References of "Sacre, Pierre-Yves"
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See detailDevelopment of a SERS strategy to overcome the nanoparticle stabilisation effect in serum-containing samples: Application to the quantification of dopamine in the culture medium of PC-12 cells
Dumont, Elodie ULiege; De Bleye, Charlotte ULiege; Cailletaud, Johan ULiege et al

in Talanta (in press)

The analysis of serum samples by surface-enhanced Raman spectroscopy (SERS) has gained ground over the last years. However, the stabilisation of colloids by the proteins contained in these samples has ... [more ▼]

The analysis of serum samples by surface-enhanced Raman spectroscopy (SERS) has gained ground over the last years. However, the stabilisation of colloids by the proteins contained in these samples has restricted their use in common practice, unless antibodies or aptamers are used. Therefore, this work was dedicated to the development of a SERS methodology allowing the analysis of serum samples in a simple and easy-to-implement way. This approach was based on the pre-aggregation of the colloid with a salt solution. Gold nanoparticles (AuNPs) were used as the SERS substrate and, owing to its physiopathological importance, dopamine was chosen as a model to implement the SERS approach. The presence of this neurotransmitter could be determined in the concentration range 0.5 to 50 ppm (2.64 – 264 µM) in the culture medium of PC-12 cells, with a R² of 0.9874, and even at lower concentrations (0.25 ppm, 1.32 µM) in another matrix containing fewer proteins. Moreover, the effect of calcium and potassium on the dopamine exocytosis from PC-12 cells was studied. Calcium was shown to have a predominant and dose-dependent effect. Finally, PC-12 cells were exposed to dexamethasone in order to increase their biosynthesis and release of dopamine. This increase was monitored with the developed SERS approach. [less ▲]

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See detailCLASSIFICATION OF FLUCONAZOLE API POLYMORPHIC FORMS IN PHARMACEUTICAL PRODUCTS BY ASSOCIATING FTIR, NIR AND RAMAN TO PLS-DA
Alaoui Mansouri, Mohammed ULiege; Sacre, Pierre-Yves ULiege; Ziemons, Eric ULiege et al

Poster (2018, June 26)

The main goal of this work was to prove the ability of the combination between vibrational spectroscopy techniques and PLS-DA to differentiate between different polymorphic forms of fluconazole in ... [more ▼]

The main goal of this work was to prove the ability of the combination between vibrational spectroscopy techniques and PLS-DA to differentiate between different polymorphic forms of fluconazole in pharmaceutical products. These are mostly manufactured based on fluconazole polymorphic form- II and form- III. These crystalline forms may undergo polymorphic transition during the manufacturing or storage conditions process. Therefore, it is important to confirm if the expected polymorphic form is still present or not. FT-IR, FT-NIR and Raman spectroscopies were associated to PLS-DA and used to build robust classification models to distinguish between form- II, Form- III and monohydrate form. Based on the results, it is shown that PLS-DA models have a high efficiency to classify various fluconazole polymorphs, with a high sensitivity and specificity. Finally, the selectivity of the PLS-DA models is proven based on the analysis of two samples of itraconazole and miconazole that belong to the same antifungal class as fluconazole. These two samples mimic potential contaminants. Based on the plots of Hotelling T² vs Q residuals, miconazole and itraconazole are significantly considered outliers and rejected. [less ▲]

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See detailLes risques sociétaux liés aux médicaments de qualité inférieure
Marini Djang'Eing'A, Roland ULiege; Mavungu Landu, Don Jethro ULiege; Sakira, Abdoul Karim ULiege et al

in Book of Abstracts - 3ème JMPO - Université de Ouaga 1 Pr Ki Zerbo (2018, January 30)

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See detailDe l'intérêt de la spectroscopie Raman pour l'analyse pharmaceutique
Avohou, Tonakpon Hermane ULiege; Cailletaud, Johan ULiege; Clavaud, Matthieu et al

Scientific conference (2018, January 15)

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See detailCritical review of surface-enhanced Raman spectroscopy applications in the pharmaceutical field
Cailletaud, Johan ULiege; De Bleye, Charlotte ULiege; Dumont, Elodie ULiege et al

in Journal of Pharmaceutical & Biomedical Analysis (2018), 147

Surface-enhanced Raman spectroscopy (SERS) is a sensitive analytical tool used in the pharmaceutical field in recent years. SERS keeps all the advantages of classical Raman spectroscopy while being is ... [more ▼]

Surface-enhanced Raman spectroscopy (SERS) is a sensitive analytical tool used in the pharmaceutical field in recent years. SERS keeps all the advantages of classical Raman spectroscopy while being is more sensitive allowing its use for the detection and the quantification of low-dose substances contained in pharmaceutical samples. However, the analytical performance of SERS is limited due to the difficulty to implement a quantitative methodology correctly validated. Nevertheless, some studies reported the development of SERS quantitative methods especially in pharmaceutical approaches. In this context, this review presents the main concepts of the SERS technique. The different steps that need to be applied to develop a SERS quantitative method are also deeply described. The last part of the present manuscript gives a critical overview of the different SERS pharmaceutical applications that were developed for a non-exhaustive list of pharmaceutical compounds with the aim to highlights the validation criteria for each application. [less ▲]

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See detailPhenotyping transgenic poplar downregulating PtaUGT72E1 to assess the role of this gene in lignin accumulation
Speeckaert, Nathanaël; Baldacci-Cresp, Fabien; Twyffels, Laure et al

Poster (2018)

In plants, UDP - glycosyltransferases (UGT) are a superfamily of enzymes catalysing the transfer of glycosyl groups to a wide range of molecules like hormones, xenobiotics and secondary metabolites ... [more ▼]

In plants, UDP - glycosyltransferases (UGT) are a superfamily of enzymes catalysing the transfer of glycosyl groups to a wide range of molecules like hormones, xenobiotics and secondary metabolites, ... These enzymes are crucial in many environmental adaptation mechanisms. In Arabidopsis thaliana, the UGT72E family was shown to function with monolignols, deriving from the phenylpropanoid pathway. Monolignols are the precursors of many essential compounds for plant growth and development, like intracellular di-, tri- or oligolignols which are considered to have plant defense properties. In the cell wall, they can polymerised to form lignin. It is a complex polymer, which has a role in plant support and allows, thanks to its hydrophobic character, the conduction of water and solutes in the xylem. Currently, our knowledge on the regulation mechanisms of monolignol polymerization into lignin and lignans remains limited. The glycosylation of monolignols and their storage in the vacuole are considered as central mechanisms for monolignol homeostasis. The purpose of this work is to gain a better knowledge on the role of UGT72E in woody plants, producing a large amount of lignin, by characterizing PtaUGT72E1 in Populus tremula x P. alba (clone INRA 717-1B4). One of the strategies chosen is the phenotyping of transgenic poplar over-expressing and down-regulating PtaUGT72E1. A particular focus was made on stem lignification. Two methods were chosen to analyse this aspect: fluorescent analysis of safrani ne staining and Raman spectroscopy. Both methods confirm the alteration of lignin deposition in the xylem cellular wall in transgenic lines: a decrease of lignification was recorded in the over-expressing lines and an increase of lignification in the down-regulating lines. These results highlight a possible role for PtaUGT72E1 in the regulation of the lignification of vascular tissues in poplar. [less ▲]

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See detailRaman Chemical Imaging in Kidney Stone Analysis
Castiglione, Vincent ULiege; Sacre, Pierre-Yves ULiege; CAVALIER, Etienne ULiege et al

Poster (2017, November 02)

Background: The structure of kidney stones might provide clinical useful information in addition to the stone composition. The Raman chemical imaging (RCI) is a new technology used for the production of ... [more ▼]

Background: The structure of kidney stones might provide clinical useful information in addition to the stone composition. The Raman chemical imaging (RCI) is a new technology used for the production of two-dimensions maps of the constituents' distribution in samples. We aimed at determining the use of RCI in urinary stone analysis. Methods: Twelve calculi were analyzed by RCI using a confocal Raman microspectrophotometer. They were selected according to their heterogeneous composition and morphology. Prior to the analysis, samples were sliced and milled in order to detect the nucleus of the stones and having a smooth surface. RCI 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, the gold standard method for the determination of urolithiasis composition. Results: RCI succeeded in identifying all the chemical components contained in each sample, including monohydrate and dihydrate calcium oxalate, anhydrous and dihydrate uric acid, apatite, struvite, brushite, whitlockite and ammonium urate. However, proteins couldn't be detected because of the huge autofluorescence background and the small concentration of these poor Raman scatterers. Carbapatite and calcium oxalate were correctly detected even when they represented less than 5 percent of the whole stones, allowing the detection of very small structures like Randall's plaques. Moreover, RCI provided the distribution of components within the stones. The nuclei were accurately identified, as well as thin layers of other components. Conversion of dihydrate to monohydrate calcium oxalate was correctly observed in the center of one sample. Conclusion: RCI showed a good accuracy in comparison with infrared spectroscopy in identifying components of kidney stones. In addition, RCI is nondestructive enabling the storage of samples. This analysis was also useful in determining the organization of components within stones, which help locating constituents in low quantity, such as nuclei. However, this analysis is time-consuming, which makes it more suitable for research studies rather than routine analysis. [less ▲]

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See detailLes risques toxicologiques liés aux médicaments de qualité inférieure
Marini Djang'Eing'A, Roland ULiege; Kalenda Tshilombo, Nicodème ULiege; Ciza Hamuli, Patient ULiege et al

Conference (2017, October 19)

Objective: Poor quality medicines regrouping counterfeit/falsified, sub-standards and degraded are a scourge for developing countries (1). Their public health consequences are often observed for cases of ... [more ▼]

Objective: Poor quality medicines regrouping counterfeit/falsified, sub-standards and degraded are a scourge for developing countries (1). Their public health consequences are often observed for cases of low dosage of active ingredients and sometimes for the absence of these. On the basis of the observed facts as well as suspected reported cases, we were interested in deepening the information through laboratory tests. Methods: Liquid chromatography (LC), thin layer chromatography (TLC), nuclear magnetic resonance (NMR), mass spectrometry (MS), Raman imagery (Rim) and near infrared spectroscopy (NIR) were used as targeted analytical techniques in this study, associated with the principal component analysis (PCA), while the suspect samples were obtained via the public health authorities of the DR Congo, Benin and Rwanda after their seizure. Results: The observed cases are presented by therapeutic class, namely: - analgesics: (1) cases of tablets supposed to contain paracetamol and which have caused abnormal adverse effects in patients who have consumed it, namely sedative effects, polyuria and hypotension. Using LC and complementary surveys by people interview, we were able to demonstrate the presence of a benzodiazepine and at very high doses. (2) Cases of paracetamol syrup whose excipient (glycerol) was substituted by diethylene glycol and which had caused the death of a hundred babies. Using the NIR and the PCA, we were able to elucidate this substitution. - antimalarials: (case 1) cases of arthemether-lumefantrine tablets which had no therapeutic effect. By means of TLC and LC, the absence of these two active ingredients was clearly demonstrated, but the presence of starch was revealed by Rim. (Case 2) case of quinine tablets that had no expected pharmacological effect. The use of several combined techniques (TLC, LC-MS, NMR and Rim) made it possible to demonstrate the presence of a substance with an imidazole structure (antamoeba). - antibiotics: (1) amoxicillin powder which after reconstitution in hospital caused poisoning of the babies until death for some. The reconstitution of the suspension had revealed the misuse of hydrogen peroxide instead of distilled water. (2) Finally a large-scale study (80 samples of amoxicillin powder) showed that 8% of the samples were above the claimed dosage. Conclusion: The cases presented indicate that there are effectively poor quality medicines and that they are responsible of public health problems and in particular of toxicity. Appropriate measures should be taken to protect users. [less ▲]

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See detailPoor quality medicines in Africa: how to combat this real scourge
Marini Djang'Eing'A, Roland ULiege; Sacre, Pierre-Yves ULiege; Ziemons, Eric ULiege et al

Conference (2017, October 04)

Poor (or low) quality medicines remain a crucial problem of public health around the world. They encompass falsified /counterfeit, substandard or degraded drugs. If proportion of 1% is estimated in ... [more ▼]

Poor (or low) quality medicines remain a crucial problem of public health around the world. They encompass falsified /counterfeit, substandard or degraded drugs. If proportion of 1% is estimated in developed countries, they are globally about 10 % of counterfeit drugs according to Food and Drug Administration, with 30% in low income countries and astonishing values (80 %) reported in some African countries. The consequences and dangers of such medicines are therapeutic failure, drug poisoning, microbial resistance or even death. For the pharmaceutical industries, there are loss of image, loss of financial income and employment. There is need to combat this scourge, but most of the time, means are very limited and even lacking. In this context, several means or tools are developed by the ULg Pharmacy Department including the simple ones including organoleptic tests, simple analytical tests such as analytical balance, pHmeter, thin layer chromatography (TLC), UV-visible spectrophotometry to the more complex including liquid chromatography (LC) coupled to UV-Vis detector, or to mass spectrometry, nuclear magnetic resonance, Raman imagery (RIM) and near infrared (NIR) spectroscopy associated with the principal component analysis (PCA). In this way, we have analyzed several suspected samples obtained via the public health authorities of the D.R. Congo, Benin and Rwanda after their seizure or through collaborations. The results are presented by therapeutic class, namely: analgesics: - by using LC and complementary information from victim patients, we were able to discover an abnormal presence of a benzodiazepine at very high doses in paracetamol tablets which was the cause of unusual adverse effects (sedative effects, polyuria and hypotension) in patients who have consumed it; - by using the NIR-PCA, we were able to elucidate the substitution of an excipient (glycerol) by diethylene glycol in paracetamol syrup which caused the death of a hundred babies. antimalarials: - we faced cases of arthemether-lumefantrine tablets which had no therapeutic effect. By means of TLC and LC, the absence of these two active ingredients was clearly demonstrated, but the presence of starch was revealed by RIM; - another case of quinine tablets that had no expected pharmacological effect was faced. The use of several combined techniques (TLC, LC-MS, NMR and RIM) allowed to detect the presence of a substance with an imidazole structure (antamoeba). antibiotics: - the case of amoxicillin powder which after reconstitution in hospital caused poisoning of the babies until death for some was investigated. The reconstitution of the suspension in the laboratory had revealed the misuse of hydrogen peroxide instead of distilled water; - we participated to a large-scale study (80 samples of amoxicillin powder) that showed 8% of overdose. The cases presented indicate that there are effectively poor quality medicines and there is need to sustain strong collaborations while reinforcing appropriate measures to protect users. [less ▲]

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

Conference (2017, September 22)

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

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

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

Poster (2017, September 21)

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

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

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

Conference (2017, September 13)

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

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

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See detailGlobal regression model for moisture content determination using near-infrared spectroscopy
Clavaud, Matthieu ULiege; Roggo, Yves; Degardin, Klara et al

in European Journal of Pharmaceutics and Biopharmaceutics (2017), 119

Near-infrared (NIR) global quantitative models were evaluated for the moisture content (MC) determination of three different freeze-dried drug products. The quantitative models were based on 3822 spectra ... [more ▼]

Near-infrared (NIR) global quantitative models were evaluated for the moisture content (MC) determination of three different freeze-dried drug products. The quantitative models were based on 3822 spectra measured on two identical spectrometers to include variability. The MC, measured with the reference Karl Fischer (KF) method, were ranged from 0.05% to 4.96%. Linear and non-linear regression models using Partial Least Square (PLS), Decision Tree (DT), Bayesian Ridge Regression (Bayes-RR), K-Nearest Neighbors (KNN), and Support Vector Regression (SVR) algorithms were created and evaluated. Among them, the SVR model was retained for a global application. The Standard Error of Calibration (SEC) and the Standard Error of Prediction (SEP) were respectively 0.12% and 0.15%. This model was then evaluated in terms of total error and risk-based assessment, linearity, and accuracy. It was observed that MC can be fastly and simultaneously determined in freeze-dried pharmaceutical products thanks to a global NIR model created with different medicines. This innovative approach allows to speed up the validation time and the in-lab release analyses. [less ▲]

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See detailRaman Hyperspectral Imaging: An essential tool in the pharmaceutical field
Sacre, Pierre-Yves ULiege; Netchacovitch, Lauranne ULiege; Dumont, Elodie ULiege 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 detailDetection of Poor Quality Artemisinin-based Combination Therapy (ACT) Medicines Marketed in Benin Using Simple and Advanced Analytical Techniques
Yemoa, Achille; Habyalimana, Védaste ULiege; Mbinze Kindenge, Jérémie ULiege et al

in Current Drug Safety (2017), 12

Background: Poor quality antimalarial medicines still represent a threat to the public health, especially in Sub-Saharan Africa which bears a disproportionate share of the global burden of malaria. It is ... [more ▼]

Background: Poor quality antimalarial medicines still represent a threat to the public health, especially in Sub-Saharan Africa which bears a disproportionate share of the global burden of malaria. It is essential and urgent to strengthen mechanisms against counterfeit medicines. One of the approaches is regular market surveillance through quality controls. Methods: 12 samples of artemether/lumefantrine were collected from formal and informal drug sellers in Cotonou (Benin) as well as additional other similar samples from Rwanda (13 samples) and from D.R. Congo (9 samples). Thin Layer Chromatography (TLC) as classical and simple identification test was applied in Benin while an analytical chemistry laboratory in Belgium (ULg, Pharmacy Department) was asked for further analyses with HPLC and Raman spectroscopy using a developed and validated HPLC method for rapid analysis of artemether/lumefantrine. Results: The results obtained in Belgium confirmed the lack of the two active ingredients in the suspected sample of ACT medicine from Benin whereas some samples from Rwanda and D.R. Congo were found to present risk of substandard drugs either for under-dosing or over-dosing. Conclusions: Counterfeit/falsified of artemisinin-based combination therapy (ACT) medicines are really scourge that needs to be fought through strong collaboration between public health authorities and appropriate quality control laboratories. [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 ULiege; Thiry, Justine ULiege; De Bleye, Charlotte ULiege et al

in Talanta (2017), 171

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

Conference given outside the academic context (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 detailLe fléau des faux médicaments
Marini Djang'Eing'A, Roland ULiege; Ziemons, Eric ULiege; Sacre, Pierre-Yves ULiege et al

Conference given outside the academic context (2017)

Detailed reference viewed: 39 (14 ULiège)