References of "Mantanus, Jérôme"
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See detailAN INNOVATIVE APPROACH TO SELECT THE PREDICTION MODEL IN THE DEVELOPMENT OF NIR SPECTROSCOPIC METHODS
Ziemons, Eric ULg; Mantanus, Jérôme ULg; Rozet, Eric ULg et al

Poster (2012, March)

Taking into account its non-invasive, non-destructive character and fast data acquisition, near infrared spectroscopy is more and more integrated in production processes to acquire analytical results ... [more ▼]

Taking into account its non-invasive, non-destructive character and fast data acquisition, near infrared spectroscopy is more and more integrated in production processes to acquire analytical results. Implementation of a NIR quantitative method is performed using an iterative heuristic approach that will ultimately build a model allowing the prediction of the concentration of the analyte of interest. In this context, the aim of the present study was to develop an innovative approach based on statistical tolerance intervals and the desirability index FMI (Fitting Model Index) to select the most appropriate prediction model from a list of candidate models instead of using conventional criteria such as R², RMSEC, RMSECV and RMSEP [1-2] without objective decision rules. This new approach is illustrated on different steps of a real pharmaceutical manufacturing process: water and Active Pharmaceutical Ingredient (API) determinations in pharmaceutical pellets. Variability sources such as production campaigns, batches, days and operators were introduced in the calibration and validation sets. Partial Least Square (PLS) regression on the calibration sets was performed to build prediction models of which the ability to quantify accurately was tested with the validation sets. Regarding the product specifications, the acceptance limits were set at 20% and 5%, for the moisture and API determination, respectively.As can be seen from Figure 1 and 2, this innovative approach based on the desirability index FMI of the accuracy profile enabled to build and select the most appropriate prediction model in full accordance with its very final goal, to quantify as accurately as possible the analytes of interest. [1] Hubert Ph. et al., J. Pharm. Biomed. Anal., 36, 2007, 579-586. [2] Rozet E. et al., Ana. Chim. Acta, 591, 2007, 239-247. [less ▲]

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See detailCritical Review of Near-Infrared Spectroscopic Methods Validations in Pharmaceutical Applications
De Bleye, Charlotte ULg; Chavez, Pierre-François ULg; Mantanus, Jérôme ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (2012), 69

Based on the large number of publications reported over the past five years, near-infrared spectroscopy (NIRS) is more and more considered an attractive and promising analytical tool regarding Process ... [more ▼]

Based on the large number of publications reported over the past five years, near-infrared spectroscopy (NIRS) is more and more considered an attractive and promising analytical tool regarding Process Analytical Technology and Green Chemistry. From the reviewed literature, few of these publications present a thoroughly validated NIRS method even if some guidelines have been published by different groups and regulatory authorities. However, as any analytical method, the validation of NIRS method is a mandatory step at the end of the development in order to give enough guarantees that each of the future results during routine use will be close enough to the true value. Besides the introduction of PAT concepts in the revised document of the European Pharmacopoeia (2.2.40) dealing with near-infrared spectroscopy recently published in Pharmeuropa, it agrees very well with this mandatory step. Indeed, the latter suggests to use similar analytical performance characteristics than those required for any analytical procedure based on acceptance criteria consistent with the intended use of the method. In this context, this review gives a comprehensive and critical overview of the methodologies applied to assess the validity of quantitative NIRS methods used in pharmaceutical applications. [less ▲]

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See detailDesign space approach in the optimization of the spray-drying process
Lebrun, Pierre ULg; Krier, Fabrice ULg; Mantanus, Jérôme ULg et al

in European Journal of Pharmaceutics & Biopharmaceutics (2012), 80(1), 226-234

From a quality by design perspective, the aim of the present study was to demonstrate the applicability of a Bayesian statistical methodology to identify the design space (DS) of a spray-drying process ... [more ▼]

From a quality by design perspective, the aim of the present study was to demonstrate the applicability of a Bayesian statistical methodology to identify the design space (DS) of a spray-drying process. Following the ICH Q8 guideline, the DS is defined as the “multidimensional combination and interaction of input variables (e.g., materials attributes) and process parameters that have been demonstrated to provide assurance of quality”. Thus, a predictive risk-based approach was set up in order to account for the uncertainties and correlations found in the process and in the derived critical quality attributes such as the yield, the moisture content, the inhalable fraction of powder, the compressibility index and the Hausner ratio. This allowed quantifying the guarantees and the risks to observe whether the process shall run according to specifications. These specifications describe satisfactory quality outputs and were defined a priori given safety, efficiency and economical reasons. Within the identified DS, validation of the optimal condition was effectuated. The optimized process was shown to perform as expected, providing a product for which the quality is built in by the design and controlled set-up of the equipment, regarding identified critical process parameters: the inlet temperature, the feed rate and the spray flow rate. [less ▲]

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See detailNear infrared and Raman spectroscopy as Process Analytical Technology tools for the manufacturing of silicone-based drug reservoirs
Mantanus, Jérôme ULg; Rozet, Eric ULg; Van Butsele, K. et al

in Analytica Chimica Acta (2011), 699

Using Near Infrared (NIR) and Raman spectroscopy as PAT tools, 3 critical quality attributes of a silicone-based drug reservoir were studied. First, the Active Pharmaceutical Ingredient (API) homogeneity ... [more ▼]

Using Near Infrared (NIR) and Raman spectroscopy as PAT tools, 3 critical quality attributes of a silicone-based drug reservoir were studied. First, the Active Pharmaceutical Ingredient (API) homogeneity in the reservoir was evaluated using Raman spectroscopy (mapping): the API distribution within the industrial drug reservoirs was found to be homogeneous while API aggregates were detected in laboratory scale samples manufactured with a non optimal mixing process. Second, the crosslinking process of the reservoirs was monitored at different temperatures with NIR spectroscopy. Conformity tests and Principal Component Analysis (PCA) were performed on the collected data to find out the relation between the temperature and the time necessary to reach the crosslinking endpoints. An agreement was found between the conformity test results and the PCA results. Compared to the conformity test method, PCA had the advantage to discriminate the heating effect from the crosslinking effect occurring together during the monitored process. Therefore the 2 approaches were found to be complementary. Third, based on the HPLC reference method, a NIR model able to quantify the API in the drug reservoir was developed and thoroughly validated. Partial Least Squares (PLS) regression on the calibration set was performed to build prediction models of which the ability to quantify accurately was tested with the external validation set. The 1.2 % RMSEP of the NIR model indicated the global accuracy of the model. The accuracy profile based on tolerance intervals was used to generate a complete validation report. The 95 % tolerance interval calculated on the validation results indicated that each future result will have a relative error below ±5 % with a probability of at least 95 %. In conclusion, 3 critical quality attributes of silicone-based drug reservoirs were quickly and efficiently evaluated by NIR and Raman spectroscopy. [less ▲]

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See detailDetermination of binary polymorphic mixtures of fluconazole using near infrared spectroscopy and X-ray powder diffraction: A comparative study based on the pre-validation stage results
Ziemons, Eric ULg; Bourichi, H.; Mantanus, Jérôme ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (2011), 55

The aim of the present study was to develop near infrared (NIR) and X-ray powder diffraction methods (XRPD) able to determine pure crystalline form II of fluconazole in a binary polymorphic mixtures ... [more ▼]

The aim of the present study was to develop near infrared (NIR) and X-ray powder diffraction methods (XRPD) able to determine pure crystalline form II of fluconazole in a binary polymorphic mixtures containing form II and III. In order to give a first performance estimation of both methods, these latters were pre-validated using accuracy profiles, a statistical approach based on β-expectation tolerance intervals. Both methods showed a good trueness, precision and accuracy and their β-expectation tolerance intervals were fully included within the acceptance limits. The comparative study was carried out using statistical analysis based on the work of Bland and Altman. A good agreement between the two methods was demonstrated indicating the interchangeability of NIR method with XRPD method. [less ▲]

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See detailRaman spectroscopic study of complex formation between major calixarene derivatives and three pharmaceutical substances
Tiuca, Ioana; Mantanus, Jérôme ULg; Iacob, Bogdan et al

Poster (2010, November)

Complex formation of six calix[n]arene derivatives – tert-butyl-calix[4]arene (C4), tert-butyl-calix[6]arene (C6), tert-butyl-calix[8]arene (C8) and their ethyl-acetic-ester derivatives (C4Es4, C6Es6 ... [more ▼]

Complex formation of six calix[n]arene derivatives – tert-butyl-calix[4]arene (C4), tert-butyl-calix[6]arene (C6), tert-butyl-calix[8]arene (C8) and their ethyl-acetic-ester derivatives (C4Es4, C6Es6, C8Es8) – has been the subject for our Raman spectroscopic study. Substances taken in study for complexation were the two widely used anticoagulants – warfarin and its 5-nitro- derivative, acenocoumarol – and their antidote, phytomenadione (also known as phylloquinone or vitamin K1). For each standard substance, Raman spectra were studied between 3620 and 90 cm-1. In order to obtain the complexes, a mixture of solutions of each calixarene and each analyte was prepared, in a stoichiometric ratio of 1:1 and then the solvents were evaporated. Spectra of solid residues obtained were compared with those of initial molecules. In all cases, there was observed a Raman band shifting or even the disappearance of some bands, indicating that calixarene derivatives interact with the studied molecules. In conclusion, the six calixarene derivatives taken in study seem to be able to form complexes with the molecules of warfarin, acenocoumarol and phylloquinone. [less ▲]

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See detailRISK MANAGMENT IN THE VALIDATION OF ANALYTICAL METHODS
Hubert, Philippe ULg; Ziemons, Eric ULg; Mantanus, Jérôme ULg et al

Conference (2010, October)

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See detailNIR AND RAMAN SPECTROSCOPY AS PAT TOOLS FOR THE MANUFACTURING OF SILICONE-BASED DRUG RESERVOIRS
Mantanus, Jérôme ULg; Ziemons, Eric ULg; Van Butsele, Kathy et al

Conference (2010, September 24)

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See detailAnalytical tools to fight against counterfeit medicines
Marini Djang'Eing'A, Roland ULg; Mbinze Kindenge, J.; Montes, M. L. A. et al

in Chimica Oggi = Chemistry Today (2010), 28(5), 10-14

Counterfeiting has been dramatically increasing this last decade throughout the world and particularly in developing countries, with many consequences such as adverse impacts on public health, economics ... [more ▼]

Counterfeiting has been dramatically increasing this last decade throughout the world and particularly in developing countries, with many consequences such as adverse impacts on public health, economics and negative reputation for the pharmaceutical industry. Recognizing the magnitude of the issue, health authorities at national, regional and international levels are trying to fight against this scourge using various strategies including the setting-up of effective quality control that need to be reinforced through generic, fast and specific detection methods. To illustrate this topic, we will present several analytical tools, including liquid chromatography, low cost capillary electrophoresis and near infrared spectroscopy, developed and applied to the detection and quantification of counterfeit drugs. [less ▲]

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