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See detailCritical review of surface-enhanced Raman spectroscopy applications in the pharmaceutical field
Cailletaud, Johan ULg; De Bleye, Charlotte ULg; Dumont, Elodie ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (in press)

Surface-enhanced Raman spectroscopy (SERS) is a sensitive analytical tool used in the pharmaceutical field in recent years. SERS keeps all the advantages of classical Raman spectroscopy while being is ... [more ▼]

Surface-enhanced Raman spectroscopy (SERS) is a sensitive analytical tool used in the pharmaceutical field in recent years. SERS keeps all the advantages of classical Raman spectroscopy while being is more sensitive allowing its use for the detection and the quantification of low-dose substances contained in pharmaceutical samples. However, the analytical performance of SERS is limited due to the difficulty to implement a quantitative methodology correctly validated. Nevertheless, some studies reported the development of SERS quantitative methods especially in pharmaceutical approaches. In this context, this review presents the main concepts of the SERS technique. The different steps that need to be applied to develop a SERS quantitative method are also deeply described. The last part of the present manuscript gives a critical overview of the different SERS pharmaceutical applications that were developed for a non-exhaustive list of pharmaceutical compounds with the aim to highlights the validation criteria for each application. [less ▲]

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See detailGlobal regression model for moisture content determination using near-infrared spectroscopy
Clavaud, Matthieu ULg; Roggo, Yves; Degardin, Klara et al

in European Journal of Pharmaceutics and Biopharmaceutics (2017)

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 detailImpact of formulation and process parameters on near-infrared spectra: Application for water determination in biopharmaceuticals
Clavaud, Matthieu ULg; Roggo, Yves; Allmendinger, Andrea et al

Poster (2017, June 11)

Traditionally, the water content of freeze-dried biopharmaceuticals is determined by time-consuming methods such as Karl Fischer titration. As a fast and non-destructive method, many studies demonstrated ... [more ▼]

Traditionally, the water content of freeze-dried biopharmaceuticals is determined by time-consuming methods such as Karl Fischer titration. As a fast and non-destructive method, many studies demonstrated the efficiency of Near-Infrared (NIR) spectroscopy for that purpose [1]. In this study, NIR was applied to different freeze-dried monoclonal antibody. The aim was to evaluate the robustness of a NIR model depending on formulation composition and process parameters of the lyophilization parameters, and the benefits of NIR when developing a freeze-drying cycle for a new pharmaceutical product. A full Design of experiments (DoE) was established in order to produce materials with various formulations and various process parameters. As a first step, a calibration model was created and validated. The model creation was based on 4 target lyophilized cycles which were manufactured to obtain samples with different water content concentration. Then, 20 lyophilized cycles were produced according to the DoE. Two levels of protein and sucrose concentration, and two levels of pressure / primary drying temperature and process time were investigated. Furthermore, several samples of each experiment stored at different temperature and relative humidity conditions were evaluated. Chemometrics using Principal Component Analysis (PCA) and Partial Least Squares (PLS) were used to evaluate the process variations and to determine the water content, respectively. NIR is capable to differentiate between different lyophilization process conditions, based on chemometrics. Robust calibration NIR model for water determination was generated against KF independent on lyophilization process parameters and formulation composition. NIR is suitable and robust method for drug product development of freeze-dried formulation. [less ▲]

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See detailRaman Hyperspectral Imaging: An essential tool in the pharmaceutical field
Sacre, Pierre-Yves ULg; Netchacovitch, Lauranne ULg; Dumont, Elodie ULg 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 detailImplementation of SFC for the quality control of pharmaceuticals
Dispas, Amandine ULg; Andri, Bertyl ULg; Lebrun, Pierre ULg et al

Conference (2017, May 17)

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See detailEtude comparative des profils de dissolution in vitro de quinine sulfate générique et princeps en utilisant la Chromatographie Liquide Haute Performance
Mbinze Kindenge, Jérémie ULg; Diallo, Tediane; Yemoa, Loconon ULg et al

in Médecine d'Afrique Noire (2017), 64

Introduction : La quinine est une molécule préconisée pour le traitement du paludisme dans les régions où les souches de P. falciparum sont polyrésistantes. Face à l’importante utilisation de ses ... [more ▼]

Introduction : La quinine est une molécule préconisée pour le traitement du paludisme dans les régions où les souches de P. falciparum sont polyrésistantes. Face à l’importante utilisation de ses médicaments génériques d’une part, et au fléau des médicaments de qualité inférieure d’autre part, il devient plus que nécessaire d’appuyer les données des tests physico-chimiques par celles de dissolution in vitro dont l’évaluation et la comparaison des cinétiques permettra de prédire le comportement in vivo du principe actif et par conséquent l’efficacité du médicament générique. L’objectif de la présente étude est de réaliser une étude comparative de la cinétique de dissolution d’un princeps et d’un générique à base de quinine comprimé 300 mg commercialisés à Kinshasa. Matériels et méthodes : L’étude a été réalisée en utilisant trois milieux de pH différents (1,2 - 4,5 - 6,8) tels que recommandés par l’Agence Européenne de Médicament et en se servant d’un appareil de dissolution, tandis que l’équipement de chromatographie liquide à haute performance couplée à un détecteur à barrette de diodes a été utilisé pour la quantification. La méthode statistique fit factor a été appliquée pour comparer les résultats de dosage de la quinine dans les trois milieux tout en ayant évalué le biais à différents temps de dissolution. Résultats : Les différents échantillons de médicaments générique et princeps ont été conformes quant à l’identification et au dosage de la quinine, par contre leurs cinétiques de dissolution étaient non similaires. Discussion : Ceci pourrait avoir une influence sur l’efficacité du produit générique et la sécurité des consommateurs, dénotant l’importance d’examiner les profils de dissolution des génériques avant toute autorisation de mise sur le marché plus particulièrement dans les pays en voie de développement. [less ▲]

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

E-print/Working paper (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 ULg; Ziemons, Eric ULg; Sacre, Pierre-Yves ULg et al

Conference given outside the academic context (2017)

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See detailINVESTIGATION DE LA QUALITE D’ANTIBIOTIQUES A BASE D'AMOXICILLINE DANS LE CADRE DE LA SURVEILLANCE DU MARCHE OFFICIEL ET PERIPHERIQUE DE QUELQUES VILLES DE LA R.D. CONGO
Kalenda Tshilombo, Nicodème ULg; Ciza Hamuli, Patient ULg; Mavungu Landu, Don Jethro ULg et al

Poster (2017, March)

Drug counterfeiting is a sad and worrisome reality, especially in developing countries where quality control is not effective and sometimes not existing at all despite political will of governments. The ... [more ▼]

Drug counterfeiting is a sad and worrisome reality, especially in developing countries where quality control is not effective and sometimes not existing at all despite political will of governments. The consequences are harmful in particular for substandard medicines that pose more threats to populations in those countries due to their direct negative impact on patients such as failure of medical treatment including development of drug resistance and even death. Socio-economic consequences and negative reputation concerning the pharmaceutical industry are also observed. Unfortunately accurate detailed data on such medicines are not easy to obtain. Most of the time available data are often estimated from case reports or studies carried out in a specific area and during a defined period.Health authorities’ in the Democratic Republic of Congo are trying to identify this scourge by set up several strategies to fight against. One of them is built on the best knowledge of drugs from several horizons through the assessment of their quality to allow appropriate measurement. In this context, we have focused our study towards amoxicillin alone and/or combined with potassium clavulanate since it is one the very used medicines in pediatric medications. The formulations are powder for suspension. Two analytical methods were developed based on the USP monography, applying isocratic liquid chromatography. Prior to their application in routine, we evaluated the suitability of these methods through validation applying the accuracy profile of total error. Since it was planned to transfer the methods to DRC, several operating factors were taken into account namely operator, day and equipment. Interesting results were obtained in terms of trueness (relative biases below than 2.3%), precision (RSD of Intermediate precision below 2.8%), accuracy (beta-expectation tolerance intervals between -6.0% and 3.8%) for the concentration levels of interest. The latter were able to allow monitoring the quality of the two active ingredients here above in the 65 samples from Congolese market. They were collected in Kinshasa, Lubumbashi, Matadi and Kolwezi at official and non-official medicines distributors, in peripheral area. The dramatic results obtained confirm that substandard and counterfeit medicines remain a crucial problem on public health in low-income countries. Appropriate measures are really needed to set up the drug quality improvement. [less ▲]

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See detailApplication of design space optimization strategy to the developmentof LC methods for simultaneous analysis of 18 antiretroviral medicinesand 4 major excipients used in various pharmaceutical formulations
Habyalimana, Védaste ULg; Mbinze Kindenge, Jérémie ULg; Yemoa, Loconon ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (2017), 139

tAs one of the world’s most significant public health challenges in low- and middle-income countries,HIV/AIDS deserves to be treated with appropriate medicines, however which are not spared from coun ... [more ▼]

tAs one of the world’s most significant public health challenges in low- and middle-income countries,HIV/AIDS deserves to be treated with appropriate medicines, however which are not spared from coun-terfeiting. For that, we developed screening and specific HPLC methods that can analyze 18 antiretroviralmedicines (ARV) and 4 major excipients. Design of experiments and design space methodology wereinitially applied for 15 ARV and the 4 excipients with prediction thanks to Monte Carlo simulations andfocusing on rapidity and affordability thus using short column and low cost organic solvent (methanol)in gradient mode with 10 mM buffer solutions of ammonium hydrogen carbonate. Two other specificmethods dedicated to ARV in liquid and in solid dosage formulations were also predicted and opti-mized. We checked the ability of one method for the analysis of a fixed-dose combination composedby emtricitabine/tenofovir/efavirenz in tablet formulations. Satisfying validation results were obtainedby applying the total error approach taking into account the accuracy profile as decision tool. Then, thevalidated method was applied to test two samples coded A and B, and claimed to contain the tested ARV.Assay results were satisfying only for sample B. [less ▲]

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See detailQuantitative determination of salbutamol sulfate impurities using achiral supercritical fluid chromatography
Dispas, Amandine ULg; Desfontaine, Vincent; Andri, Bertyl ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (2017), 134

In the last years, supercritical fluid chromatography has largely been acknowledged as a singular and performing technique in the field of separation sciences. Recent studies highlighted the interest of ... [more ▼]

In the last years, supercritical fluid chromatography has largely been acknowledged as a singular and performing technique in the field of separation sciences. Recent studies highlighted the interest of SFC for the quality control of pharmaceuticals, especially in the case of the determination of the active pharmaceutical ingredient (API).Nevertheless, quality control requires also the determination of impurities. The objectives of the present work were to i) demonstrate the interest of SFC as a reference technique for the determination of impurities in salbutamol sulfate API and ii) to propose an alternative to a reference HPLC method from the European Pharmacopeia (EP) involving ionpairing reagent. Firstly, a screening was carried out to select the most adequate and selective stationary phase. Secondly, in the context of robust optimization strategy, the method was developed using design space methodology. The separation of salbutamol sulfate and related impurities was achieved in 7 minutes, which is seven times faster than the LC-UV method proposed by European Pharmacopeia (total run time of 50 minutes). Finally, full validation using accuracy profile approach was successfully achieved for the determination of impurities B, D, F and G in salbutamol sulfate raw material. The validated dosing range covered 50 to 150 % of the targeted concentration (corresponding to 0.3 % concentration level), LODs close to 0.5 μg/mL were estimated. The SFC method proposed in this study could be presented as a suitable fast alternative to EP LC method for the quantitative determination of salbutamol impurities. [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 ULg; Thiry, Justine ULg; De Bleye, Charlotte ULg et al

in Talanta (2017)

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 detailChapter 11 - Validation of Supercritical Fluid Chromatography Methods
Dispas, Amandine ULg; Lebrun, Pierre ULg; Hubert, Philippe ULg

in Poole, Colin (Ed.) Supercritical Fluid Chromatography - Handbook in Separation Science (2017)

Method validation is the process of proving that an analytical method is acceptable for its intended purpose. The present chapter defines the validation criteria described in regulatory documents. Despite ... [more ▼]

Method validation is the process of proving that an analytical method is acceptable for its intended purpose. The present chapter defines the validation criteria described in regulatory documents. Despite the abundance of guidelines, the conclusion about method validity remains confused. In this context, the state-of-the-art validation methodology named total error approach is briefly explained as the methodology that should be followed for all method validations. Finally, a review of literature presents quantitative development and validation of supercritical fluid chromatography (SFC) methods considering a wide range of applications and analytical fields. [less ▲]

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