 417.0, for GLcN and IS, respectively. Reliability of the results was demonstrated through the validation of the method using an approach based on the accuracy profile allowing managing the risk associated to the use of these methods in routine analysis: it is thus guaranteed that each future result will fall in the +/-30% acceptance limits with a probability of at least 90%. Successful application of the method to a preliminary pharmacokinetic study illustrated the usefulness of the method for pre-clinical studies. [less ▲]

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See detailValidation of a method for the quantitation of ghrelin and unacylated ghrelin by HPLC.
Rozet, Eric ULg; Staes, Edith; Ucakar, Bernard et al

in Journal of Pharmaceutical & Biomedical Analysis (2010), 51(3), 633-9

An HPLC/UV method was first optimized for the separation and quantitation of human acylated and unacylated (or des-acyl) ghrelin from aqueous solutions. This method was validated by an original approach ... [more ▼]

An HPLC/UV method was first optimized for the separation and quantitation of human acylated and unacylated (or des-acyl) ghrelin from aqueous solutions. This method was validated by an original approach using accuracy profiles based on tolerance intervals for the total error measurement. The concentration range that achieved adequate accuracy extended from 1.85 to 59.30microM and 1.93 to 61.60microM for acylated and unacylated ghrelin, respectively. Then, optimal temperature, pH and buffer for sample storage were determined. Unacylated ghrelin was found to be stable in all conditions tested. At 37 degrees C acylated ghrelin was stable at pH 4 but unstable at pH 7.4, the main degradation product was unacylated ghrelin. Finally, this validated HPLC/UV method was used to evaluate the binding of acylated and unacylated ghrelin to liposomes. [less ▲]

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See detailCritical analysis of several analytical method validation strategies in the framework of the fit for purpose concept.
Rozet, Eric ULg; Bouabidi, A.; Fillet, Marianne ULg et al

in Journal of Chromatography. A (2010), 1217

Analytical method validation is a mandatory step at the end of the development in all analytical laboratories. It is a highly regulated step of the life cycle of a quantitative analytical method. However ... [more ▼]

Analytical method validation is a mandatory step at the end of the development in all analytical laboratories. It is a highly regulated step of the life cycle of a quantitative analytical method. However, even if some documents have been published there is a lack of clear guidance for the methodology to follow to adequately decide when a method can be considered as valid. This situation has led to the availability of several methodological approaches and it is therefore the responsibility of the analyst to choose the best one. The classical decision processes encountered during method validation evaluation are compared, namely the descriptive, difference and equivalence approaches. Furthermore a validation approach using accuracy profile computed by means of beta-expectation tolerance interval and total measurement error is also available. In the present paper all of these different validation approaches were applied to the validation of two analytical methods. The evaluation of the producer and consumer risks by Monte Carlo simulations were also made in order to compare the appropriateness of these various approaches. The classical methodologies give rise to inadequate and contradictory conclusions which do not allow them to answer adequately the objective of method validation, i.e. to give enough guarantees that each of the future results that will be generated by the method during routine use will be close enough to the true value. It is found that the validation methodology which gives the most guarantees with regards to the reliability or adequacy of the decision to consider a method as valid is the one based on the use of the accuracy profile. [less ▲]

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See detailValidation of a fast gas chromatographic method for the study of semiochemical slow release formulations
Rozet, Eric ULg; Heuskin, Stéphanie ULg; Lorge, Stéphanie et al

in Journal of Pharmaceutical & Biomedical Analysis (2010), 53

The validation of a fast GC-FID analytical method for the quantitative determination of semiochemical sesquiterpenes (E-β-farnesene and β-caryophyllene) to be used in an integrated pest management ... [more ▼]

The validation of a fast GC-FID analytical method for the quantitative determination of semiochemical sesquiterpenes (E-β-farnesene and β-caryophyllene) to be used in an integrated pest management approach is described. Accuracy profiles using total error as decision criteria for validation were used to verify the overall accuracy of the method results within a well defined range of concentrations and to determine the lowest limit of quantification for each analyte. Furthermore it allowed to select a very simple and reliable regression model for calibration curve for the quantification of both analytes as well as to provide measurement uncertainty without any additional experiments. Finally, this validated method was used for the quantification of semiochemicals in slow release formulations. The goal was to verify the protection efficiency of alginate gel beads formulations against oxidation and degradation of sesquiterpenes. The results showed that the alginate beads are adequate slow release devices which protect the bio-active molecules during at least twenty days. [less ▲]

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See detailSuggested mechanism of action of classical and deformable liposomes through pig ear skin
Gillet, Aline ULg; Lecomte, Frédéric ULg; Rozet, Eric ULg et al

in Journal of Pharmacy & Pharmacology (2010), 62(6), 788-807

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See detailActive content determination of non-coated pharmaceutical pellets by near infrared spectroscopy: Method development, validation and reliability evaluation
Mantanus, Jérôme ULg; Ziemons, Eric ULg; Lebrun, Pierre ULg et al

in Talanta (2010), 80

A robust near infrared (NIR) method able to quantify the active content of pilot non-coated pharmaceutical pellets was developed. A protocol of calibration was followed, involving 2 operators, independent ... [more ▼]

A robust near infrared (NIR) method able to quantify the active content of pilot non-coated pharmaceutical pellets was developed. A protocol of calibration was followed, involving 2 operators, independent pilot batches of non-coated pharmaceutical pellets and two different NIR acquisition temperatures. Prediction models based on Partial Least Squares (PLS) regression were then carried out. Afterwards, the NIR method was fully validated for an active content ranging from 80 to 120% of the usual active content using new independent pilot batches to evaluate the adequacy of the method to its final purpose. Conventional criteria such as the R2, the Root Mean Square Error of Calibration (RMSEC), the Root Mean Square Error of Prediction (RMSEP) and the number of PLS factors enabled the selection of models with good predictive potential. However, such criteria sometimes fail to choose the most fitted for purpose model. Therefore, a novel approach based on accuracy profiles of the validation results was used, providing a visual representation of the actual and future performances of the models. Following this approach, the prediction model using signal pre-treatment Multiplicative Scatter Correction (MSC) was chosen as it showed the best ability to quantify accurately the active content over the 80–120% active content range. The reliability of the NIR method was tested with new pilot batches of non-coated pharmaceutical pellets containing 90 and 110% of the usual active content, with blends of validation batches and industrial batches. All those batches were also analyzed by the HPLC reference method and relative errors were calculated: the results showed low relative errors in full accordance with the results obtained during the validation of the method, indicating the reliability of the NIR method and its interchangeability with the HPLC reference method. [less ▲]

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See detailSimultaneous quantification os asiaticoside, asiatic acid, madecassoside and madecassic acid in leaves of Centella asiatica (L.) urb.
Rafamantanana, M. H.; Rozet, Eric ULg; Raoelison, G. E. et al

Poster (2010)

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See detailL'erreur totale pour le transfert de méthodes
Rozet, Eric ULg

Conference (2010)

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See detailBuilding the quality into pellet manufacturing environment - feasibility study and validation of an in-line quantitative near infrared (NIR) method
Mantanus, Jérôme ULg; Ziemons, Eric ULg; Rozet, Eric ULg et al

in Talanta (2010), 83

The present study focuses on the implementation of an in-line quantitative near infrared (NIR) spectroscopic method for determining the active content of pharmaceutical pellets. The first aim was to non ... [more ▼]

The present study focuses on the implementation of an in-line quantitative near infrared (NIR) spectroscopic method for determining the active content of pharmaceutical pellets. The first aim was to non-invasively interface a dispersive NIR spectrometer with four realistic particle streams existing in the pellets manufacturing environment. Regardless of the particle stream characteristics investigated, NIR together with principal component analysis (PCA) was able to classify the samples according to their active content. Further, one of these particle stream interfaces was non-invasively investigated with a FT-NIR spectrometer. A predictive model based on Partial Least Squares (PLS) regression was able to determine the active content of pharmaceutical pellets. The NIR method was finally validated with an external validation set for an API concentration range from 80 to 120 % of the targeted active content. The prediction error of 0.9 % (root mean standard error of prediction, RMSEP) was low, indicating the accuracy of the NIR method. The accuracy profile on the validation results, an innovative approach based on tolerance intervals, demonstrated the actual and future performance of the in-line NIR method. Accordingly, the present approach paves the way for real-time release-based quality system. [less ▲]

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See detailUrinary NGAL: Use of absolute value or ratio to creatinine?
Cavalier, Etienne ULg; Bekaert, Anne-Catherine ULg; Legrand, Delphine ULg et al

in Acta Clinica Belgica (2010), 65-3

Introduction: Neutrophil gelatinase-associated lipocalin (NGAL) has emerged as a promising marker for the detection of acute kidney injury. This marker has been proposed for urinary measurement. However ... [more ▼]

Introduction: Neutrophil gelatinase-associated lipocalin (NGAL) has emerged as a promising marker for the detection of acute kidney injury. This marker has been proposed for urinary measurement. However, in the literature, authors indistinctly use "absolute" value or NGAL to creatinine ratio. Up to now, there are no strong arguments favouring for one. This question is of importance as this marker is sensed to be used only on urine random samples. To find an answer to this very practical matter, one approach could be to compare biological CV(intra-individual variation) of the "absolute" and ratio results. [less ▲]

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See detailA double-cartridge SPE-HPLC-UV method for monitoring a humanfriendly anticancer in plasma: Ketoglutarate levels in metastatic carcinoma
Michail, K.; Rozet, Eric ULg; Hubert, Philippe ULg et al

Poster (2010)

We present a fully validated HPLC-UV assay for the concurrent quantification of ketoglutaric acid and hydroxymethylfurfural, a ‘targeted therapy’ composition inducing a synergistic metabolic distress to ... [more ▼]

We present a fully validated HPLC-UV assay for the concurrent quantification of ketoglutaric acid and hydroxymethylfurfural, a ‘targeted therapy’ composition inducing a synergistic metabolic distress to the tumoral microenvironment. The analytes were exclusively extracted from the biomatrix via a combined-cartridge solid phase extraction assembly. The method is based on derivatizing both analytes with 2-nitrophenylhydrazine directed to their chemically divergent but commonly occurring carbonyl function. The reaction is kinetically catalyzed. Acidifying the buffered eluate post-extraction is critical for the feasibility of the reaction. The chromatographic separation is successfully accomplished on octyl columns in less than 15 min at 330 nm using 0.028% TFAA-methanol-acetonitrile (58:32:10, v/v) as eluant. The assay was validated using the concept of accuracy profile. The selectivity of the method was demonstrated in pre- and post-dosed patients from a pilot study. Quality control samples were prepared and analyzed during the routine use of the method. Life samples collected from patients enduring oesophageal and breast carcinoma with lung metastases were monitored for ketoglutarate in a trial to correlate its plasma levels with the malignancy. [less ▲]

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See detailEstimation of the Stability of Parathyroid Hormone when Stored at -80°C for a Long Period
Cavalier, Etienne ULg; Delanaye, Pierre ULg; Hubert, Philippe ULg et al

in Clinical Journal of the American Society of Nephrology (2009), 4(12), 1988-92

Detailed reference viewed: 48 (22 ULg)