References of "Sacre, Pierre-Yves"
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See detailGlobal regression model for moisture content determination using near-infrared spectroscopy
Clavaud, Matthieu ULiege; Roggo, Yves; Degardin, Klara et al

in European Journal of Pharmaceutics and Biopharmaceutics (2017), 119

Near-infrared (NIR) global quantitative models were evaluated for the moisture content (MC) determination of three different freeze-dried drug products. The quantitative models were based on 3822 spectra ... [more ▼]

Near-infrared (NIR) global quantitative models were evaluated for the moisture content (MC) determination of three different freeze-dried drug products. The quantitative models were based on 3822 spectra measured on two identical spectrometers to include variability. The MC, measured with the reference Karl Fischer (KF) method, were ranged from 0.05% to 4.96%. Linear and non-linear regression models using Partial Least Square (PLS), Decision Tree (DT), Bayesian Ridge Regression (Bayes-RR), K-Nearest Neighbors (KNN), and Support Vector Regression (SVR) algorithms were created and evaluated. Among them, the SVR model was retained for a global application. The Standard Error of Calibration (SEC) and the Standard Error of Prediction (SEP) were respectively 0.12% and 0.15%. This model was then evaluated in terms of total error and risk-based assessment, linearity, and accuracy. It was observed that MC can be fastly and simultaneously determined in freeze-dried pharmaceutical products thanks to a global NIR model created with different medicines. This innovative approach allows to speed up the validation time and the in-lab release analyses. [less ▲]

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See detailRaman Hyperspectral Imaging: An essential tool in the pharmaceutical field
Sacre, Pierre-Yves ULiege; Netchacovitch, Lauranne ULiege; Dumont, Elodie ULiege et al

E-print/Working paper (2017)

Resulting from the combination of Raman spectroscopy and optical microscopy, Raman hyperspectral imaging has proven to be an indispensable tool in the pharmaceutical field. This article will broach a ... [more ▼]

Resulting from the combination of Raman spectroscopy and optical microscopy, Raman hyperspectral imaging has proven to be an indispensable tool in the pharmaceutical field. This article will broach a number of Raman hyperspectral imaging applications that were developed in our laboratory, in order to demonstrate the significance of the technique. [less ▲]

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See detailDetection of Poor Quality Artemisinin-based Combination Therapy (ACT) Medicines Marketed in Benin Using Simple and Advanced Analytical Techniques
Yemoa, Achille; Habyalimana, Védaste ULiege; Mbinze Kindenge, Jérémie ULiege et al

in Current Drug Safety (2017), 12

Background: Poor quality antimalarial medicines still represent a threat to the public health, especially in Sub-Saharan Africa which bears a disproportionate share of the global burden of malaria. It is ... [more ▼]

Background: Poor quality antimalarial medicines still represent a threat to the public health, especially in Sub-Saharan Africa which bears a disproportionate share of the global burden of malaria. It is essential and urgent to strengthen mechanisms against counterfeit medicines. One of the approaches is regular market surveillance through quality controls. Methods: 12 samples of artemether/lumefantrine were collected from formal and informal drug sellers in Cotonou (Benin) as well as additional other similar samples from Rwanda (13 samples) and from D.R. Congo (9 samples). Thin Layer Chromatography (TLC) as classical and simple identification test was applied in Benin while an analytical chemistry laboratory in Belgium (ULg, Pharmacy Department) was asked for further analyses with HPLC and Raman spectroscopy using a developed and validated HPLC method for rapid analysis of artemether/lumefantrine. Results: The results obtained in Belgium confirmed the lack of the two active ingredients in the suspected sample of ACT medicine from Benin whereas some samples from Rwanda and D.R. Congo were found to present risk of substandard drugs either for under-dosing or over-dosing. Conclusions: Counterfeit/falsified of artemisinin-based combination therapy (ACT) medicines are really scourge that needs to be fought through strong collaboration between public health authorities and appropriate quality control laboratories. [less ▲]

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See detailGlobal approach for the validation of an in-line Raman spectroscopic method to determine the API content in real-time during a hot-melt extrusion process
Netchacovitch, Lauranne ULiege; Thiry, Justine ULiege; De Bleye, Charlotte ULiege et al

in Talanta (2017), 171

Since the Food and Drug Administration (FDA) published a guidance based on the Process Analytical Technology (PAT) approach, real-time analyses during manufacturing processes are in real expansion. In ... [more ▼]

Since the Food and Drug Administration (FDA) published a guidance based on the Process Analytical Technology (PAT) approach, real-time analyses during manufacturing processes are in real expansion. In this study, in-line Raman spectroscopic analyses were performed during a Hot-Melt Extrusion (HME) process to determine the Active Pharmaceutical Ingredient (API) content in real-time. The method was validated based on a univariate and a multivariate approach and the analytical performances of the obtained models were compared. Moreover, on one hand, in-line data were correlated with the real API concentration present in the sample quantified by a previously validated off-line confocal Raman microspectroscopic method. On the other hand, in-line data were also treated in function of the concentration based on the weighing of the components in the prepared mixture. The importance of developing quantitative methods based on the use of a reference method was thus highlighted. The method was validated according to the total error approach fixing the acceptance limits at ± 15% and the α risk at ± 5%. This method reaches the requirements of the European Pharmacopeia norms for the uniformity of content of single-dose preparations. The validation proves that future results will be in the acceptance limits with a previously defined probability. Finally, the in-line validated method was compared with the off-line one to demonstrate its ability to be used in routine analyses. [less ▲]

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See detailRaman Hyperspectral Imaging: An essential tool in the pharmaceutical field
Sacre, Pierre-Yves ULiege; De Bleye, Charlotte ULiege; Netchacovitch, Lauranne ULiege et al

Conference given outside the academic context (2017)

Raman hyperspectral imaging results from the powerful combination of spatial (imaging) and spectral (Raman) information. It is increasingly used both in R&D and in the industry because it allows the ... [more ▼]

Raman hyperspectral imaging results from the powerful combination of spatial (imaging) and spectral (Raman) information. It is increasingly used both in R&D and in the industry because it allows the investigation of many characteristics of solid samples. This technique provides an accurate tool for qualitative and quantitative analysis of a pharmaceutical solid formulation. In this webinar, Assoc. Prof. Ziemons will present fundamental concepts of hyperspectral imaging data analysis and key applications in pharmaceutical and biomedical field. [less ▲]

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See detailLe fléau des faux médicaments
Marini Djang'Eing'A, Roland ULiege; Ziemons, Eric ULiege; Sacre, Pierre-Yves ULiege et al

Conference given outside the academic context (2017)

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See detailDevelopment of an analytical method for crystalline content determination in amorphous solid dispersions produced by Hot-Melt Extrusion using transmission Raman spectroscopy: A feasibility study.
Netchacovitch, Lauranne ULiege; Dumont, Elodie ULiege; Cailletaud, Johan ULiege et al

in International Journal of Pharmaceutics (2017), 530(1-2), 249-255

The development of a quantitative method determining the crystalline percentage in an amorphous solid dispersion is of great interest in the pharmaceutical field. Indeed, the crystalline Active ... [more ▼]

The development of a quantitative method determining the crystalline percentage in an amorphous solid dispersion is of great interest in the pharmaceutical field. Indeed, the crystalline Active Pharmaceutical Ingredient transformation into its amorphous state is increasingly used as it enhances the solubility and bioavailability of Biopharmaceutical Classification System class II drugs. One way to produce amorphous solid dispersions is the Hot-Melt Extrusion (HME) process. This study reported the development and the comparison of the analytical performances of two techniques, based on backscattering and transmission Raman spectroscopy, determining the crystalline remaining content in amorphous solid dispersions produced by HME. Principal Component Analysis (PCA) and Partial Least Squares (PLS) regression were performed on preprocessed data and tended towards the same conclusions: for the backscattering Raman results, the use of the DuoScan™ mode improved the PCA and PLS results, due to a larger analyzed sampling volume. For the transmission Raman results, the determination of low crystalline percentages was possible and the best regression model was obtained using this technique. Indeed, the latter acquired spectra through the whole sample volume, in contrast with the previous surface analyses performed using the backscattering mode. This study consequently highlighted the importance of the analyzed sampling volume. [less ▲]

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See detailMoisture content determination in an antibody-drug conjugate freeze-dried medicine by near-infrared spectroscopy: a case study for release testing
Clavaud, Matthieu ULiege; Roggo, Yves; Dégardin, Klara et al

in Journal of Pharmaceutical and Biomedical Analysis (2016), 131

The use of Near-infrared spectroscopy (NIRS) as a fast and non-destructive technique was employed for moisture content (MC) determination in Antibody-drug conjugates (ADCs) in replacement to Karl Fischer ... [more ▼]

The use of Near-infrared spectroscopy (NIRS) as a fast and non-destructive technique was employed for moisture content (MC) determination in Antibody-drug conjugates (ADCs) in replacement to Karl Fischer (KF) method. The lab analysis of ADCs, high potent medicines, should be performed in conditions ensuring the operator’s safety and using secured analytical tools like NIRS. A NIRS method was first developed and validated in compliance with current guidelines. The novelty of this work first lies in the large number of samples prepared for a wide moisture calibration range of 0.51% to 4.01%. Then, the classical Partial Least Square (PLS) regression was used as chemometric tool for the computation of the model. Excellent predictive calibration results were shown. A coefficient of correlation (r) value of 0.99 was obtained. An intercept value of 0.02 and a slope of 0.99 were observed, while the root mean square error of calibration (RMSEC) and the root mean square error of prediction (RMSEP) were respectively 0.10% and 0.12%. In addition, instrumentation, model performances and robustness of the method were evaluated, demonstrating the validation results. Calibration transfer issue and impact of the number of samples were also evaluated. Consequently, a validation strategy was introduced as a basis for submission to the health authorities’ for release and stability activities in a cGMP environment in replacement of the KF method. [less ▲]

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See detailMonitoring of anatabine release by methyl jasmonate elicited BY-2 cells using surface-enhanced Raman scattering
De Bleye, Charlotte ULiege; Dumont, Elodie ULiege; Dispas, Amandine ULiege 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 ULiege; Thiry, Justine ULiege; De Bleye, Charlotte ULiege 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 detailScreening study of SFC critical method parameters for the determination of pharmaceutical compounds
Dispas, Amandine ULiege; Lebrun, Pierre ULiege; Sacre, Pierre-Yves ULiege et al

in Journal of Pharmaceutical and 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 ULiege; Ziemons, Eric ULiege; Hubert, Philippe ULiege et al

Article for general public (2016)

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See detailFrom Near-Infrared and Raman to Surface-Enhanced Raman Spectroscopy: Progress, Limitations, Perspectives in Bioanalysis
Dumont, Elodie ULiege; De Bleye, Charlotte ULiege; Sacre, Pierre-Yves ULiege 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 detailPoplar-root-knot nematode interaction: a model for perennial woody species
Baldacci-Cresp, Fabien; Sacre, Pierre-Yves ULiege; Twyffels, Laure et al

in Molecular Plant-Microbe Interactions (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 ULiege; Mbinze Kindenge, Jérémie; Kalenda Tshilombo, Nicodème ULiege 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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