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See detailRaman Hyperspectral Imaging: An essential tool in the pharmaceutical field
Sacre, Pierre-Yves ULg; Netchacovitch, Lauranne ULg; Dumont, Elodie ULg et al

E-print/Working paper (2017)

Resulting from the combination of Raman spectroscopy and optical microscopy, Raman hyperspectral imaging has proven to be an indispensable tool in the pharmaceutical field. This article will broach a ... [more ▼]

Resulting from the combination of Raman spectroscopy and optical microscopy, Raman hyperspectral imaging has proven to be an indispensable tool in the pharmaceutical field. This article will broach a number of Raman hyperspectral imaging applications that were developed in our laboratory, in order to demonstrate the significance of the technique. [less ▲]

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See detailRaman Hyperspectral Imaging: An essential tool in the pharmaceutical field
Sacre, Pierre-Yves ULg; De Bleye, Charlotte ULg; Netchacovitch, Lauranne ULg et al

E-print/Working paper (2017)

Raman hyperspectral imaging results from the powerful combination of spatial (imaging) and spectral (Raman) information. It is increasingly used both in R&D and in the industry because it allows the ... [more ▼]

Raman hyperspectral imaging results from the powerful combination of spatial (imaging) and spectral (Raman) information. It is increasingly used both in R&D and in the industry because it allows the investigation of many characteristics of solid samples. This technique provides an accurate tool for qualitative and quantitative analysis of a pharmaceutical solid formulation. In this webinar, Assoc. Prof. Ziemons will present fundamental concepts of hyperspectral imaging data analysis and key applications in pharmaceutical and biomedical field. [less ▲]

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See detailGlobal approach for the validation of an in-line Raman spectroscopic method to determine the API content in real-time during a hot-melt extrusion process
Netchacovitch, Lauranne ULg; Thiry, Justine ULg; De Bleye, Charlotte ULg et al

in Talanta (2017)

Since the Food and Drug Administration (FDA) published a guidance based on the Process Analytical Technology (PAT) approach, real-time analyses during manufacturing processes are in real expansion. In ... [more ▼]

Since the Food and Drug Administration (FDA) published a guidance based on the Process Analytical Technology (PAT) approach, real-time analyses during manufacturing processes are in real expansion. In this study, in-line Raman spectroscopic analyses were performed during a Hot-Melt Extrusion (HME) process to determine the Active Pharmaceutical Ingredient (API) content in real-time. The method was validated based on a univariate and a multivariate approach and the analytical performances of the obtained models were compared. Moreover, on one hand, in-line data were correlated with the real API concentration present in the sample quantified by a previously validated off-line confocal Raman microspectroscopic method. On the other hand, in-line data were also treated in function of the concentration based on the weighing of the components in the prepared mixture. The importance of developing quantitative methods based on the use of a reference method was thus highlighted. The method was validated according to the total error approach fixing the acceptance limits at ± 15% and the α risk at ± 5%. This method reaches the requirements of the European Pharmacopeia norms for the uniformity of content of single-dose preparations. The validation proves that future results will be in the acceptance limits with a previously defined probability. Finally, the in-line validated method was compared with the off-line one to demonstrate its ability to be used in routine analyses. [less ▲]

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See detailMonitoring of anatabine release by methyl jasmonate elicited BY-2 cells using surface-enhanced Raman scattering
De Bleye, Charlotte ULg; Dumont, Elodie ULg; Dispas, Amandine ULg et al

in Talanta (2016), 160

A new application of surface-enhanced Raman scattering (SERS) in the field of plant material analysis is proposed in this study. The aim was to monitor the release of anatabine by methyl jasmonate (MeJa ... [more ▼]

A new application of surface-enhanced Raman scattering (SERS) in the field of plant material analysis is proposed in this study. The aim was to monitor the release of anatabine by methyl jasmonate (MeJa) elicited Bright Yellow-2 (BY-2) cells. Gold nanoparticles (AuNps) were used as SERS substrate. The first step was to study the SERS activity of anatabine in a complex matrix comprising the culture medium and BY-2 cells. The second step was the calibration. This one was successfully performed directly in the culture medium in order to take into account the matrix effect, by spiking the medium with different concentrations of anatabine, leading to solutions ranging from 250 to 5000 µg L-1. A univariate analysis was performed, the intensity of a band situated at 1028 cm-1, related to anatabine, was plotted against the anatabine concentration. A linear relationship was observed with a R2 of 0.9951. During the monitoring study, after the MeJa elicitation, samples were collected from the culture medium containing BY-2 cells at 0, 24h, 48h, 72h and 96h and were analyzed using SERS. Finally, the amount of anatabine released in the culture medium was determined using the response function, reaching a plateau after 72h of 82 µg of anatabine released / g of fresh weight (FW) MeJa elicited BY-2 cells. [less ▲]

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See detailA simple calibration approach based on film-casting for confocal Raman microscopy to support the development of a Hot-Melt Extrusion process
Netchacovitch, Lauranne ULg; Thiry, Justine ULg; De Bleye, Charlotte ULg et al

in Talanta (2016), 154

When developing a new formulation, the development, calibration and validation steps of analytical methods based on vibrational spectroscopy are time-consuming. For each new formulation, real samples must ... [more ▼]

When developing a new formulation, the development, calibration and validation steps of analytical methods based on vibrational spectroscopy are time-consuming. For each new formulation, real samples must be produced and a “reference method” must be used in order to determine the Active Pharmaceutical Ingredient (API) content of each sample. To circumvent this issue, the paper presents a simple approach based on the film-casting technique used as a calibration tool in the framework of hot-melt extrusion process. Confocal Raman microscopic method was successfully validated for the determination of itraconazole content in film-casting samples. Then, hot-melt extrusion was carried out to produce real samples in order to confront the results obtained with confocal Raman microscopy and Ultra High Performance Liquid Chromatography (UHPLC). The agreement between both methods was demonstrated using a comparison study based on the Bland and Altman’s plot. [less ▲]

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See detailFrom Near-Infrared and Raman to Surface-Enhanced Raman Spectroscopy: Progress, Limitations, Perspectives in Bioanalysis
Dumont, Elodie ULg; De Bleye, Charlotte ULg; Sacre, Pierre-Yves ULg et al

in Bioanalysis (2016), 8(10), 1077-1103

Over recent decades, spreading environmental concern entailed the expansion of green chemistry analytical tools. Vibrational spectroscopy, belonging to this class of analytical tool, is particularly ... [more ▼]

Over recent decades, spreading environmental concern entailed the expansion of green chemistry analytical tools. Vibrational spectroscopy, belonging to this class of analytical tool, is particularly interesting taking into account its numerous advantages such as fast data acquisition and no sample preparation. In this context, Near-Infrared, Raman and mainly Surface-Enhanced Raman Spectroscopy (SERS) have thus gained interest in many fields including bioanalysis. The two former techniques only ensure the analysis of concentrated compounds in simple matrices, whereas the emergence of SERS improved the performances of vibrational spectroscopy to very sensitive and selective analyses. Complex SERS substrates were also developed enabling biomarker measurements, paving the way for SERS immunoassays. Therefore, in this paper, the strengths and weaknesses of these techniques will be highlighted with a focus on recent progress. [less ▲]

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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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