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See detailComparing the qualitative performances of handheld NIR and Raman spectrophotometers for the detection of falsified pharmaceutical products
Ciza Hamuli, Patient ULiege; Sacre, Pierre-Yves ULiege; Waffo Tchounga, Christelle ULiege et al

in Talanta (2019), 202

Over the last decade, the growth of the global pharmaceutical market has led to an overall increase of substandard and falsified drugs especially on the African market (or emerging countries). Recently ... [more ▼]

Over the last decade, the growth of the global pharmaceutical market has led to an overall increase of substandard and falsified drugs especially on the African market (or emerging countries). Recently, several methods using handheld/portable vibrational spectroscopy have been developed for rapid and on-field drug analysis. The objective of this work was evaluate the performances of various NIR and Raman handheld spectrophotometers in specific brand identification of medicines through their primary packaging. Three groups of drug samples (artemether-lumefantrine, paracetamol, and ibuprofen) were used in tablet or capsule forms. In order to perform a critical comparison, the analytical performances of the two analytical systems was compared statistically using three methods: hierarchical clustering algorithm (HCA), data-driven soft independent modeling of class analogy (DD-SIMCA) and hit quality index (HQI). The overall results show good detection abilities for NIR systems compared to Raman systems based on Matthews’s correlation coefficients, generally close to one. Raman systems are less sensitive to the physical state of the samples than the NIR systems, it also suffers of the auto-fluorescence phenomenon and the signal of highly dosed active pharmaceutical ingredient (e.g. paracetamol or lumefantrine) may mask the signal of low-dosed and weaker Raman active compounds (e.g. artemether). Hence, Raman systems are less effective for specific product identification purposes but are interesting in the context of falsification because they allow a visual interpretation of the spectral signature (presence or absence of API). [less ▲]

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See detailIntegrated microfluidic device for in-line monitoring of glyphosate assisted by Surface Enhanced Raman Spectroscopy
Emonds-Alt, Gauthier ULiege; Avohou, Tonakpon Hermane ULiege; Kasemiire, Alice ULiege et al

Conference (2019, June 17)

Glyphosate is one of the most widely used pesticides as it is a non-selective systemic herbicide that is quickly degrade in soil. Glyphosate disrupts the biochemical shikimate pathway, which produces ... [more ▼]

Glyphosate is one of the most widely used pesticides as it is a non-selective systemic herbicide that is quickly degrade in soil. Glyphosate disrupts the biochemical shikimate pathway, which produces aromatic amino acids that are essential for plant growth and development. It acts as a competitive inhibitor of the 5-enolpyruvylshikimate-3-phosphate (EPSP) synthase, an enzyme absent from mammals. Therefore, glyphosate has been presented as (a) non-toxic for humans and (b) non-persistent. However, these premises have been recently questioned since traces of glyphosate and its main metabolite (aminomethylphosphonic acid, AMPA) have been detected in surface water, groundwater, soil as well as in cotton products. Quantifying and monitoring trace amounts of glyphosate and pesticide residues in the environment typically relies on analytical methods such as Gas Chromatography (GC) or Liquid Chromatography (LC) coupled with mass spectrometry (MS). However, these types of methods are expensive and often not suitable for in situ field analysis. Surface Enhanced Raman Spectroscopy (SERS) coupled with microfluidic could be an alternative method, which allows a fast and direct quantification on the field with miniaturised instrumentation. Indeed, SERS combines the advantage of Raman spectroscopy and is able to detect traces due to the signal enhancement resulting from the adsorption of the analyte on the rough nanoparticle surface. Here we focus on the development of an inline analytical method for water monitoring assisted by SERS. The inline detection of glyphosate is performed in a microfluidic setup, constructed with high-purity PFA coils (1/16" o.d., 0.01" i.d.), divided in three compartments (Figure 1) : (a) in situ synthesis of silver nanoparticles (Ag NPs), (b) mixing of the analyte with the Ag NPs and (c) the detection zone. Experimental parameters such as the type of micromixers for the synthesis of Ag NPs and the mixing between glyphosate and Ag NPs, the concentration of reagents for the synthesis of Ag NPs, the residence time or the flow applied in the setup were investigated and optimized through D-optimal (26 runs) and I-optimal design of experiments. In particular, we will discuss how the experimental parameters influence the quantitative detection of SERS intensity. [less ▲]

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See detailComparison of hyperspectral imaging techniques for the elucidation of falsified medicines composition
Coic, Laureen ULiege; Sacre, Pierre-Yves ULiege; Dispas, Amandine ULiege et al

in Talanta (2019), 198

Hyperspectral imaging has shown a high potential to analyze falsifications of solid pharmaceutical products since the last decade. Thanks to the non-destructive, ecological and non-invasive properties, it ... [more ▼]

Hyperspectral imaging has shown a high potential to analyze falsifications of solid pharmaceutical products since the last decade. Thanks to the non-destructive, ecological and non-invasive properties, it is a preferred technique for these kinds of applications. Moreover, thanks to the spectroscopic properties, it is possible to detect as well organic compounds as inorganic compounds in a single analysis. Therefore, we recommend using it as second-line laboratory analysis technique. Raman microscopy and Fourier Transform Infrared (FT-IR) microscopy are two interesting techniques that are complementary. In this study, the potential of the two hyperspectral imaging techniques is evaluated to elucidate the composition of falsified antimalarial tablets. Hyperspectral data are analyzed by Multivariate Curve Resolution-Alternating Least Square (MCR-ALS). The results obtained from this study show that Raman hyperspectral imaging seems to be more suited to detect low dosed compounds possibly due to a smallest sampling volume. It has been also possible to link formulations of falsified samples of two different brands. [less ▲]

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See detailField survey to evaluate the prevalence of poor quality anti-infective medicines in Cameroon
Waffo Tchounga, Christelle Ange ULiege; Ciza Hamuli, Patient ULiege; Sacre, Pierre-Yves ULiege et al

Conference (2019, May 20)

Poor quality medicines pose a threat to all health systems. It is obvious that they have harmful consequences not only from the point of view of public health, but also from the economic and socio ... [more ▼]

Poor quality medicines pose a threat to all health systems. It is obvious that they have harmful consequences not only from the point of view of public health, but also from the economic and socio-economic point of view [1]. Over the past 15 years, substandards and falsified drugs have received increasing attention in scientific publications. However, there is little reliable data determining their prevalence with accuracy due to the scarcity of well-designed studies identified as having good methodological quality as well as representative sampling strategy [2-4]. In this context, we have decided to evaluate the prevalence of poor quality anti-infective medicines in two Cameroon areas (Yaoundé and Douala), inspired by the Medicines Quality Assessment Reporting Guidelines (MEDGUARG) [3] and WHO recommendations [4] for the sampling strategy and the methodology. Our study will focus on the formal private sector. Pharmacies as well as drugs products will be sampled by a stratified random sampling strategy. The study will focus on two anti-infective medicines (ciprofloxacin and metronidazole 500mg tablets) in tablets, from 96 outlets in the cities of Yaoundé and Douala that are the two main cities (Yaoundé and Douala) of Cameroon representing almost 70% of private outlets of the country. Mystery shoppers will collect samples using a specific scenario. As a prelude to our field study, screening and dosage methods have to be developed and validated in Liège University. They se methods consist of vibrational spectroscopy (near infrared and Raman spectroscopy) as first screening techniques and HPLC for identification and assay. For vibrational spectroscopy, qualitative models will be developed for identification using chemometric tools. HPLC methods will be validated following the total error approach using accuracy profile as decision tool. The medicines collected will be first analysed visually (physical appearance tests), then field methods will be implemented (screening methods: Paper Analytical Devices (PADs), handled NIR device). Finally laboratory testing (assay and confirmation methods: HPLC reference method and pharmacotechnical tests) will be performed at LANACOME (Yaoundé, Cameroon). Suspect and unusual samples will be transported to Liège University for further analyses. All these methods will be applied according to a decision tree based on observed facts. The study will be submitted to the ethics committee of the Ministry of Health in Cameroon. An accurate and fast HPLC method for identification and quantification of both metronidazole and ciprofloxacin has been developed. Identification models for some brands of ciprofloxacin and metronidazole using handled NIR and Raman devices has been developed before implementation on field. This study will allow us to evaluate not only the prevalence of poor quality anti-infective medicines marketed in Cameroon but also outlets dispensing substandard and falsified medicines. They will be distinguished into sub-standard, degraded or falsified and classified according to their country of origin, manufacturer and city of sampling. The results will be notified to the drug regulatory authority in Cameroon and if poor quality medicines are detected, we will proceed with an alert to the WHO Global Surveillance System. The estimation of the prevalence of counterfeit and falsified anti-infective medicines would be extrapolated to the entire population and depending on the information obtained, evaluate the patient health risk exposed to substandard and falsified anti-infective medicines and develop capacity-building interventions in the fight against poor quality medicines. [less ▲]

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See detailHANDHELD RAMAN SPECTROSCOPY: AN ESSENTIAL TOOL TO TACKLE THE SUBSTANDARD MEDICINES ISSUE?
Coic, Laureen ULiege; Sacre, Pierre-Yves ULiege; Dispas, Amandine ULiege et al

Conference (2019, May 20)

According to the World Health Organization, there is a growing concern about the quality of medicines around the world. Indeed, more and more substandard and falsified medicines are identified. That is ... [more ▼]

According to the World Health Organization, there is a growing concern about the quality of medicines around the world. Indeed, more and more substandard and falsified medicines are identified. That is why several spectroscopic techniques such as Raman, near- or mid-infrared spectroscopy, have gained great interest for this purpose. By means of chemometrics, interesting results have been shown in terms of elucidation of falsified medicines composition by hyperspectral imaging (L. Coic) and with benchtop spectrophotometers (O.Ye. Rodionova). However, these instruments are rather expensive, heavy and are not appropriated for low and middle-income countries. To circumvent these issues, several low-cost and middle-cost handheld spectrophotometers have been developed. In some cases of falsification, there is presence of a wrong or an absence of active pharmaceutical ingredient (API) that is often easy to prove with spectroscopy. However, the major part of the burden is constituted of lower dosed API that is trickier to evaluate in the field with conventional tools. In this study, the potential of handheld Raman spectroscopy to assay API in a solid dosage form was evaluated. For this purpose, fifteen formulations with a various proportion of mannitol and microcrystalline cellulose, seven level of concentration of ibuprofen (14 % – 26 % (m/m)) were produced thanks to a design of experiments, following the ICH Q3 guidelines. The calibration set was realized by analysing 3 tablets per formulation and each tablet was assayed using a previously validated benchtop NIR model. The PLS model was developed using PLS-Toolbox running in a Matlab® environment. The PLS model calibration has shown very nice results, with a R² of calibration / R² of cross-validation of 0.981 / 0.968 and a RMSECV of 0.83% (m/m). As explained, the validation set was projected on model and showed a RMSEP of 0.89 % (m/m). Then, the quantitative model has been validated following the total error approach with 4 series, 5 levels of concentration and 3 replicates. The acceptance limits were set at +/-15 % following the European Pharmacopeia criteria for uniformity of content. In a nutshell, handheld Raman spectrophotometer has shown very interesting results for studied formulation. Thanks to the 14 – 26 % (m/m) range, the model could be applied to get the quantitative information of the dosage of substandard medicines on the field. [less ▲]

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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 detailVibrational spectroscopy in analysis of pharmaceuticals: Critical review of innovative portable and handheld NIR and Raman spectrophotometers
Deidda, Riccardo ULiege; Sacre, Pierre-Yves ULiege; Clavaud, Matthieu et al

in TrAC: Trends in Analytical Chemistry (2019), 114

The fast pace of changes occurring in the pharmaceutical world emphasizes the need for powerful technologies that allow checking the quality of pharmaceutical products. Infrared and Raman spectroscopies ... [more ▼]

The fast pace of changes occurring in the pharmaceutical world emphasizes the need for powerful technologies that allow checking the quality of pharmaceutical products. Infrared and Raman spectroscopies have shown great potentialities for drug analysis in the last decades and consequently caught the attention of the scientific world as well as of industrial developers, leading to major technological advancements. These fast, eco-friendly, and non-destructive techniques help gather essential information about the samples under examination with consistent advantages. This review focuses on the application of portable/handheld NIR and Raman spectrophotometers in the analysis of pharmaceutical products for both in-process and quality control tests. Moreover, several analytical methods developed by several authors are described in order to illustrate the applications explored until now. [less ▲]

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See detailProcess Analysis - Overview
Ziemons, Eric ULiege; Hubert, Cédric ULiege; Hubert, Philippe ULiege

in Miro, Manuel; Worsfold, Paul; Townshend, Alan (Eds.) et al Encyclopedia of Analytical Science (2019)

Process analysis is the application of analytical science to the monitoring and control of industrial processes. The data obtained from process analysis allow the optimization, dynamic changes, monitoring ... [more ▼]

Process analysis is the application of analytical science to the monitoring and control of industrial processes. The data obtained from process analysis allow the optimization, dynamic changes, monitoring or quality control of industrial processes by providing information from which the chemical and/or physical composition of the process stream can be inferred. [less ▲]

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See detailProcess Analysis: Maintenance, Reliability, and Training
Hubert, Cédric ULiege; Widart, Joëlle ULiege; Ziemons, Eric ULiege et al

in Encyclopedia of Analytical Science 3rd Edition (2019)

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See detailOptimisation of a surface enhanced Raman scattering method using design of experiments and Bayesian design space modelling
Deidda, Riccardo ULiege; Avohou, Tonakpon Hermane ULiege; Kasemiire, Alice ULiege et al

Poster (2019, January 30)

Surface enhanced Raman scattering (SERS) is an alternative technique based on Raman spectroscopy, which has been increasingly applied to pharmaceutical analytical chemistry in the last decade. It consists ... [more ▼]

Surface enhanced Raman scattering (SERS) is an alternative technique based on Raman spectroscopy, which has been increasingly applied to pharmaceutical analytical chemistry in the last decade. It consists in enhancing the Raman effect by performing analyses using metallic surfaces, such as silver and gold colloids, on which the target molecules are adsorbed to be detected. It has been observed that in this way, an enhancement factor of 103-106 times can be obtained and the lack of sensibility related to conventional Raman scattering overcome [1]. Nowadays, design of experiment (DoE) is widely employed for modelling phenomena in analytical method development and optimisation, especially in the context of separation techniques. It is a structured approach that allows correlating key responses to controllable variables. Ideally, a certain number of factors may affect the critical method attributes (CMAs) of an analytical process in a negative or positive way. These factors are named critical method parameters (CMPs). DoE is employed, as a chemometric tool, to individuate CMPs and then, deeply study how they affect the process under study. To do so, CMAs are linked to CMPs by a regression model built by means of multivariate linear or partial least squares regression. Generally, the designs can be classified in two categories: screening and optimization designs. The formers are generally implemented when a high number of parameters are supposed to influence the analytical process and no much prior information is available. They result in useful tools to study the effects of both continuous and discontinuous factors. Instead, the optimisation designs are principally used to study wisely selected continuous factors [2]. The design space (DS) is defined as a multidimensional area in which the specifications given to the CMAs are met with a defined level of probability. Obviously, the larger the DS is, the more robust the method is. Its computation is achieved by several approaches, such as Monte-Carlo simulations, Bayesian methods as well as bootstrapping techniques [3]. The aim of this project was to combine and apply two potent chemometric tools such as DoE and Bayesian DS to SERS method development and optimisation. [1] Cailletaud, J., De Bleye, C., Dumont, E., Sacré, P.-Y., Netchacovitch, L., Gut, Y., Boiret, M., Ginot, Y.-M., Hubert, P., Ziemons, E., Critical review of surface-enhanced Raman spectroscopy applications in the pharmaceutical field. J. Pharm. Biomed. Anal. 147, 458-472, 2018. [2] Sahu, P.K., Ramisetti, N.R., Cecchi, T., Swain, S., Patro, C.S., Panda, J., An overview of experimental design in HPLC method development and validation, J. Pharm. Biomed. Anal. 147, 590-611, 2018. [3] Deidda, R., Orlandini, S., Hubert, P., Hubert, C., Risk-based approach for method development in pharmaceutical quality control context: A critical review. J. Pharm. Biomed. Anal. 161, 110-121, 2018. [less ▲]

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See detailUpdate of the progresses and development prospects of the FEDER project Phare
Emonts, Paul ULiege; Penoy, Noémie ULiege; Rocks, Natacha ULiege et al

Scientific conference (2019, January 19)

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See detailAuthentication of falsified medicine tablets by handheld Raman spectroscopy class modeling
Coic, Laureen ULiege; Sacre, Pierre-Yves ULiege; Avohou, Tonakpon Hermane ULiege et al

Conference (2019, January 01)

Since last decades, the world has known significant changes in the pharmaceutical products sale. The emergence of the internet trade is an important issue because it is easy to sell medicines without ... [more ▼]

Since last decades, the world has known significant changes in the pharmaceutical products sale. The emergence of the internet trade is an important issue because it is easy to sell medicines without passing any control. Moreover, in low- and middle-income countries (LMIC), the number of local pharmacies has grown, increasing the risk to have substandard or falsified medicines. Indeed, according to the World Health Organization (WHO) it is difficult to ensure quality medicines due to areas conflict, corrupted governments and poor health system [1]. For that reason, several analytical techniques have been developed since last decade. One of the most interesting tool is the Minilab, developed by the Global Pharma Health Fund (GPHF), which is a mobile mini-laboratory for fast drug quality control. Moreover, Raman spectroscopy has gained a great interest because it can be used at any step of analytical chain or on the fieldwork with handheld devices. However, spectroscopic data implies development of chemometrics models to gather relevant information. Several unsupervised techniques have already been used to authenticate drug products [2-3]. Due to the intrinsic properties of classification methods, class modeling is more appropriated to this kind of analysis. Indeed, falsified medicines can be quite different from the calibration set, so that, it does not have sense to attribute a class meanwhile it is dissimilar to the calibration set. In this study, the performances of two class-modeling techniques will be evaluated on handheld Raman spectra, to separate falsified medicines from authentic drugs. Three different generics of paracetamol, ibuprofen and artemether-lumefantrine with different dosage, dosage form and formulations were analyzed. Most of them were gathered in local Belgium pharmacies and other were gathered in Africa (artemether-lumefantrine formulations). Samples were analyzed with a handheld Raman spectrophotometer Pharma 21CFR part 11 qualified (Truscan RM, Thermo Scientific, USA) directly through the blister. In order to have a good representativeness of intra-batch variability, 10 tablets were analyzed per sample. The acquisition parameters were set to default. Two models were tested: one-class PLS (OC-PLS) [4] and the data driven-soft independent modeling class analogy (DD-SIMCA) [5]. All the computations were done in Matlab® (R2017b). The calibration and validation set was the same for each model and composed of 60 spectra for each, with different batch number. Because of the nature of each algorithm, there is a significant difference in terms of separation. Looking at Figure 1, the separation of dosage form for ibuprofen is much different between the two models. For the DD-SIMCA, it is more difficult to separate the long acting release from the soft capsule/coated tablet compared to the OC-PLS model. For the other API, similar results are obtained for the dosage and for the brand. It seems that the OC-PLS is more sensitive to the small spectral variabilities. In the case of artemether-lumefantrine formulations, the separation between samples is much more difficult. Indeed, the lumefantrine is a high Raman scatterer. This can explain that the signal of artemether and excipients is difficult to access. Elsewhere, in terms of development, the DD-SIMCA is much harder to optimize because there are more tunable parameters than for OC-PLS. Furthermore, both models are really influenced by spectral pretreatment. An optimization has to be done for each. The authentication of pharmaceutical products by handheld Raman spectroscopy has been possible thanks to class modeling. Both tested algorithms shown interesting results regarding the separation of samples depending on their characteristics. The optimization of data processing and pre-processing is the key-step to improve as sensitivity as specificity of both class modeling methods. [less ▲]

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See detailVibra-Santé Hub
De Bleye, Charlotte ULiege; Widart, Joëlle ULiege; Sacre, Pierre-Yves ULiege et al

Poster (2018, December 19)

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See detailDevelopment and optimization of a derivatization protocol for phenethylamine compounds using FITC-CE-LIF method
Emonts, Paul ULiege; Dispas, Amandine ULiege; Ninane, Caroline et al

Poster (2018, December 19)

In the framework of the development of an innovative microfluidic system based on capillary electrophoresis separation, we optimized a fluorescein isothiocyanate (FITC) derivatization protocol for Laser ... [more ▼]

In the framework of the development of an innovative microfluidic system based on capillary electrophoresis separation, we optimized a fluorescein isothiocyanate (FITC) derivatization protocol for Laser Induced Fluorescence (LIF) detection. The microfluidic device will present a high sensitivity thanks to the fluorescence detection and an innovative hydrodynamic injection approach. To highlight the analytical performances of this microfluidic system, we will use synthetic cathinones (and some derivatives) as targeted compounds. They present a panel of closely related structures and isobaric compounds. In addition to analytical challenges, this category of drugs is a current topic regarding to public health. Indeed synthetic cathinones were described as the second most frequently seized group of new psychoactive substances in EU in 2016. Moreover some of them are currently sell on internet as bath salts without any legislation. In this context, fast, easy and reliable analytical tools are required to track and quantify these compounds. In the present study, we initiated the optimization of the derivatization of model compounds (phenethylamine family) using FITC. The panel of model analytes includes primary and secondary amino groups to be representative of future real samples. Design of experiments strategy was used to optimize the derivatization protocol in order to reach an easy sample preparation and to maximize the derivatization efficiency. Finally, the CE developed method will be transferred to the microfluidic system. Then separation performances comparison of traditional CE-LIF vs µCE-LIF will allow to highlight the advantages of microfluidics such as the lower amount of sample required, the gain in time and money, the significant decrease of solvent and its compact size. [less ▲]

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See detailDevelopment of graphical user interface (GUI) for database building and for falsification applications
Coic, Laureen ULiege; Sacre, Pierre-Yves ULiege; Dispas, Amandine ULiege et al

Scientific conference (2018, December 19)

Inside a research unit, there are several kind of information which are gathered in a continuous flow from operators. It is important to centralize all of the information not to lose any interesting ... [more ▼]

Inside a research unit, there are several kind of information which are gathered in a continuous flow from operators. It is important to centralize all of the information not to lose any interesting result. Because of the cost and/or the non-applicability of commercial database software, it is interesting to build its own one. Indeed, in the case of spectroscopic data, the use of a market database software is not user-friendly because, stored data cannot be directly manipulated in multivariate analyses applications. The database under development actually contains the data of various pharmaceutical samples (genuine and falsified) obtained on several spectroscopic devices. For this application, a Matlab® graphical user interface (GUI) is being developed. It provides the access to spectroscopic data for any operator and allows the automatic implementation of new instruments and/or new formulation groups. Moreover, in case of falsification suspicion, another GUI has been developed to provide qualitative information regarding the composition of the medicines. It is an interesting tool because it provides an instantaneously visual comparison between reference database and the unknown spectrum. Moreover, statistical tools, as Hit Quality Index or correlation coefficient, can provide a numerical result to quantify the match between spectra. In the future, results from other kind of techniques (e.g. HPLC, dissolution curves, photos) will be added to centralize samples information. [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 detailRaman chemical imaging, a new tool in kidney stone structure analysis: Case-study and comparison to Fourier Transform Infrared spectroscopy
Castiglione, Vincent ULiege; Sacre, Pierre-Yves ULiege; Cavalier, Etienne ULiege et al

Poster (2018, November 16)

The kidney stone’s structure might provide clinical information in addition to the stone composition. The Raman chemical imaging is a technology used for the production of two- dimension maps of the ... [more ▼]

The kidney stone’s structure might provide clinical information in addition to the stone composition. The Raman chemical imaging is a technology used for the production of two- dimension maps of the constituents’ distribution in samples. We aimed at determining the use of Raman chemical imaging in urinary stone analysis. Fourteen calculi were analyzed by Raman chemical imaging using a confocal Raman micro- spectrophotometer. They were selected according to their heterogeneous composition and morphology. Raman chemical imaging was performed on the whole section of stones. Once acquired, the data were baseline corrected and analyzed by MCR-ALS. Results were then compared to the spectra obtained by Fourier Transform Infrared spectroscopy. [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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