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See detailQualitative and quantitative analyses of a pharmaceutical formulation produced by hot melt extrusion using Raman spectroscopy
Netchacovitch, Lauranne ULg; De Bleye, Charlotte ULg; Sacre, Pierre-Yves ULg et al

Poster (2014, May 15)

In the pharmaceutical industry, Hot Melt Extrusion (HME) is a recent technique used to integrate poor water soluble drugs in pharmaceutical formulations. Indeed, more and more active pharmaceutical ... [more ▼]

In the pharmaceutical industry, Hot Melt Extrusion (HME) is a recent technique used to integrate poor water soluble drugs in pharmaceutical formulations. Indeed, more and more active pharmaceutical ingredients (API) belong to the Biopharmaceutical Classification System (BCS) II and IV. Their integration in pharmaceutical solid forms is a big deal. HME processes increase the bioavailability and the solubility of those API by encompassing them in a polymeric carrier and by forming solid dispersions [1]. Moreover, in 2004, the FDA’s guidance initiative promoted the usefulness of Process Analytical Technology (PAT) tools when developing a manufacturing process. Vibrational spectroscopy is an appropriate PAT tool to analyze extrudates [2 – 3]. In this case, Raman spectroscopy, which belongs to vibrational spectroscopy, was used to analyze itraconazole extrudates qualitatively and quantitatively. During HME, the main objective is to develop solid dispersions by converting a crystalline API in an amorphous one, in order to improve its solubility and bioavailability [4]. According to Raman spectra, it is possible to identify the polymorphic form of the components in the extrudates by integrating or rationing the Raman bands that are characteristic of the API or by calculating the width at half intensity of some bands [5]. After determining the polymorphic form of the API, a quantitative method was developed in order to measure the ratio between the API and the polymer. Finally, chemical imaging was performed on extrudates to identify the distribution of the homogeneity of the API inside the polymer [6]. In conclusion, Raman spectroscopy is an appropriate tool to follow an extrusion process. By qualitative and quantitative analyses it is possible to determine the composition, the polymorphic form, the homogeneity, and the concentration of pharmaceutical matrices according to Raman fingerprint. References: [1] S. Shah et. al., Int J Pharm 453 (2013) 233 – 252. [2] L. Saerens et. al., Anal Chem 85 (2013) 5420 – 5429. [3] T. De Beer et. al., J Pharm Biomed Anal 48 (2008) 772 – 779. [4] A. Sarode et. al., Eur J Pharm Sci 48 (2013) 371 – 384. [5] E. Widjaja et. al., Eur J Pharm Sci 42 (2011) 45 – 54. [6] J. M. Amigo, Anal Bioanal Chem 398 (2010) 93 – 109. [less ▲]

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See detailDevelopment of an analytical method to detect simultaneously bisphenols using a multiplexed surface-enhanced Raman scattering quantitative approach
De Bleye, Charlotte ULg; Dumont, Elodie ULg; Sacre, Pierre-Yves ULg et al

Poster (2014, May 15)

Over the last decade, bisphenol A (BPA) attracted a lot of attention. This molecule, commonly used as a precursor to produce epoxy-resin and plastics, is an endocrine disruptor presenting an estrogenic ... [more ▼]

Over the last decade, bisphenol A (BPA) attracted a lot of attention. This molecule, commonly used as a precursor to produce epoxy-resin and plastics, is an endocrine disruptor presenting an estrogenic activity [1]. Despite its health toxicity, BPA is present in a broad variety of consumer goods released from plastic bottles and packaging for example. Since the discovery of its adverse health effect of BPA, the manufacturers tend to use structural analogues of BPA such as BPS, BPF and BPB to produce plastic materials [2]. However, the health safety of these molecules is still not demonstrated. Currently, bisphenols are actively researched and quantified using solid phase extraction and chromatography techniques which are time and solvents consuming. Therefore, it could be very interesting to quantify simultaneously bisphenols using a fast and “green” technique. Surface-enhanced Raman scattering (SERS) exalts dramatically the Raman scattering of molecules adsorbed or very closed to metallic surface enabling to detect very low amounts of analytes while keeping the structural information obtained from the spectrum which is very interesting to consider multiplexed analyses [3-4]. Moreover, SERS, which is a solvent free and fast acquisition technique, is an attractive tool in “Green Chemistry” [5]. In this context, the development of a multiplexed quantitative approach to detect bisphenol was considered. Silver nanoparticles (AgNps) were selected as SERS substrate and their functionalization was investigated taking into account the weak affinity of phenolic molecules for gold and silver surface [6]. Pyridine was selected as surface modifier and allowed to attract bisphenols around metallic surface thanks to hydrophobic interaction and hydrogen bonds [7]. Afterwards, the SERS samples preparation was optimized playing on the concentrations of pyridine and aggregating agent used to get the nanoparticles closer to each other which promotes the SERS effect. Tap water samples were spiked with different concentration of BPA from 5 ppb to 1000 ppb and analyzed using the optimized SERS sample preparation. A good linearity of the response was observed and a calibration curve with coefficient of determination (R2) of 0.9922 was obtained by plotting the intensity of a principal band of BPA versus the concentration. This last step was repeated using BPB as analyte and a calibration curve with a R2 of 0.9991 was obtained for the same range of concentration using a specific band intensity of BPB. Finally, tap water samples were spiked with different concentrations of BPA and BPB simultaneously and analyzed using SERS and it was possible to detect selectively the two molecules thanks to specific bands and a good linearity of the response was observed for both. To conclude, promising results were obtained which pave the way to “green” multiplexed quantitative analyses of very low concentrated analytes using SERS. References: [1] J.-H. Kang et al., Toxicology 226 (2006) 79-89 [2] C. Liao et al., J. Agric. Food Chem. 61 (2013) 4655-4662 [3] K. Kneipp et al., Chem. Rev. 99 (1999) 2957-2975. [4] R.F. Aroca et al., Adv.Colloid Interface Sci. 116 (2005) 45-61. [5] C. De Bleye et al., Talanta 116 (2013) 899-905. [6] X.X. Han et al., Anal. Chem., 83 (2011) 8582-8588. [7] B. San Vicente et al., Anal. Bioanal. Chem. 380 (2004) 115-122. [less ▲]

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See detailLutter contre le fléau des médicaments contrefaits
Rudaz, Serge; Hubert, Philippe ULg

in Spectra Analyse (2014), 298

Editorial

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See detailLa spectroscopie proche infrarouge, une technique non destructive dans la lutte contre la contrefaçon des médicaments
Mbinze Kindenge, Jérémie ULg; Kalenda Tshilombo, Nicodème; Chavez, Pierre-François ULg et al

in Spectra Analyse (2014), 43

Near infrared spectroscopy is a very promising and expanding analytical technique. It has to be noted that this technique is becoming more used in the pharmaceutical field for the quality control of ... [more ▼]

Near infrared spectroscopy is a very promising and expanding analytical technique. It has to be noted that this technique is becoming more used in the pharmaceutical field for the quality control of products. Indeed near infrared spectroscopy allows to perform fast, non-destructive, versatile analysis of the sample and minimization of the sample preparation. Based on those advantages, this spectroscopic method is one of the first reliable analytical techniques for fighting against counterfeit medicines. [less ▲]

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See detailStratégies analytiques pour la détection de contrefaçons de médicaments pour la dysfonction érectile
Sacre, Pierre-Yves ULg; Deconinck, Eric; Marini Djang'Eing'A, Roland ULg et al

in Spectra Analyse (2014), 43

Erectile dysfunction drugs are among the most counterfeit drug classes in industrialized countries. To fight against this plague, several analytical approaches are available for control laboratories. The ... [more ▼]

Erectile dysfunction drugs are among the most counterfeit drug classes in industrialized countries. To fight against this plague, several analytical approaches are available for control laboratories. The present article reviews the main used techniques and concludes presenting a general strategy for the detection and handling of drug counterfeits. [less ▲]

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See detailMéthodes chromatographiques génériques de criblage pour lutter contre les médicaments de qualité inférieure
Habyalimana, Védaste; Kalenda Tshilombo, Nicodème; Dispas, Amandine ULg et al

in Spectra Analyse (2014), 43

Poor quality medicines are a danger and a threat to public health. In this context, several generic analytical methods have been developed to screen molecules of interest grouped by pharmacological class ... [more ▼]

Poor quality medicines are a danger and a threat to public health. In this context, several generic analytical methods have been developed to screen molecules of interest grouped by pharmacological class using an innovative strategy based on design of experiments followed in some cases by independent component analysis and calculation of design space. Once validated via the classical total error measurement approach, these methods were applied to quantify antimalarial, non-steroidal anti-inflammatory and antibiotic medicines. Alarming results regarding the dosage of these drugs widely used by people confirm the need to fight against this scourge. [less ▲]

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See detailTowards a real time release approach for manufacturing tablets using NIR spectroscopy
Pestieau, Aude ULg; Krier, Fabrice ULg; Thoorens, Grégory et al

in Journal of Pharmaceutical & Biomedical Analysis (2014), 98

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See detailContribution à l'amélioration de l'accès à une eau potable de qualité pour les populations de la région nord du Burkina Faso
Some, Issam; Guel, Boubié; Hantson, Anne-Lise et al

Poster (2014, March 19)

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See detailDevelopment of a quantitative approach using surface-enhanced Raman chemical imaging: First step for the determination of an impurity in a pharmaceutical model
De Bleye, Charlotte ULg; Sacre, Pierre-Yves ULg; Dumont, Elodie ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (2014), 90

This publication reports, for the first time, the development of a quantitative approach using surface-enhanced Raman chemical imaging (SER-CI). A pharmaceutical model presented as tablets based on ... [more ▼]

This publication reports, for the first time, the development of a quantitative approach using surface-enhanced Raman chemical imaging (SER-CI). A pharmaceutical model presented as tablets based on paracetamol, which is the most sold drug around the world, was used to develop this approach. 4-Aminophenol is the main impurity of paracetamol and is actively researched in pharmaceutical formulations because of its toxicity. As its concentration is generally very low (<0.1%, w/w), conventional Raman chemical imaging cannot be used. In this context, a SER-CI method was developed to quantify 4-aminophenol assessing a limit of quantification below its limit of specification of 1000 ppm. Citrate-reduced silver nanoparticles were used as SERS substrate and these nanoparticles were functionalized using 1-butanethiol. Different ways to cover the tablets surface by butanethiol-functionalized silver nanoparticles were tested and a homogeneity study of the silver nanoparticles covering was realized. This homogeneity study was performed in order to choose the best way to cover the surface of tablets by silver colloid. Afterwards, the optimization of the SER-CI approach was necessary and different spectral intensity normalizations were tested. Finally, a quantitative approach using SER-CI was developed enabling to quantify 4-aminophenol from 0.025% to 0.2% in paracetamol tablets. This quantitative approach was tested on two different series of tablets using different batches of silver nanoparticles. [less ▲]

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See detailDevelopment of a liquid chromatographic method for thesimultaneous quantification of curcumin, -arteether,tetrahydrocurcumin and dihydroartemisinin. Application to lipid-based formulations
Memvanga Bondo, Patrick; Mbinze Kindenge, Jérémie ULg; Rozet, Eric ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (2014), 88(-), 447-456

A liquid chromatographic method was developed for the simultaneous separation of curcumin, B-arteether, tetrahydrocurcumin and dihydroartemisinin based on the design of experiments and the design space ... [more ▼]

A liquid chromatographic method was developed for the simultaneous separation of curcumin, B-arteether, tetrahydrocurcumin and dihydroartemisinin based on the design of experiments and the design space methodology. The influence of the percentage of organic modifier, flow rate of the mobile phase and column temperature on the analytes separation was investigated. The optimal chromatographic separation was achieved on a C18 column (125 mm × 4 mm, 5 µm) using an isocratic elution with a mobile phase consisting of methanol:ammonium acetate (pH 4; 10 mM) (80/20, v/v) at a flow rate of 0.45 ml/min and a column temperature of 32.5◦C. This method was then validated for simultaneous quantification of curcumin and B -arteether contained in lipid-based formulations taking into account the B -expectation tolerance interval for the total error measurement. Finally, the suitability of the proposed liquid chromatographic method for routine analysis of curcumin and B -arteether loaded in lipid-based formulations has been proven. [less ▲]

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See detailImprovement of a stability-indicating method by Quality-by-Design versus Quality-by-Testing: A case of a learning process
Hubert, Cédric ULg; Lebrun, Pierre ULg; Houari, Sabah ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (2014), 88

The understanding of the method is a major concern when developing a stability-indicating method and even more so when dealing with impurity assays from complex matrices. In the presented case study, a ... [more ▼]

The understanding of the method is a major concern when developing a stability-indicating method and even more so when dealing with impurity assays from complex matrices. In the presented case study, a Quality-by-Design approach was applied in order to optimize a routinely used method. An analytical issue occurring at the last stage of a long-term stability study involving unexpected impurities perturbing the monitoring of characterized impurities needed to be resolved. A compliant Quality-by-Design (QbD) methodology based on a Design of Experiments (DoE) approach was evaluated within the framework of a Liquid Chromatography (LC) method. This approach allows the investigation of Critical Process Parameters (CPPs), which have an impact on Critical Quality Attributes (CQAs) and, consequently, on LC selectivity. Using polynomial regression response modeling as well as Monte Carlo simulations for error propagation, Design Space (DS) was computed in order to determine robust working conditions for the developed stability-indicating method. This QbD compliant development was conducted in two phases allowing the use of the Design Space knowledge acquired during the first phase to define the experimental domain of the second phase, which constitutes a learning process. The selected working condition was then fully validated using accuracy profiles based on statistical tolerance intervals in order to evaluate the reliability of the results generated by this LC/ESI-MS stability-indicating method. A comparison was made between the traditional Quality-by-Testing (QbT) approach and the QbD strategy, highlighting the benefit of this QbD strategy in the case of an unexpected impurities issue. On this basis, the advantages of a systematic use of the QbD methodology were discussed. [less ▲]

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See detailQuantitative approaches based on Surface-Enhanced Raman Scattering (SERS) and Surface-Enhanced Raman Chemical Imaging (SER-CI)
De Bleye, Charlotte ULg; Sacre, Pierre-Yves ULg; Dumont, Elodie ULg et al

Conference (2014, January 20)

Surface-enhanced Raman scattering (SERS), discovered in 1978, is a recent technique enabling to circumvent the main limitations of classical Raman spectroscopy by dramatically exalting the Raman ... [more ▼]

Surface-enhanced Raman scattering (SERS), discovered in 1978, is a recent technique enabling to circumvent the main limitations of classical Raman spectroscopy by dramatically exalting the Raman scattering of the target molecules which are adsorbed or very closed to metallic surfaces while reducing the fluorescence impact on spectra [1]. This technique combines the sensitivity of the fluorescence keeping the structural information of molecules obtained from the SERS spectrum [2]. This last point allows to implement multiplex analyses. Moreover, it is possible to perform Surface-enhanced Raman chemical imaging (SER-CI) analyses which enable to acquire a visual representation of samples combining spectral and spatial measurements. Therefore SERS could become an attractive technique in numerous fields such as pharmaceutical and biomedical research. In this context, the feasibility of developing quantitative approaches using SERS and SER-CI on a pharmaceutical model was studied. The aim was to develop methods allowing the quantification of 4-aminophenol (4-AP) in a pharmaceutical formulation based on paracetamol. 4-AP is the main impurity of paracetamol and is actively research because of its toxicity. This pharmaceutical model was first investigated using SERS and a quantitative method enabling to quantify 4-AP from 3 to15 µg/mL was developed and validated using the standard addition method as a calibration method [3]. From these results, the possibility of developing a quantitative approach using SER-CI was investigated. Tablets based on paracetamol comprising different concentrations of 4-AP were prepared. Different ways to cover the sample surface by the SERS substrate were tested and a homogeneity study was performed to improve the repeatability of SER-CI analyses. Different spectral intensity normalizations were also tested in order to optimize the SER-CI method. Finally, a quantitative approach using SER-CI was developed allowing the quantification of 4-AP from 0.025% to 0.2% (w/w) in paracetamol tablets [4]. This first quantitative approach could pave the way to quantitative analysis of small molecules using SER-CI in complex matrices. References [1] P.L. Stiles, J.A. Dieringer, N.C. Shah, R.P. Van Duyne, Annu. Rev. Anal. Chem. 1 (2008) 601-626. [2] R.F. Aroca, R.A. Alvarez-Puebla, N. Pieczonka, S. Sanchez-Cortez, J.V. Garcia-Ramos, Adv. Colloid Interface Sci. 116 (2005) 45-61. [3] C. De Bleye, E. Dumont, E. Rozet, P.-Y. Sacré, P.-F. Chavez, L. Netchacovitch, G. Piel, Ph. Hubert, E. Ziemons, Talanta 116 (2013) 899-905. [4] C. De Bleye, P.-Y. Sacré, E. Dumont, L. Netchacovitch, P.-F. Chavez, G. Piel, P. Lebrun, Ph. Hubert, E. Ziemons, J. Pharm. Biomed. Anal. (in Press) [less ▲]

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See detailRobust method optimization strategy – a useful tool for method transfer: the case of SFC
Dispas, Amandine ULg; Lebrun, Pierre ULg; Andri, Bertyl ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (2014), 88

The concept of Quality by Design (QbD) is now well established in pharmaceutical industry and should be applied to the development of any analytical methods. In this context, the key concept of Design ... [more ▼]

The concept of Quality by Design (QbD) is now well established in pharmaceutical industry and should be applied to the development of any analytical methods. In this context, the key concept of Design Space (DS) was introduced in the field of analytical method optimization. In chromatographic words, the DS is the space of chromatographic conditions that will ensure the quality of peaks separation, thus DS is a zone of robustness. In the present study, the interest of robust method optimization strategy was investigated in the context of direct method transfer from sending to receiving laboratory. The benefit of this approach is to speed up the method life cycle by performing only one quantitative validation step in the final environment of method use. A Supercritical Fluid Chromatography (SFC) method previously developed was used as a case study in this work. Moreover, the interest of geometric transfer was investigated simultaneously in order to stress a little bit more the transfer exercise and, by the way, emphasize the additional benefit of DS strategy in this particular context. Three successful transfers were performed on two column geometries. In order to compare original and transferred methods, the observed relative retention times (RT) were modelled as a function of the predicted relative RT and of the method type (original or transferred). The observed relative RT of the original and transferred methods are not statistically different and thus the method transfer is successfully achieved thanks to the robust optimization strategy. Furthermore, the analytical method was improved considering analysis time (reduced five times) and peak capacity (increased three times). To conclude, the advantage of using a DS strategy implemented for the optimization and transfer of SFC method was successfully demonstrated in this work. [less ▲]

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See detailA new criterion to assess distributional homogeneity in hyperspectral images of solid pharmaceutical dosage forms
Sacre, Pierre-Yves ULg; Lebrun, Pierre ULg; Chavez, Pierre-François ULg et al

in Analytica Chimica Acta (2014), 818

During galenic formulation development, homogeneity of distribution is a critical parameter to check since it may influence activity and safety of the drug. Raman hyperspectral imaging is a technique of ... [more ▼]

During galenic formulation development, homogeneity of distribution is a critical parameter to check since it may influence activity and safety of the drug. Raman hyperspectral imaging is a technique of choice for assessing the distributional homogeneity of compounds of interest. Indeed, the combination of both spectroscopic and spatial information provides a detailed knowledge of chemical composition and component distribution. Actually, most authors assess homogeneity using parameters of the histogram of intensities (e.g. mean, skewness and kurtosis). However, this approach does not take into account spatial information and loses the main advantage of imaging. To overcome this limitation, we propose a new criterion: Distributional Homogeneity Index (DHI). DHI has been tested on simulated maps and formulation development samples. The distribution maps of the samples were obtained without validated calibration model since different formulations were under investigation. The results obtained showed a linear relationship between content uniformity values and DHI values of distribution maps. Therefore, DHI methodology appears to be a suitable tool for the analysis of homogeneity of distribution maps even without calibration during formulation development. [less ▲]

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See detailDetermination of 4-aminophenol in a pharmaceutical formulation using Surface Enhanced Raman scattering: from development to method validation
De Bleye, Charlotte ULg; Dumont, Elodie ULg; Rozet, Eric ULg et al

in Talanta (2013), 116

A Surface Enhanced Raman Scattering (SERS) method able to quantify 4-aminophenol in a pharmaceutical formulation based on acetaminophen, also called paracetamol, was developed and, for the first time ... [more ▼]

A Surface Enhanced Raman Scattering (SERS) method able to quantify 4-aminophenol in a pharmaceutical formulation based on acetaminophen, also called paracetamol, was developed and, for the first time, successfully validated. In this context, silver nanoparticles were synthesized according to the method described by Lee-Meisel and used as SERS substrate. The repeatability of the silver colloid synthesis was tested using different methods to characterise the size and the zeta potential of silver nanoparticles freshly synthesized. To optimize the SERS samples preparation, a design of experiments implicating concentrations of citrate-reduced silver nanoparticles and aggregating agent was performed in order to maximize the Raman signal enhancement. Finally, an approach based on tolerance intervals and accuracy profiles was applied in order to thoroughly validate the method in a range of concentrations comprised from 3 to 15 µg mL-1 using normalized band intensities. The standard addition method was selected as method calibration. Therefore, measurements were carried out on 4-aminophenol spiked solutions of the pharmaceutical formulation. Despite the well-known stability and reproducibility problems of SERS, the validation was performed using two operators and 5 batches of nanoparticles, one for each validation day. [less ▲]

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See detailValidation data treatment
Marini Djang'Eing'A, Roland ULg; Rozet, Eric ULg; Hubert, Philippe ULg

Learning material (2013)

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