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See detailA simple approach for ultrasensitive detection of bisphenols by multiplexed surface-enhanced Raman scattering
De Bleye, Charlotte ULg; Dumont, Elodie ULg; Hubert, Cédric ULg et al

in Analytica Chimica Acta (2015), 888

Bisphenol A (BPA) is well known for its use in plastic manufacture and thermal paper production despite its risk of health toxicity as an endocrine disruptor in humans. Since the publication of new ... [more ▼]

Bisphenol A (BPA) is well known for its use in plastic manufacture and thermal paper production despite its risk of health toxicity as an endocrine disruptor in humans. Since the publication of new legislation regarding the use of BPA, manufacturers have begun to replace BPA with other phenolic molecules such as bisphenol F (BPF) and bisphenol B (BPB), but there are no guarantees regarding the health safety of these compounds at this time. In this context, a very simple, cheap and fast surface-enhanced Raman scattering (SERS) method was developed for the sensitive detection of these molecules in spiked tap water solutions. Silver nanoparticles were used as SERS substrates. An original strategy was employed to circumvent the issue of the affinity of bisphenols for metallic surfaces and the silver nanoparticles surface was functionalized using pyridine in order to improve again the sensitivity of the detection. Semi-quantitative detections were performed in tap water solutions at a concentrations range from 0.25 to 20 µg L-1 for BPA and BPB and from 5 to 100 µg L-1 for BPF. Moreover, a feasibility study for performing a multiplex-SERS detection of these molecules was also performed before successfully implementing the developed SERS method on real samples. [less ▲]

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See detailDevelopment of a simple approach for ultrasensitive detection of bisphenols by multiplexed surface enhanced Raman scattering
De Bleye, Charlotte ULg; Dumont, Elodie ULg; Netchacovitch, Lauranne ULg et al

Poster (2015, July 13)

A very simple, cheap and fast SERS method using functionalized silver nanoparticles was developed to detect bisphenols. This method was applied for the semi-quantitative detection of bisphenol A (BPA ... [more ▼]

A very simple, cheap and fast SERS method using functionalized silver nanoparticles was developed to detect bisphenols. This method was applied for the semi-quantitative detection of bisphenol A (BPA), bisphenol B (BPB) and bisphenol F (BPF) separately. Afterwards, a feasibility study of performing a multiplex SERS detection of BPA, BPB and BPF was successfully carried out. Finally, this developed method was applied on real samples which were solutions comprising cash receipts collected from different stores. [less ▲]

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See detailThorough characterization of a Self-Emulsifying Drug Delivery System with Raman hyperspectral imaging: A case study.
Sacre, Pierre-Yves ULg; Netchacovitch, Lauranne ULg; De Bleye, Charlotte ULg et al

in International Journal of Pharmaceutics (2015), 484

Newly developed drugs often have poor bioavailability due to their poor water solubility (BCS class 2 drugs). It is therefore necessary to develop new strategies to enhance their solubility and their ... [more ▼]

Newly developed drugs often have poor bioavailability due to their poor water solubility (BCS class 2 drugs). It is therefore necessary to develop new strategies to enhance their solubility and their activity, among which, Self-Emulsifying Drug Delivery System (SEDDS). The efficacy of the drugs contained in these preparations is mainly affected by the solid state and the particle size of the active pharmaceutical ingredient (API). However, it is quite complex, long and expensive to characterize these parameters with classical techniques such as X-Ray powder diffraction, differential scanning calorimetry or hot stage microscopy. The present article presents, through a case study, the advantages of the Raman hyperspectral imaging in the characterization of such formulations. Indeed, Raman chemical imaging may fully characterize SEDDS with single equipment and operator in a non-destructive way allowing the follow-up of the formulation during stability studies. Raman imaging is therefore a tool of choice in the PAT framework since it increases the knowledge of the formulation and the process. A quantitative multivariate method using Raman hyperspectral imaging to assay the API in the lipid based formulation has been developed and fully validated following the “total error” approach. [less ▲]

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See detailIntérêt de la spectroscopie vibrationnelle dans le cadre du PAT
Ziemons, Eric ULg; Chavez, Pierre-François ULg; Netchacovitch, Lauranne ULg et al

Scientific conference (2014, November 13)

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See detailRaman hyperspectral imaging: a single tool to characterise pharmaceutical products
Netchacovitch, Lauranne ULg; De Bleye, Charlotte ULg; Chavez, Pierre-François ULg et al

in European Pharmaceutical Review (2014), 19(5), 8-11

Raman hyperspectral imaging is an increasingly used tool in the pharmaceutical field because it allows for the investigation of many characteristics on a solid sample. This paper delves into Raman ... [more ▼]

Raman hyperspectral imaging is an increasingly used tool in the pharmaceutical field because it allows for the investigation of many characteristics on a solid sample. This paper delves into Raman spectroscopy and imaging, including spectral and spatial information, and presents some applications of Raman hyperspectral imaging in the pharmaceutical field. [less ▲]

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See detailData processing of vibrational chemical imaging for pharmaceutical applications.
Sacre, Pierre-Yves ULg; De Bleye, Charlotte ULg; Chavez, Pierre-François ULg et al

in Journal of Pharmaceutical & Biomedical Analysis (2014), 101

Vibrational spectroscopy (MIR, NIR and Raman) based hyperspectral imaging is one of the most powerful tools analyze pharmaceutical preparation. Indeed, it combines the advantages of vibrational ... [more ▼]

Vibrational spectroscopy (MIR, NIR and Raman) based hyperspectral imaging is one of the most powerful tools analyze pharmaceutical preparation. Indeed, it combines the advantages of vibrational spectroscopy to imaging techniques and allows therefore the visualization of distribution of compounds, crystallization processes. However, these techniques provide a huge amount of data that must be processed to extract the relevant information. This review presents fundamental concepts of hyperspectral imaging, the basic theory of the most used chemometric tools used to pre-process, process and post-process the generated data. The last part of the present paper focuses on pharmaceutical applications of hyperspectral imaging and highlights the data processing approaches to enable the reader making the best choice among the different tools available. [less ▲]

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See detailDevelopment of a multiplexed surface-enhanced Raman scattering quantitative approach for bisphenols detection
De Bleye, Charlotte ULg; Dumont, Elodie ULg; Sacre, Pierre-Yves ULg et al

Conference (2014, June 23)

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 detailApplication of hyperspectral Raman imaging to the analysis of a self-emulsifying drug delivery system (SEDDS).
Sacre, Pierre-Yves ULg; De Bleye, Charlotte ULg; Netchacovitch, Lauranne ULg et al

Poster (2014, June)

Self-emulsifying drug delivery systems (SEDDS) are mixtures of drug and excipients that undergo emulsification when exposed to water. This pharmaceutical form is used to enhance the oral absorption of ... [more ▼]

Self-emulsifying drug delivery systems (SEDDS) are mixtures of drug and excipients that undergo emulsification when exposed to water. This pharmaceutical form is used to enhance the oral absorption of poorly water-soluble drugs. The API is finely dispersed in the excipients and forms a solid solution increasing its dissolution rate. Hyperspectral Raman imaging is a powerful tool that combines both spectral and spatial information. It returns qualitative and quantitative information useful during the development or the characterization of pharmaceutical preparations. The studied formulation consisted of a BCS 2 API (high permeability, low solubility) dispersed in excipients mainly composed of Lauroyl macrogol-32 glycerides (>50%). Two different preparations were analyzed: 100% of API dissolved and 70% of API dissolved with 30% of API powder added to the formulation. The two formulations have therefore exactly the same qualitative and quantitative composition but different spatial distribution and dispersion of the API mimicking a problem during the process. First a confocal Raman microscopic analysis was performed to evaluate the solid state of the API in the formulations. Then, an evaluation of the particle size was performed. These results are important since they can affect the bioavailability of the API and therefore its activity. Beside the microscopic scale analysis, a macroscopic imaging quantitative PLS model has been developed. The method has been validated within +/- 10% acceptance limits following the total error approach. This validated quantitative model enables reliable quantitative analysis at the pixel level of Raman images providing meaningful chemical images. [less ▲]

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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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