References of "Cailletaud, Johan"
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See detailTowards a spray-coating method for the detection of low-dose compounds in pharmaceutical tablets using surface-enhanced Raman chemical imaging (SER-CI)
Cailletaud, Johan ULiege; De Bleye, Charlotte ULiege; Dumont, Elodie ULiege et al

in Talanta (2018), 188

Surface-enhanced Raman chemical imaging (SER-CI) is a highly sensitive analytical tool recently used in the pharmaceutical field owing to the possibility to obtain high sensitivity along with spatial ... [more ▼]

Surface-enhanced Raman chemical imaging (SER-CI) is a highly sensitive analytical tool recently used in the pharmaceutical field owing to the possibility to obtain high sensitivity along with spatial information. However, the covering method of the pharmaceutical samples such as tablets with metallic nanoparticles is a major issue for SER-CI analyses due to the difficulty to obtain a homogeneous covering of tablet surface with the SERS substrates. In this context, a spray-coating method was proposed in order to fully exploit the potential of SER-CI. A homemade apparatus has been developed from an electrospray ionization (ESI) probe in order to cover the pharmaceutical tablets with the colloidal suspension in a homogeneous way. The silver substrate was pulled through the airbrush by a syringe pump which was then nebulized into small droplets due to the contact of the solution with the gas flow turbulence. A robust optimization of the process was carried out by adjusting experimental parameters such as the liquid flow rate and the spraying time. Besides, the performances of this spraying technique were compared with two others covering methods found in the literature which are drop casting and absorption coating. A homogeneity study, conducted by SER-CI and matrix assisted laser desorption/ ionization mass spectrometry imaging (MALDI-MSI) applied to the different covering techniques was performed. The influence of the metallic nanoparticles deposit on soluble compounds was also investigated in order to highlight the advantages of using this new spray coating approach. [less ▲]

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See detailA simple and easy-to-implement SERS approach overcoming the nanoparticle stabilisation by serum proteins: application to dopamine and PC-12 cells
Dumont, Elodie ULiege; De Bleye, Charlotte ULiege; Cailletaud, Johan ULiege et al

Conference (2018, September 11)

This lecture presents the different steps regarding the development of a label-free SERS analytical method that was able to overcome the nanoparticle stabilisation caused by serum proteins. It relied on ... [more ▼]

This lecture presents the different steps regarding the development of a label-free SERS analytical method that was able to overcome the nanoparticle stabilisation caused by serum proteins. It relied on the pre-aggregation of the SERS substrate, which was a suspension of gold nanoparticles. Furthermore, several applications of the developed methodology were presented: the quantification of dopamine in the culture medium of rat phaeochromocytoma PC-12 cells as well as the influence of calcium, potassium and dexamethasone on dopamine exocytosis from these cells. [less ▲]

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See detailDetection of low-dose of piroxicam polymorphs in pharmaceutical tablets by surface-enhanced Raman chemical imaging and multivariate analysis
Cailletaud, Johan ULiege; De Bleye, Charlotte ULiege; Dumont, Elodie ULiege et al

Poster (2018, September)

In the pharmaceutical industry, the detection and the identification of polymorphic forms of an active pharmaceutical ingredient (API) is an important concern during the drug development and the ... [more ▼]

In the pharmaceutical industry, the detection and the identification of polymorphic forms of an active pharmaceutical ingredient (API) is an important concern during the drug development and the manufacturing process. The necessity to detect polymorphic forms especially at low concentrations is an area of particular interest in pharmaceutical applications due the difference of physico-chemical properties exhibited by the polymorphs. The polymorphic behavior of drugs can affect the therapeutic efficacy of the drug substance and can also have an impact from an intellectual property (IP) standpoint. Indeed, much effort are expended by the regulatory authorities to determine if the polymorph present in the final product is covered by a patent for IP rights aspects. Various analytical techniques can be used for polymorph detection and characterization such as X-ray powder diffraction (XRPD), solid-state nuclear magnetic resonance spectroscopy (ssNMR) and vibrational spectroscopy. Despite low sensitivity and long image acquisition times, Raman microscopy is well suited to the analysis of polymorphic forms since it enables the acquisition of spectral and spatial information at the same time. This technique can be combined with surface-enhanced Raman scattering (SERS), resulting in surface-enhanced Raman chemical imaging (SER-CI). SER-CI is a promising tool for the detection and the visualization of low-dose compounds or impurities in tablets taking account of the high sensitivity of this technique. Consequently, we firstly focused on the development of a reproducible spray-coating method to control the deposition of SERS nanoparticles on pharmaceutical samples in order to fully exploit the potential of SER-CI. Besides, this spraying technique, coupled with SER-CI, was applied to model tablets consisting of one excipient and a 10% (w/w) API concentration. Piroxicam, a non-steroidal anti-inflammatory drug which presents three polymorphic forms was used as a model API. The model formulation was a binary mixture of the form β and the form α2 polymorphs of piroxicam. Using SER-CI and multivariate analysis, it was possible to detect the β form polymorph in these model tablets below 1% (w/w) while reducing the image acquisition time. To conclude, the combination of the spray-coating method and SER-CI enabled the detection of low-dose of piroxicam polymorphs in model pharmaceutical formulations. This approach can serve as a potential way for the development of methods validation for semi-quantitative and quantitative analyses [less ▲]

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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 (2018), 186

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 detailInvestigation of solid surface-enhanced Raman scattering (SERS) substrates for the quantification of dopamine in cell culture media
Dumont, Elodie ULiege; De Bleye, Charlotte ULiege; Cailletaud, Johan ULiege et al

Poster (2018, May 17)

Since its discovery, surface-enhanced Raman spectroscopy (SERS) has constantly gained ground among the analytical techniques. One field of SERS that is rapidly expanding concerns the development of solid ... [more ▼]

Since its discovery, surface-enhanced Raman spectroscopy (SERS) has constantly gained ground among the analytical techniques. One field of SERS that is rapidly expanding concerns the development of solid SERS substrates. These are made up of metallic nanomaterials set in a fixed configuration: either by complex and expensive techniques (lithography, printing) or by the immobilisation of suspensions of nanoparticles (NPs) previously synthesised. In bioanalysis, solid SERS substrates allow the performance of real-time monitoring of biological or cellular processes such as the release of neurotransmitters by stimulated cells or intercellular communications between cancer cells and the immune system. Dopamine (DA) is an important neurotransmitter of the central and peripheral nervous systems, as evidenced by the diseases arising when DA levels are dysregulated. Consequently, analytical techniques being able to determine DA in sensitive and specific ways are requested. In this context, this work was dedicated to the development of solid SERS substrates enabling the quantification of DA in the culture medium of rat phaeochromocytoma PC-12 cells. These cells are a cellular model for the neurosecretion of DA. The solid SERS substrates developed could furthermore be employed to investigate the cellular release of DA under various stimulation conditions directly in the culture medium. [less ▲]

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See detailApplication of surface-enhanced Raman spectroscopy (SERS) in the biological and the pharmaceutical fields: state of the art and new perspectives
De Bleye, Charlotte ULiege; Cailletaud, Johan ULiege; Deidda, Riccardo ULiege et al

Scientific conference (2018, May 16)

The next CIRM presentation, entitled « Application of surface-enhanced Raman spectroscopy (SERS) in the biological and pharmaceutical fields : State of the art and new perspectives”, will be presented by ... [more ▼]

The next CIRM presentation, entitled « Application of surface-enhanced Raman spectroscopy (SERS) in the biological and pharmaceutical fields : State of the art and new perspectives”, will be presented by Elodie Dumont, Johan Cailletaud, Riccardo Deidda and Charlotte De Bleye from the Laboratory of Pharmaceutical Analytical Chemistry. The aim of this presentation is to give a general overview of this technique including the advantages, the synthesis of SERS substrates, the parameters influencing the signal exaltation and its laboratory developed applications. In this context, after browsing the SERS theoretical aspect, Johan Cailletaud will present his work focusing on the development of a covering method of pharmaceutical samples with metallic nanoparticles, which is a major issue for SERS chemical imaging analyses. He will also discuss about the feasibility of detecting low dose polymorph in dosage form using SERS chemical imaging. Regarding the application of SERS in the biological field, Elodie Dumont will present a SERS methodology that she developed in order to analyze the amount of dopamine, an important neurotransmitter, released by rat phaeochromocytoma PC-12 cells in their culture medium. This SERS approach was based on the salt-induced pre-aggregation of the colloidal SERS substrate before the addition of the sample. A calibration curve was established before the investigation of the calcium, potassium and dexamethasone effects on the exocytosis of dopamine from PC-12 cells. Finally, Riccardo Deidda will present the main objectives of his thesis, which are principally focused on the combination of the SERS technique with Raman handheld instruments and the development of quantitative methods in the pharmaceutical field based on this association. [less ▲]

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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 and 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 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 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 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 detailDevelopment of an analytical method for crystalline content determination in amorphous solid dispersions produced by Hot-Melt Extrusion using transmission Raman spectroscopy: A feasibility study.
Netchacovitch, Lauranne ULiege; Dumont, Elodie ULiege; Cailletaud, Johan ULiege et al

in International Journal of Pharmaceutics (2017), 530(1-2), 249-255

The development of a quantitative method determining the crystalline percentage in an amorphous solid dispersion is of great interest in the pharmaceutical field. Indeed, the crystalline Active ... [more ▼]

The development of a quantitative method determining the crystalline percentage in an amorphous solid dispersion is of great interest in the pharmaceutical field. Indeed, the crystalline Active Pharmaceutical Ingredient transformation into its amorphous state is increasingly used as it enhances the solubility and bioavailability of Biopharmaceutical Classification System class II drugs. One way to produce amorphous solid dispersions is the Hot-Melt Extrusion (HME) process. This study reported the development and the comparison of the analytical performances of two techniques, based on backscattering and transmission Raman spectroscopy, determining the crystalline remaining content in amorphous solid dispersions produced by HME. Principal Component Analysis (PCA) and Partial Least Squares (PLS) regression were performed on preprocessed data and tended towards the same conclusions: for the backscattering Raman results, the use of the DuoScan™ mode improved the PCA and PLS results, due to a larger analyzed sampling volume. For the transmission Raman results, the determination of low crystalline percentages was possible and the best regression model was obtained using this technique. Indeed, the latter acquired spectra through the whole sample volume, in contrast with the previous surface analyses performed using the backscattering mode. This study consequently highlighted the importance of the analyzed sampling volume. [less ▲]

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