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See detailPrinciples of Analytical Quality by Design for the development of quality control methods in a pharmaceutical context
Deidda, Riccardo ULiege; Avohou, Tonakpon Hermane ULiege; Jambo, Hugues ULiege et al

Conference (2019, May 20)

Pharmaceutical regulatory agencies increasingly require the implementation of systematic approaches covering the entire life-cycle of pharmaceutical products, from manufacturing processes to quality ... [more ▼]

Pharmaceutical regulatory agencies increasingly require the implementation of systematic approaches covering the entire life-cycle of pharmaceutical products, from manufacturing processes to quality control tests. In 2009, the International Council for Harmonisation (ICH) of technical requirements for pharmaceuticals for human use proposed a systematic approach named “Quality by Design” (QbD) to be implemented in the pharmaceutical field [1]. In this context, the QbD strategy have been progressively applied also to other aspects of the pharmaceutical chain, such as the analytical method development in quality control laboratories. The QbD applied to analytical chemistry is commonly named “Analytical Quality by Design” (AQbD) and in the last decade it has been widely applied in academia for the development of separation methods, involving different techniques such as LC, CE as well as SFC. However, its implementation in quality control laboratories still remains limited and then its advantages not completely exploited. Indeed, this approach presents a lot of conveniences, such as the deep knowledge acquired during the method development/optimisation by studying how critical method parameters (CMPs) affect critical method attributes (CMAs). Moreover, this strategy allows the possibility to define a method operable design region (MODR) consisting of a multitude of possible working points and for each of them a specific probability of success (π) is given. Indeed, the concept of risk plays a central role in this strategy as the MODR is considered of a zone of theoretical robustness limited by the so-called edges of failure, outside which the method performances are not accepted [2]. This presentation focuses first on the theoretical aspects regarding each step of this strategy. The analytical target profile definition, the selection of CMPs and CMAs, as well as screening and optimisation of CMPs and MODR definition are accurately described and illustrated. Some considerations about the choice of the working point, its validation and the planning of an efficient control strategy are also given. In the second part of this presentation all these concepts are once again showcased but from a practical point of view, by giving two concrete case-studies following the AQbD approach. The first one concerns the development of a liquid chromatography coupled to UV (LC-UV) method aimed at quantifying the cannabinoids content in cannabis extracts used for medicinal purposes [3]. The second one shows the approach applied to the development of a stability indicating method by using another analytical technique, the supercritical-fluid-chromatography coupled to mass spectrometry (SFC-MS). This latter is intended to be used for the quantification of hydro-soluble vitamins and amino acids in a complex medium. References [1] ICH Harmonised Tripartite guideline. Pharmaceutical Development Q8(R2) (2009) International Council for harmonisation of technical Requirements for Pharmaceutical for Human Use. [2] R. Deidda, S. Orlandini, Ph. Hubert, C. Hubert, Risk-based approach for method development in pharmaceutical quality control context: A critical review, J. Pharm. Biomed. Anal. 161 (2018) 110-121. [3] R. Deidda, H.T. Avohou, R. Baronti, P.L. Davolio, B. Pasquini, M. Del Bubba, C. Hubert, Ph. Hubert, S. Orlandini, S. Furlanetto, Analytical quality by design: Development and control strategy for a LC method to evaluate the cannabinoids content in cannabis olive oil extracts, J. Pharm. Biomed. Anal. 166 (2019) 326-335. [less ▲]

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See detailDéveloppement d’une méthode SFC-MS pour le dosage de vitamines en matrice complexe : Application de la stratégie « Analytical Quality by Design »
Deidda, Riccardo ULiege; Mignolet, Marie ULiege; Jambo, Hugues ULiege et al

Conference (2019, March 26)

Les agences réglementaires pharmaceutiques exigent de plus en plus fréquemment la mise en œuvre des approches systématiques couvrant l'ensemble du cycle de vie des produits pharmaceutiques, des processus ... [more ▼]

Les agences réglementaires pharmaceutiques exigent de plus en plus fréquemment la mise en œuvre des approches systématiques couvrant l'ensemble du cycle de vie des produits pharmaceutiques, des processus de fabrication jusqu’aux tests de contrôle qualité. En 2009, the International Council for Harmonisation of Technical Requirements for Pharmaceutical for Human Use (ICH) a proposé une approche systématique appelée « quality by design » appliqué à la production pharmaceutique. Ce concept étendu aux méthodes analytiques, « analytical quality by design (AQbD) », fait l’objet de recherches approfondies dans les milieux universitaires. Cette stratégie est appliquée aux méthodes séparatives telles que la LC, la CE et la SFC, mais reste actuellement relativement peu étendu au niveau des laboratoires de contrôle de qualité des industries pharmaceutiques. Pourtant, la stratégie AQbD présente un avantage considérable. En effet, elle permet d’obtenir une connaissance approfondie de la méthode et ce, tout au long du développement et de l’optimisation de celle-ci. L’évaluation des paramètres critiques de la méthode (CMPs) sur base de ses attributs critiques (CMAs) rend possible la définition d’une région opérationnelle probable (MODR). Cette région consiste en une multitude de conditions de travail possibles, où pour chacune d’elles, une probabilité de succès spécifique (π) est attribuée. En effet, la notion de risque joue un rôle primordial permettant ainsi d’assurer la robustesse de la méthode tout au long de son cycle de vie. Ce projet s'est concentré sur les aspects pratiques de cette stratégie en donnant un exemple concret de développement d'une méthode SFC-MS (entièrement conforme à la stratégie AQbD) pour une étude de stabilité d’une matrice complexe dans un contexte de contrôle de la qualité. Le développement de la méthode AQbD commence par la définition des requis analytiques (ATP), qui représentent l'objectif de la méthode dans le cadre de son utilisation spécifique. Dans ce cas-ci, l'échantillon étudié est constitué d'un milieu de culture cellulaire complexe constitué de plus de 40 composés et pour lequel les données relatives à la composition qualitative et quantitative ne sont pas complètement disponibles. Ensuite, plusieurs vitamines hydrophiles doivent être quantifiées afin de contrôler la stabilité de ce milieu. Dans la mesure où un effet matrice conséquent avait été mis en évidence dans une étude antérieure (UHPLC-MS), la chromatographie en phase supercritique couplée à la spectrométrie de masse a été choisie comme technique analytique alternative. En effet, dans certaines conditions, la SFC-MS peut être moins affectée par les effets de matrice que la LC-MS [3]. Afin de mettre en place correctement la stratégie AQbD, des expériences préliminaires ont été menées de manière rationnelle dans le but de sélectionner les meilleures conditions de départ. Dans cette phase, appelée « scouting », plusieurs phases stationnaires ont été testées et les colonnes les plus prometteuses ont été sélectionnées afin de mener des essais complémentaires. Différents gradients et modificateurs ont également été préalablement testés afin de sélectionner les conditions permettant l’élution des analytes d’intérêt. En effet, les vitamines ciblées présentent un comportement chromatographique varié entrainant des rétentions très différentes. Les critères de séparation et l'effet de matrice ont été étudiés et optimisés, en prenant en compte non seulement les aspects chromatographiques mais également ceux liés à la détection par MS. Dans ce contexte, une phase « screening » a été menée pour identifier les CMPs ayant une incidence importante sur les CMAs. Ensuite, les CMPs ont fait l’objet d’une étude approfondie au cours de la phase d’optimisation afin de mieux comprendre leur influence sur les performances de séparation et détection de la méthode. Cette dernière partie permettra d’introduire le concept de risque en appliquant des simulations de Monte-Carlo et une approche bayésienne capable d’évaluer l’incertitude du model proposé [4]. Par conséquent, une MODR liée à une probabilité de réussite définie, en termes de respect des spécifications données aux CMAs, sera obtenue. La MODR représente une zone de robustesse théorique dont chacun des points peut être sélectionné comme une condition opératoire en vue d’être validée. Cela démontre l'utilité de cette approche pour la mise au point d'une méthode analytique appliquée aux études de stabilité et ce, dans un contexte de contrôle de la qualité [2]. References [1] ICH Harmonised Tripartite guideline. Pharmaceutical Development Q8(R2) (2009) International Council for harmonisation of technical Requirements for Pharmaceutical for Human Use. [2] R. Deidda, S. Orlandini, Ph. Hubert, C. Hubert, Risk-based approach for method development in pharmaceutical quality control context: A critical review, J. Pharm. Biomed. Anal. 161 (2018) 110-121. [3] V. Desfontaine, F. Capetti, R. Nicoli, T. Kuuranne, J.-L. Veuthey, D. Guillarme, Systematic evaluation of matrix effects in supercritical fluid chromatography versus liquid chromatography coupled to mass spectrometry for biological samples, J. Chromatogr. B 1079 (2018) 51-61. [4] E. Rozet, P. Lebrun, Ph. Hubert, B. Debrus, B. Boulanger, Design Spaces for analytical methods, Trends Anal. Chem. 42 (2013) 157-167. [less ▲]

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See detailSFC-MS for the quality control of cannabis: addressing the potential adulteration with synthetic cannabinoids
Jambo, Hugues ULiege; Dispas, Amandine ULiege; Avohou, Tonakpon Hermane ULiege et al

Scientific conference (2018, December 19)

Recent years have been the stage to a shift in cannabis policies and trends that have impacted cannabis usage and public perception. On the other hand, there has also been a rise in the development and ... [more ▼]

Recent years have been the stage to a shift in cannabis policies and trends that have impacted cannabis usage and public perception. On the other hand, there has also been a rise in the development and distribution of synthetic cannabinoids which are synthetic compounds that also act on the endocannabinoid receptors. They are mostly used as recreational drugs and because their potency and toxicity are not always known, they can lead to severe adverse effects after consumption. The detection of cannabis counterfeiting with synthetic cannabinoids is essential to produce safe cannabis-based medicines and we aimed to develop a generic supercritical fluid chromatography hyphenated to mass spectrometry (SFC-MS) method that could help in detecting such adulterations using representative synthetic cannabinoids from multiple classes. Method development started with a screening of stationary phases using seven different SFC-dedicated columns. Then, an optimization following analytical quality-by-design principles was performed followed by an assessment of the quantitative performances with a validation according to the total-error strategy. This innovative tool should prove useful in the context of counterfeit drugs tracking in the challenges to come. [less ▲]

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See detailSFC-MS as a preventive tool for the quality control of potentially adulterated cannabis with synthetic cannabinoids
Jambo, Hugues ULiege; Dispas, Amandine ULiege; Avohou, Tonakpon Hermane ULiege et al

Conference (2018, October 19)

Recent years have been the stage to a shift in cannabis policies and trends that have impacted cannabis usage and public perception. It has also caught the attention of the pharmaceutical industry and ... [more ▼]

Recent years have been the stage to a shift in cannabis policies and trends that have impacted cannabis usage and public perception. It has also caught the attention of the pharmaceutical industry and cannabis is increasingly evaluated as a medicine in the treatment of various conditions. On the other hand, there has also been a rise in the development and distribution of synthetic cannabinoids which are synthetic compounds that have the same pharmacological action as the natural cannabinoids found in the plant. They are mostly used as recreational drugs and because their potency and toxicity are not always known, they can lead to severe adverse effects after consumption. The detection of counterfeiting cannabis with synthetic cannabinoids is essential to produce safe cannabis-based medicines. Our aim was to develop a generic supercritical fluid chromatography hyphenated to mass spectrometry (SFC-MS) method that could help in detecting such adulterations using representative synthetic cannabinoids from multiple classes. Method development started with a screening of stationary phases using seven different SFC-dedicated columns. The Torus 1-AA (amino-anthracene) provided the best retention and resolution for the analytes and was selected for the study. Likewise, the mobile phase modifier composition (methanol/water 98:2 v/v) was set after these preliminary tests. The next step performed was the optimization of the method using a design of experiments (DoE) and Bayesian design space (DS) methodology. The temperature, pressure, isocratic and gradient time were selected as parameters for the DoE (central composite design). The separation criterion (S) was set to -0.5 to maximize the separation capacity of the generic method. This Quality by Design (QbD) approach is advantageous as it permits the testing of various conditions within the design space (DS) to achieve a desirable separation since unassessed compounds will probably be encountered during routine analysis. Finally, the quantitative performances were demonstrated by means method validation based on total error approach for the quantification of a selected synthetic cannabinoid in fiber type cannabis plant matrix. Sample preparation was performed with solid-liquid extraction (SLE) followed by filtration and dilution. The acceptance limits were set at ±15% and the β-expectation tolerance limits at 90 % probability level. The results show that the method is valid over the whole dosing range assessed of 2.5 - 7.5% (w/w) with the LOD equal to 14.40 ng/mL. The implementation of this method should be straightforward considering the ease of sample preparation, the use of a fast and green SFC separation and the high specificity and sensitivity achieved with mass spectrometry. Ensuring medicinal cannabis quality is challenging and this work adds an innovative tool that should prove useful in the context of counterfeit drugs tracking. [less ▲]

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See detailComment garantir la fiabilité de vos futurs résultats ?
Jambo, Hugues ULiege; Hubert, Cédric ULiege; Hubert, Philippe ULiege

Scientific conference (2018, June 21)

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See detailSupercritical fluid chromatography: a promising alternative to current bioanalytical techniques
Dispas, Amandine ULiege; Jambo, Hugues ULiege; André, Sébastien ULiege et al

in Bioanalysis (2018), 10(2), 107-124

During the last years, chemistry was involved in the worldwide effort toward environmental problems leading to the birth of green chemistry. In this context, green analytical tools were developed as ... [more ▼]

During the last years, chemistry was involved in the worldwide effort toward environmental problems leading to the birth of green chemistry. In this context, green analytical tools were developed as modern Supercritical Fluid Chromatography in the field of separative techniques. This chromatographic technique knew resurgence a few years ago, thanks to its high efficiency, fastness and robustness of new generation equipment. These advantages and its easy hyphenation to MS fulfill the requirements of bioanalysis regarding separation capacity and high throughput. In the present paper, the technical aspects focused on bioanalysis specifications will be detailed followed by a critical review of bioanalytical supercritical fluid chromatography methods published in the literature. [less ▲]

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See detailQuality control of medicinal cannabis: implementation of a generic sfc-ms method to address counterfeiting with synthetic cannabinoids
Jambo, Hugues ULiege; Dispas, Amandine ULiege; Avohou, Tonakpon Hermane ULiege et al

Poster (2018)

There is a growing interest in using cannabis for medicinal purposes as research shows evidence of its therapeutic properties. However, to be successfully ported in the pharmaceutical field, several ... [more ▼]

There is a growing interest in using cannabis for medicinal purposes as research shows evidence of its therapeutic properties. However, to be successfully ported in the pharmaceutical field, several aspects such as its quality must be evaluated and ensured. In this context, we address the possibility of counterfeiting of cannabis with synthetic cannabinoids and report the development of a robust method based on supercritical fluid chromatography coupled with mass spectrometry (SFC-MS) that could help in detecting such adulterations. Considering the high number of already available synthetic cannabinoids and the high rate of development of novel structures, we aimed to develop a generic method suitable for the analysis of a large panel of substances using seventeen synthetic cannabinoids from multiple classes as model compounds. Firstly, a suitable column was chosen after a screening phase. The mobile phase (modifier composition) was also set after these preliminary tests. Secondly, a method optimization was carried out using a design of experiments (DoE) and Bayesian design space (DS) methodology that follows ICH Q8 R2 guideline recommendations. This approach is increasingly recommended for the robust optimization of analytical methods. The DoE selected was a four-factor central composite design. Then, according to the goal of adequately analyzing future unknown compounds, the criterion separation S was set to -0.5 to obtain a method with the highest separation capacity. This quality by design (QbD) approach shows flexibility as it permits the testing of various conditions within the DS to tune the separation taking into account that some adaptations might be needed during routine analysis, since it is impossible to predict which compound will be found. Finally, the quantitative performances of the method were demonstrated by means of a validation step based on total error approach for the quantification of a selected synthetic cannabinoid in fiber type cannabis plant matrix. Sample preparation was performed with solid-liquid extraction (SLE) followed by filtration and dilution. The acceptance limits were set at ±15% and the β- expectation tolerance limits at 90 % probability level. The results show that the method is valid over the whole dosing range assessed of 2.5 - 7.5% (w/w) and the LOD equal to 14.40 ng/mL. The implementation of this method should be straightforward considering the ease of sample preparation, the use of a simple modifier composition and the high specificity and sensitivity achieved with mass spectrometry. This work adds an innovative tool to address the challenges of ensuring medicinal cannabis quality and will prove useful in the context of counterfeit drugs tracking. [less ▲]

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See detailImplementation of a generic SFC-MS method for the quality control of potentially counterfeited medicinal cannabis with synthetic cannabinoids
Jambo, Hugues ULiege; Dispas, Amandine ULiege; Avohou, Tonakpon Hermane ULiege et al

in Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences (2018), 1092

In this study, we describe the development of a SFC-MS method for the quality control of cannabis plants that could be potentially adulterated with synthetic cannabinoids. Considering the high number of ... [more ▼]

In this study, we describe the development of a SFC-MS method for the quality control of cannabis plants that could be potentially adulterated with synthetic cannabinoids. Considering the high number of already available synthetic cannabinoids and the high rate of development of novel structures, we aimed to develop a generic method suitable for the analysis of a large panel of substances using seventeen synthetic cannabinoids from multiple classes as model compounds. Firstly, a suitable column was chosen after a screening phase. Secondly, optimal operating conditions were obtained following a robust optimization strategy based on a design of ex- periments and design space methodology (DoE-DS). Finally, the quantitative performances of the method were assessed with a validation according to the total error approach. The developed method has a run time of 9.4 min. It uses a simple modifier composition of methanol with 2% H2O and requires minimal sample pre- paration. It can chromatographically separate natural cannabinoids (except THC-A and CBD-A) from the syn- thetics assessed. Also, the use of mass spectrometry provides sensitivity and specificity. Moreover, this quality by design (QbD) approach permits the tuning of the method (within the DS) during routine analysis to achieve a desirable separation since the future compounds that should be analyzed could be unknown. The method was validated for the quantitation of a selected synthetic cannabinoid in fiber-type cannabis matrix over the range of 2.5% – 7.5% (w/w) with LOD value as low as 14.4 ng/mL. This generic method should be easy to implement in customs or QC laboratories in the context of counterfeit drugs tracking. [less ▲]

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See detailTowards a covering aerospray method for quantitative analyses of pharmaceutical tablets using surface-enhanced Raman chemical imaging (SER-CI)
Cailletaud, Johan ULiege; De Bleye, Charlotte ULiege; Dumont, Elodie ULiege et al

Conference (2017, September 22)

In recent years, the use of SERS-CI in pharmaceutical sciences has increased in order to study the distribution of low-dose compounds in solid dosage forms [1]. This technique allows to improve the ... [more ▼]

In recent years, the use of SERS-CI in pharmaceutical sciences has increased in order to study the distribution of low-dose compounds in solid dosage forms [1]. This technique allows to improve the sensitivity of conventional Raman microscopy and to reduce significantly the image acquisition time by exalting the signal information. However, the applications of SERS-CI in the pharmaceutical field remain limited, especially due to the difficulty of obtaining a homogeneous deposit of metallic nanoparticles on the sample surface. Generally, the covering method used on the tablet is a drop casting deposition due to its simplicity and rapidity of implementation. Despite the colloidal solution deposit is not fully controlled. The inhomogeneous covering is the result of the “coffee-ring” effect that concentrates the nanoparticles at the edges of the droplet [2]. This implies remarkable variations of the SERS analyte signal’s intensity at different places. For a more reproducible and homogeneous coating, an aerospray method using a homemade apparatus was developed (Figure 1). The device is composed with a pair of coaxial tubes, the colloidal solution is pulled through the inner tube from a syringe pump and the outer tube is connected to a source of high pressure gas. Nitrogen, used as a nebulizing gas, creates a flow of small droplets of nanoparticles that are nearly dry when they hit the sample surface. The aerospray device is easy to implement and the entire surface of the tablet is covered by the SERS substrate in a homogeneous way. By using this covering method, the potential of SERS-CI is improved and making it a suitable technique for quantitative analyses of low drug concentrations or impurities in pharmaceutical tablets. [less ▲]

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See detailTowards the development of a dual mode fluorescence/SERS dopamine aptasensor
Dumont, Elodie ULiege; De Bleye, Charlotte ULiege; Cailletaud, Johan ULiege et al

Poster (2017, September 21)

This work was dedicated to the development of a dual mode fluorescence and surface-enhanced Raman scattering (SERS) dopamine aptasensor. The preparation of the aptasensor was first optimised. Thereafter ... [more ▼]

This work was dedicated to the development of a dual mode fluorescence and surface-enhanced Raman scattering (SERS) dopamine aptasensor. The preparation of the aptasensor was first optimised. Thereafter, calibration curves were realised by means of fluorescence quenching and SERS. Finally, the specificity of both methods was tested. [less ▲]

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See detailDevelopment of SERS nanosensors for the detection of small bioactive molecules by cellular analysis in complex matrices: Application to dopamine
Dumont, Elodie ULiege; De Bleye, Charlotte ULiege; Cailletaud, Johan ULiege et al

Conference (2017, September 13)

This communication reports the different steps undertaken in order to develop a new Surface-Enhanced Raman Scattering (SERS) nanosensor for the quantification of dopamine in the culture medium of PC-12 ... [more ▼]

This communication reports the different steps undertaken in order to develop a new Surface-Enhanced Raman Scattering (SERS) nanosensor for the quantification of dopamine in the culture medium of PC-12 cells. First, the synthesis of the SERS substrate, gold nanoparticles, and its characterization. Then the development of the method with the help of a design of experiments and the demonstration of the specificity of the method over other structurally related catecholamines. And finally, the implementation of the method on the culture medium of PC-12 cells, on an HEPES buffer having served to wash the cells and on the PC-12 cells. [less ▲]

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