References of "Ziemons, Eric"
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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 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 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 detailOptimization and validation of a fast Supercritical Fluid Chromatography method for the quantitative determination of vitamin D3 and its related impurities.
Andri, Bertyl ULg; Lebrun, Pierre ULg; Dispas, Amandine ULg et al

in Journal of Chromatography. A (2017)

In the uprising context of green analytical chemistry, Supercritical Fluid Chromatography (SFC) is often suggested as an alternative to Normal Phase Liquid Chromatography. Indeed, SFC provides fast ... [more ▼]

In the uprising context of green analytical chemistry, Supercritical Fluid Chromatography (SFC) is often suggested as an alternative to Normal Phase Liquid Chromatography. Indeed, SFC provides fast, efficient and green separations. In this report, the quantitative performances of SFC were challenged on a real-life case study: the Quality Control (QC) of vitamin D3. A rapid and green SFC method was optimized thanks to the Design of Experiments–Design Space (DoE–DS) methodology. It provided robust and high quality separation of the compounds within a 2 min timeframe, using a gradient of ethanol as co-solvent of the carbon dioxide. The analytical method was fully validated according to the total error approach, demon- strating the compliance of the method to the specifications of U.S. Pharmacopeia (USP: 97.0–103.0%) and European Pharmacopeia (EP: 97.0–102.0%) for an interval of [50–150%] of the target concentration. In order to allow quantification of impurities using vitamin D3 as an external standard in SFC-UV, correction factors were determined and verified during method validation. Thus, accurate quantification of impu- rities was demonstrated at the specified levels (0.1 and 1.0% of the main compound) for a 70.0–130.0% dosing range. This work demonstrates the validity of an SFC method for the QC of vitamin D3 raw material and its application to real samples. Therefore, it supports the switch to a greener and faster separative technique as an alternative to NPLC in the pharmaceutical industry. [less ▲]

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See detailContinuous Production of Itraconazole-based Solid Dispersions by Hot Melt Extrusion: Preformulation, Optimization and Design Space Determination.
Thiry, Justine ULg; Lebrun, Pierre; Vinassa, Chloé et al

in International Journal of Pharmaceutics (2016), 515(1-2), 114-124

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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 ULg; Roggo, Yves; Dégardin, Klara et al

in Journal of Pharmaceutical & 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 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 detailMédicaments usage de faux
Sacre, Pierre-Yves ULg; Ziemons, Eric ULg; Hubert, Philippe ULg et al

Article for general public (2016)

Detailed reference viewed: 56 (12 ULg)
See detailApproches intégrées en Sciences Pharmaceutiques
Servais, Anne-Catherine ULg; Ziemons, Eric ULg

Conference (2016, May 13)

Detailed reference viewed: 16 (1 ULg)
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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 ▲]

Detailed reference viewed: 117 (25 ULg)