References of "Hubert, Philippe"
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See detailMonitoring of anatabine release by methyl jasmonate elicited BY-2 cells using surface-enhanced Raman scattering
De Bleye, Charlotte ULg; Dumont, Elodie ULg; Dispas, Amandine ULg et al

in Talanta (2016), 160

A new application of surface-enhanced Raman scattering (SERS) in the field of plant material analysis is proposed in this study. The aim was to monitor the release of anatabine by methyl jasmonate (MeJa ... [more ▼]

A new application of surface-enhanced Raman scattering (SERS) in the field of plant material analysis is proposed in this study. The aim was to monitor the release of anatabine by methyl jasmonate (MeJa) elicited Bright Yellow-2 (BY-2) cells. Gold nanoparticles (AuNps) were used as SERS substrate. The first step was to study the SERS activity of anatabine in a complex matrix comprising the culture medium and BY-2 cells. The second step was the calibration. This one was successfully performed directly in the culture medium in order to take into account the matrix effect, by spiking the medium with different concentrations of anatabine, leading to solutions ranging from 250 to 5000 µg L-1. A univariate analysis was performed, the intensity of a band situated at 1028 cm-1, related to anatabine, was plotted against the anatabine concentration. A linear relationship was observed with a R2 of 0.9951. During the monitoring study, after the MeJa elicitation, samples were collected from the culture medium containing BY-2 cells at 0, 24h, 48h, 72h and 96h and were analyzed using SERS. Finally, the amount of anatabine released in the culture medium was determined using the response function, reaching a plateau after 72h of 82 µg of anatabine released / g of fresh weight (FW) MeJa elicited BY-2 cells. [less ▲]

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See detailA simple calibration approach based on film-casting for confocal Raman microscopy to support the development of a Hot-Melt Extrusion process
Netchacovitch, Lauranne ULg; Thiry, Justine ULg; De Bleye, Charlotte ULg et al

in Talanta (2016), 154

When developing a new formulation, the development, calibration and validation steps of analytical methods based on vibrational spectroscopy are time-consuming. For each new formulation, real samples must ... [more ▼]

When developing a new formulation, the development, calibration and validation steps of analytical methods based on vibrational spectroscopy are time-consuming. For each new formulation, real samples must be produced and a “reference method” must be used in order to determine the Active Pharmaceutical Ingredient (API) content of each sample. To circumvent this issue, the paper presents a simple approach based on the film-casting technique used as a calibration tool in the framework of hot-melt extrusion process. Confocal Raman microscopic method was successfully validated for the determination of itraconazole content in film-casting samples. Then, hot-melt extrusion was carried out to produce real samples in order to confront the results obtained with confocal Raman microscopy and Ultra High Performance Liquid Chromatography (UHPLC). The agreement between both methods was demonstrated using a comparison study based on the Bland and Altman’s plot. [less ▲]

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See detailMOISTURE CONTENT DETERMINATION OF FREEZE-DRIED PRODUCTS BY NEAR-INFRARED SPECTROSCOPY: A CASE STUDY FOR UNIVERSAL REGRESSION MODEL
Clavaud, Matthieu ULg; Roggo, Yves; Degardin, Klara et al

Poster (2016, June 06)

Karl Fischer titration is the reference method for moisture content determination in the pharmaceutical industry. Near-infrared spectroscopy is considered the most suitable alternative technique. Indeed ... [more ▼]

Karl Fischer titration is the reference method for moisture content determination in the pharmaceutical industry. Near-infrared spectroscopy is considered the most suitable alternative technique. Indeed, NIRS is a safe and fast method which does not require sample preparation. Nevertheless, the development and validation phases are time-consuming. In addition, the NIRS methods presented so far were mostly product specific. The main objective of this study is to highlight that an universal calibration model can be validated for several freeze-dried products in order to speed up the validation time. This objective was led in two steps. A universal model was first evaluated. A calibration set and a validation set were built up with three freeze-dried products. An antibody drug conjugate, a large molecule and a small molecule all packed in sealed vials were used to introduce more variability. Regression methods were then compared in order to optimize the prediction values. [less ▲]

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See detailScreening study of SFC critical method parameters for the determination of pharmaceutical compounds
Dispas, Amandine ULg; Lebrun, Pierre ULg; Sacre, Pierre-Yves ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (2016), 125

Nowadays, supercritical fluid chromatography is commonly presented as a promising alternative technique in the field of separation sciences. Nevertheless the selection of chromatographic conditions and ... [more ▼]

Nowadays, supercritical fluid chromatography is commonly presented as a promising alternative technique in the field of separation sciences. Nevertheless the selection of chromatographic conditions and sample preparation of pharmaceutical compounds remain a challenge and peak distortion was previously highlighted. The main objective of the present work was to evaluate the impact of different critical method parameters (CMPs), i.e. stationary phase, mobile phase composition and injection solvent nature. The experiments were performed considering two groups of antimalarial molecules: one group with neutral/apolar compounds and the other one with salt form of polar compounds. In this context, another objective was to propose a suitable sample solvent for quantitative analysis. The interest of new generation stationary phase to obtain good peak shape and the interest to tune the mobile phase composition were demonstrated. During this study, design of experiments and desirability function approach enabled to highlight optimal chromatographic conditions in order to maximise peak capacity and to get acceptable value of symmetry factor. Regarding sample injection solvent composition, some counterintuitive results were observed: solvents closer to the mobile phase polarity (i.e heptane or 2-propanol/heptane mixture) did not provide best results in terms of peak symmetry. In addition, acetonitrile and short aliphatic alcohols offered an interesting alternative as injection solvent: toxicity of solvents used is clearly reduced and better quantitative performances could be expected while keeping high peak capacity and symmetric sharp peaks. Finally, the quantitative performances were evaluated by the method validation for the quantitative determination of quinine sulfate in a pharmaceutical formulation. These better understandings on critical method parameters led SFC to be an even more promising technique in the field of the analysis of pharmaceutical compounds. [less ▲]

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See detailMédicaments usage de faux
Sacre, Pierre-Yves ULg; Ziemons, Eric ULg; Hubert, Philippe ULg et al

Article for general public (2016)

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See detailImplementing principles of Quality by Design (QbD) in validation context
Hubert, Cédric ULg; Lebrun, Pierre ULg; Rozet, Eric et al

Conference (2016, May 10)

Analytical method performances have to be specified by the analyst trough the definition of the “Analytical Target Profile (ATP)”, as proposed by the regulatory bodies. In the specific context of the ... [more ▼]

Analytical method performances have to be specified by the analyst trough the definition of the “Analytical Target Profile (ATP)”, as proposed by the regulatory bodies. In the specific context of the pharmaceutical industry, regulatory authorities have recently imposed the assessment and management of risk throughout the entire product lifecycle. This includes the analytical procedure and consequently its own lifecycle. The development step of an analytical method is still largely addressed using a “Changing One Separate Factor a Time (COST)” approach (also known as the “Quality-by-Testing (QbT)” approach). This strategy can lead to a suitable method for assessing the risk of routine use, even where the experimental domain is not examined. However, in order to consider an experimental domain rather than a set of specific experimental conditions during the development phase, a multivariate approach must be considered: the “Quality-by-Design (QbD)” strategy. This strategy allows the definition of a “Design Space (DS)” by means of design of experiments (DoE). This DS, computed considering critical method parameters, allows the analyst to focus on the main objective of an analytical method: obtaining reliable results using a robust method. In the course of a specific case study, the benefits of the QbD strategy in terms of managing the qualitative part of the analytical process were highlighted. Working in the context of analytical procedure, the validation step is a major part of the analytical method lifecycle. Indeed, the objective of analytical method validation is to demonstrate that this method is suited for quantifying the target analytes with an established and suitable level of accuracy, as defined by the “ATP”. This is sometimes called the “fit-for-future-purpose” concept. The decision regarding the validity of a method based on prediction can be achieved by using the “β-expectation tolerance interval” (accuracy profile). The capability of this approach to manage the quantitative part of the analytical procedure is nowadays largely illustrated in scientific literatures. Considering the assessment and management of risk throughout the analytical lifecycle, a global strategy allowing the unification of the development and validation phases in a single step was considered. With this innovative approach, a strategy allowing the management of global analytical risk (i.e., for both qualitative and quantitative part of the analytical method) was proposed. Indeed, the developed strategy allows validating an entire experimental domain by means of the accuracy profile rather than a single set of specific experimental conditions. With this strategy, the DS is no longer simply the place where qualitative performances are obtained, but also the space where quantitative performances of the analytical procedure are assessed and managed. [less ▲]

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See detailFrom Near-Infrared and Raman to Surface-Enhanced Raman Spectroscopy: Progress, Limitations, Perspectives in Bioanalysis
Dumont, Elodie ULg; De Bleye, Charlotte ULg; Sacre, Pierre-Yves ULg et al

in Bioanalysis (2016), 8(10), 1077-1103

Over recent decades, spreading environmental concern entailed the expansion of green chemistry analytical tools. Vibrational spectroscopy, belonging to this class of analytical tool, is particularly ... [more ▼]

Over recent decades, spreading environmental concern entailed the expansion of green chemistry analytical tools. Vibrational spectroscopy, belonging to this class of analytical tool, is particularly interesting taking into account its numerous advantages such as fast data acquisition and no sample preparation. In this context, Near-Infrared, Raman and mainly Surface-Enhanced Raman Spectroscopy (SERS) have thus gained interest in many fields including bioanalysis. The two former techniques only ensure the analysis of concentrated compounds in simple matrices, whereas the emergence of SERS improved the performances of vibrational spectroscopy to very sensitive and selective analyses. Complex SERS substrates were also developed enabling biomarker measurements, paving the way for SERS immunoassays. Therefore, in this paper, the strengths and weaknesses of these techniques will be highlighted with a focus on recent progress. [less ▲]

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See detailModélisation du comportement chromatographique en SFC
Andri, Bertyl ULg; Dispas, Amandine ULg; Hubert, Philippe ULg et al

Conference (2016, January 21)

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See detailOverview of the Analytical Lifecycle of Supercritical Fluid Chromatography Methods
Andri, Bertyl ULg; Dispas, Amandine ULg; Marini Djang'Eing'A, Roland ULg et al

in American Journal of Analytical Chemistry (2016), 7

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See detailPoplar-root-knot nematode interaction: a model for perennial woody species
Baldacci-Cresp, Fabien; Sacre, Pierre-Yves ULg; Twyffels, Laure et al

in Molecular Plant-Microbe Interactions [=MPMI] (2016), 29(7), 560-572

Plant root-knot nematode interaction studies are performed on several host plant models. However, even though root-knot nematodes interact with trees, no perennial woody model has been explored so far. We ... [more ▼]

Plant root-knot nematode interaction studies are performed on several host plant models. However, even though root-knot nematodes interact with trees, no perennial woody model has been explored so far. We show here that poplar (Populus tremula x Populus alba) grown in vitro is susceptible to Meloidogyne incognita as this nematode is able to penetrate, to induce feeding sites and to reproduce in poplar roots. As analyzed by Raman spectromicroscopy, the cell walls of the giant cells, with typical characteristics of transfer cell walls, were not lignified and were composed mainly of pectin and cellulose. To better depict the poplar-nematode interaction at the molecular level, a quantitative RT-PCR analysis was performed to study changes in poplar gene expression in galls compared to non-infected roots. Three marker genes, reported for other plant hosts, including expansin A, histone 3.1 and asparagine synthase, were conserved for poplar-nematode interaction. In addition, the down-regulation of four genes coding for enzymes of the lignin biosynthesis pathway was evidenced in galls, suggesting a modification in lignin composition within galls developed in poplar roots. Together, this study shows that poplar is a suitable model host for specific traits of tree-nematode interaction. [less ▲]

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See detailAnalytical Tools and Strategic Approach to Detect Poor Quality Medicines, Identify Unknown Components, and Timely Alerts for Appropriate Measures: Case Study of Antimalarial Medicines
Habyalimana, Védaste ULg; Mbinze Kindenge, Jérémie; Kalenda Tshilombo, Nicodème ULg et al

in American Journal of Analytical Chemistry (2015), 6

Nowadays, the circulation of poor quality medicines is becoming an alarming worldwide phenomenon with serious public health and socio-economic concerns. The situation is particularly critical in ... [more ▼]

Nowadays, the circulation of poor quality medicines is becoming an alarming worldwide phenomenon with serious public health and socio-economic concerns. The situation is particularly critical in developing countries where drug quality assurance and regulatory systems for drug manufacturing, importation, distribution and sales are weak. A sustained vigilance on poor quality medicines that regroup counterfeit/falsified, substandard and degraded medicines is therefore required to ensure patient safety and genuine medicines integrity. A case situation is illustrated including a strategic approach and analytical tools that were found useful to detect poor quality medicines, identify unknown components, and timely alerts for appropriate measures against the spread of those harmful products. Several suspected medicines randomly sampled in several strategic Rwandan areas were firstly check-controlled by means of visual inspection and then applying several analytical techniques from simple to more complex ones. The following medicines were studied: quinine sulfate tablets, artemisinin-based combination tablets, and artesunate powders for injection. Taking into account the pharmaceutical forms and the chemical characteristics, the following tests were applied: uniformity of mass, friability, disintegration, fluorescence, identification and assay. They were followed by more complex analytical techniques that allowed more comprehension of abnormal findings among which the presence of a wrong active pharmaceutical ingredient in quinine sulfate tablets which is mainly discussed in this paper to illustrate a strategic approach and various analytical tools that can be used in detecting and identifying unknown component in poor quality medicines. [less ▲]

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