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See detailEffect of different parameters on composition of volatile components of Myristica fragrans seeds extracted by hydrodistillation assisted by microwave and head-space solid-phase microextraction
Bouchachia, C; Benkaci-Ali, F; Eppe, Gauthier ULiege et al

in Journal of Essential Oil Research (in press)

Hydrodistillation assisted by microwave (HDAM) and Head space solid phase micro-extraction (HSSPME) of Myristica fragrans houtt (MF) were investigated. A kinetic study was performed for MF seeds using two ... [more ▼]

Hydrodistillation assisted by microwave (HDAM) and Head space solid phase micro-extraction (HSSPME) of Myristica fragrans houtt (MF) were investigated. A kinetic study was performed for MF seeds using two techniques (HDAM: Hydrodistillation assisted by microwave and SDAM: steam distillation assisted by microwave). The effect of the cryogenic grinding (CG) showed differences in yields and composition of volatile oils compared to the simple grinding (SG). HDAM–SG (3.4%) and SDAM–SG (2.55%) allowed extraction of substantial amounts of volatile oils in less time compared with HDAM–CG (4.75%) and SDAM–CG (3.8%). The kinetic study (differential and accumulated yields) of essential oil extraction was quantitatively and qualitatively performed showing a significant variation of composition with the extraction time, especially for accumulated yields such as sabinene (31.48–38.78%), α-pinene (12.74–14.09%) and β-pinene (10.01–12.11%). Similarly, the HS-SPME–GC–MS analysis showed also a significant variation of MF seeds volatile composition according some parameters as the type of fibre coating (PDMS: Polydimethylsiloxane and PDMS– DVB: Polydimethylsiloxane divenylbenzene), particle size, grinding mode and the mass used. The chemical groups (monoterpenoids, aliphatic and aromatic alcohols and esters) showed specific behaviour in SPME analysis. SPME sampling parameters were optimized for these components. [less ▲]

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See detailBio-chemical Raman imaging using targeted-SERS
Verdin, Alexandre ULiege; Malherbe, Cédric ULiege; Eppe, Gauthier ULiege et al

Poster (2017, September)

Raman and SERS spectral imaging, which consists in reconstructing a Raman intensity profile over a 2D or 3D section of a given sample (in presence or not of a nanosubstrate), allow to visualise the ... [more ▼]

Raman and SERS spectral imaging, which consists in reconstructing a Raman intensity profile over a 2D or 3D section of a given sample (in presence or not of a nanosubstrate), allow to visualise the variation of the chemical composition associated with the micro-structure of the sample. In particular, targeted-SERS imaging also enables the specific imaging of various macromolecules targeted by SERS probes in complex biological samples such as cancerous cells. To illustrate the versatility of Raman imaging, we describe two applications that were investigated recently in our laboratory. First, 3D Raman imaging was used to investigate a microcavity in a matrix of gypsum, revealing fossilised carbonaceous compounds dispersed in a filamentous shape, highly suggesting the presence of fossilised bacteria. Secondly, SERS probes were synthesised to specifically target the FRα receptor of folic acid which are often over-expressed at the surface of cancerous cells. Confocal Raman imaging was used to study the localization of the probes after incubation with KB cells (oral cancer) to confirm the specific targeting of FRα membrane receptors (Fig. 1). Moreover, our SERS probes allowed us to distinguish two different cancerous cell lines (namely KB and PC-3), based on the degree of expression of the FRα receptor of these two lines (high for KB and low for PC-3). In the future, these SERS probes may be used for distinguishing between cancerous and healthy cells since healthy cells have a lower degree of expression of FRα. [less ▲]

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See detailSpray-drying as a tool to disperse conductive carbon inside Na2FePO4F particles by addition of carbon black or carbon nanotubes to the precursor solution
Mahmoud, Abdelfattah ULiege; Caes, Sebastien; Brisbois, Magali et al

in Journal of Solid State Electrochemistry (2017)

In this work, Na2FePO4F-carbon composite powders were prepared by spray-drying a solution of inorganic precursors with 10 and 20 wt% added carbon black (CB) or carbon nanotubes (CNTs). In order to compare ... [more ▼]

In this work, Na2FePO4F-carbon composite powders were prepared by spray-drying a solution of inorganic precursors with 10 and 20 wt% added carbon black (CB) or carbon nanotubes (CNTs). In order to compare the effect of CB and CNTwhen added to the precursor solutions, the structural, electrochemical, and morphological properties of the synthesized Na2FePO4F-xCB and Na2FePO4F-xCNT samples were systematically investigated. In both cases, X-ray diffraction shows that calcination at 600 °C in argon leads to the formation of Na2FePO4F as the major inorganic phase. 57Fe Mössbauer spectroscopy was used as complementary technique to probe the oxidation states, local environment, and identify the composition of the iron-containing phases. The electrochemical performance is markedly better in the case of Na2FePO4F-CNT (20 wt%), with specific capacities of about 100 mAh/g (Na2FePO4F-CNT) at C/4 rate vs. 50 mAh/g for Na2FePO4F-CB (20 wt%). SEM characterization of Na2FePO4F-CB particles revealed different particle morphologies for the Na2FePO4F-CNT and Na2FePO4F-CB powders. The carbon-poor surface observed for Na2FePO4FCB could be due to a slow diffusion of carbon in the droplets during drying. On the contrary, Na2FePO4F-CNT shows a better CNT dispersion inside and at the surface of the NFPF particles that improves the electrochemical performance. [less ▲]

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See detailMicroplastics found in the stomach contents of Squalius cephalus from the Seine River
Collard, France ULiege; Gilbert, Bernard ULiege; Eppe, Gauthier ULiege et al

Poster (2017, June)

Microplastics (plastics < 5 mm) are emerging pollutants of growing concern. Since the 2000s their abundance, degradation and impacts on wildlife are more and more studied and understood. However, few data ... [more ▼]

Microplastics (plastics < 5 mm) are emerging pollutants of growing concern. Since the 2000s their abundance, degradation and impacts on wildlife are more and more studied and understood. However, few data are available particularly in freshwater ecosystems. Some fish species have plastic in their stomach contents such as: Gobio gobio, Alburnus alburnus, Leuciscus leuciscus while other species have not. In controlled conditions, microplastics were found to cause negative impacts in fish: leaching of micropollutants, endocrine disruption, hatching inhibition and decrease of growth rate of larvae. The first step in the understanding of these impacts is the quantification and the characterisation of ingested plastics by organisms in the field. Plastics and other anthropogenic particles (textile fibres) were isolated from 40 stomachs of Squalius cephalus (the European chub) collected in the Seine River (Paris) in August 2016. One station is upstream and the three others are downstream of the Paris Megacity conurbation. This megacity exerts a great pressure on the Seine River. Plastics were isolated thanks to a method using sodium hypochlorite and all particles were then analysed by Raman spectroscopy. The method consists in a degradation overnight of the organic matter in the stomach contents by sodium hypochlorite. This mixture is then filtrated and particles longer than 5 µm are resuspended into an ethanol (99%) solution for centrifugation. The precipitate, containing all particles denser than ethanol, is collected (1.3 ml) and spread on a mount for Raman spectroscopy. Several lasers were used, depending on the particle’s colour. Spectra were recorded with an accumulation ranging from 5 to 50s. Preliminary results showed that 7 individuals out of 25 already analysed (28%) had ingested at least one anthropogenic particle (AP). Eight APs were found and characterized, the majority of them (7) being dyed fibres. One of these fibres was made of a plastic polymer, the polyethylene terephthalate. The others were made of an undetermined material as Raman analyses gave only information on the dye. The eighth particle was a fragment of polypropylene. It is the first time that fish are studied as a part of plastic pollution in the Seine River. All isolated particles have been analysed leading to precise results. The percentage of occurrence is in the common range of other studies while much lower than the European flounder coming from the River Thames and higher than fish coming from Geneva Lake. It is not surprising that the majority of APs were fibres as another study in the river Seine found that the fibres concentration in water is far greater than the fragments concentration, as well as in urban runoff. It is also possible that the retention time of fibres in the gut is longer than fragments. Toxicological impacts of fibre ingestion is still unknown despite their ubiquity in many freshwater environments. [less ▲]

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See detailStraightforward prediction of the Ni1−xO layers stoichiometry by using optical and electrochemical measurements
Manceriu, Laura ULiege; Colson, Pierre ULiege; Maho, Anthony ULiege et al

in Journal of Physics : D Applied Physics (2017), 50

In this study, we propose a straightforward method for x determination in sub-stoichiometric nickel oxide (Ni1−xO) films prepared by ultrasonic spray pyrolysis on fluor-tin oxide (FTO) substrates by ... [more ▼]

In this study, we propose a straightforward method for x determination in sub-stoichiometric nickel oxide (Ni1−xO) films prepared by ultrasonic spray pyrolysis on fluor-tin oxide (FTO) substrates by varying the post-deposition thermal treatment. The Ni3+ concentration, the flat band potential (Φfb) and the open circuit potential (Voc) were determined by electrochemical impedance analysis in aqueous media and correlated to the transmission of Ni1−xO films. An x-ray photoelectron spectroscopy study was also performed to quantify the amount of Ni3+ in the films and compare it with the one determined by electrochemical analysis. The electrochromic behavior of the Ni1−xO films in non-aqueous electrolyte was investigated as well. With increasing Ni3+ concentration the films became more brownish and more conductive, both Voc and Φfb values increased. Calibration curves of transmission at 550 nm or open circuit potential versus carrier concentration were plotted and allowed the prediction of x in an unknown Ni1−xO sample. The Ni1−xO films characterized by the highest Ni3+ concentration have a darker colored state but lower transmission modulation, due to their reduced specific surface and increased crystallinity. [less ▲]

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See detailMetabolic inhibitors accentuate the anti-tumoral effect of HDAC5 inhibition
Hendrick, Elodie ULiege; Peixoto, Paul; Blomme, Arnaud et al

in Oncogene (2017)

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See detailSpatial variation in the accumulation of POPs and mercury in bottlenose dolphins of the Lower Florida Keys and the coastal Everglades (South Florida)
Damseaux, France ULiege; Kiszka, J.; Heithaus, M.R. et al

in Environmental Pollution (2017), 220

The bottlenose dolphin (Tursiops truncatus) is an upper trophic level predator and the most common cetacean species found in nearshore waters of southern Florida, including the Lower Florida Keys (LFK ... [more ▼]

The bottlenose dolphin (Tursiops truncatus) is an upper trophic level predator and the most common cetacean species found in nearshore waters of southern Florida, including the Lower Florida Keys (LFK) and the Florida Coastal Everglades (FCE). The objective of this study was to assess contamination levels of total mercury (T-Hg) in skin and persistent organic pollutants (PCBs, PBDEs, DDXs, HCHs, HCB, Σ PCDD/Fs and Σ DL-PCBs) in blubber samples of bottlenose dolphins from LFK (n = 27) and FCE (n = 24). PCBs were the major class of compounds found in bottlenose dolphin blubber and were higher in individuals from LFK (Σ 6 PCBs LFK males: 13421 ± 7730 ng.g-1 lipids, Σ 6 PCBs LFK females: 9683 ± 19007 ng.g-1 lipids) than from FCE (Σ 6 PCBs FCE males: 5638 ng.g-1 ± 3627 lipids, Σ 6 PCBs FCE females: 1427 ± 908 ng.g-1 lipids). These levels were lower than previously published data from the southeastern USA. The Σ DL-PCBs were the most prevalent pollutants of dioxin and dioxin like compounds (Σ DL-PCBs LFK: 739 ng.g-1 lipids, Σ DL-PCBs FCE: 183 ng.g-1 lipids) since PCDD/F concentrations were low for both locations (mean 0.1 ng.g-1 lipids for LFK and FCE dolphins). The toxicity equivalences of PCDD/Fs and DL-PCBs expressed as TEQ in LFK and FCE dolphins is mainly expressed by DL-PCBs (81% LFK - 65% FCE). T-Hg concentrations in skin were significantly higher in FCE (FCE median 9314 ng.g-1 dw) compared to LFK dolphins (LFK median 2941 ng.g-1 dw). These bottlenose dolphins concentrations are the highest recorded in the southeastern USA, and may be explained, at least partially, by the biogeochemistry of the Everglades and mangrove sedimentary habitats that create favourable conditions for the retention of mercury and make it available at high concentrations for aquatic predators. [less ▲]

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See detailMorphology of the filtration apparatus of three planktivorous fishes and relation with ingested anthropogenic particles
Collard, France ULiege; Gilbert, Bernard ULiege; Eppe, Gauthier ULiege et al

in Marine Pollution Bulletin (2017)

Anthropogenic particles (APs), including microplastics, are ingested by a wide variety of marine organisms. Exposure of Clupeiformes (e.g. herrings, anchovies, sardines) is poorly studied despite their ... [more ▼]

Anthropogenic particles (APs), including microplastics, are ingested by a wide variety of marine organisms. Exposure of Clupeiformes (e.g. herrings, anchovies, sardines) is poorly studied despite their economic and ecological importance. This study aims to describe the morphology of the filtration apparatus of three wild-caught Clupeiformes (Sardina pilchardus, Clupea harengus and Engraulis encrasicolus) and to relate the results to ingested APs. Consequently, the species with the more efficient filtration apparatus will be more likely to ingest APs. We hypothesized that sardines were the most exposed species. The filtration area and particle retention threshold were determined in the three species, with sardines displaying the highest filtration area and the closest gill rakers. Sardines ingested more fibers and smaller fragments, confirming that it is the most efficient filtering species. These two results lead to the conclusion that, among the three studied, the sardine is the species most exposed to APs. [less ▲]

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See detailOn the Habitability of Desert Varnish: a Combined Study by Micro-Raman Spectroscopy, X-Ray Diffraction and Methylated Pyrolysis-Gas Chromatography-Mass Spectrometry
Malherbe, Cédric ULiege; Hutchinson, Ian; Ingley, Richard et al

in Astrobiology (2017)

In 2020, the ESA ExoMars and NASA Mars 2020 missions will be launched to Mars, searching for evidence of past and present life. In preparation for these missions, terrestrial analogue samples of rock ... [more ▼]

In 2020, the ESA ExoMars and NASA Mars 2020 missions will be launched to Mars, searching for evidence of past and present life. In preparation for these missions, terrestrial analogue samples of rock formations on Mars are studied in detail in order to optimize the scientific information that the analytical instrumentation will return. Desert varnishes are thin mineral coatings found on rocks in arid and semi-arid environments on Earth that are recognized as analogue samples. During the formation of desert varnishes (which takes many hundreds of years) organic matter is incorporated and microorganisms may also play an active role in the formation process. During this study, four complementary analytical techniques proposed for Mars missions (X-rays diffraction, Raman spectroscopy, elemental analysis and pyrolysis-gas chromatography-mass spectrometry) were used to interrogate samples of desert varnish and to describe their capacity to sustain life under extreme scenario. For the first time, both the geochemistry and the organic compounds associated with desert varnish are described using an identical set of samples. XRD and Raman spectroscopy measurements were used to non-destructively interrogate the mineralogy of the samples. In addition, the use of Raman spectroscopy instruments enabled the detection of β-carotene, a highly Raman active biomarker. The content and the nature of the organic material in the samples was further investigated using elemental analysis and methylated Py-GC-MS and a bacterial origin was determined to be likely. In the context of planetary exploration, we describe the habitable nature of desert varnish based on the bio-geochemical composition of the samples. Possible interference of the geological substrate on the detectability of pyrolysis products is also suggested. [less ▲]

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See detailExploring the Fundamentals of Microreactor Technology with Multidisciplinary Lab Experiments Combining the Synthesis and Characterization of Inorganic Nanoparticles
Emmanuel, Noémie ULiege; Emonds-Alt, Gauthier ULiege; Lismont, Marjorie et al

in Journal of Chemical Education (2017)

Multidisciplinary lab experiments combining microfluidics, nanoparticle synthesis and characterization are presented. These experiments rely on the implementation of affordable yet efficient microfluidic ... [more ▼]

Multidisciplinary lab experiments combining microfluidics, nanoparticle synthesis and characterization are presented. These experiments rely on the implementation of affordable yet efficient microfluidic setups based on PFA capillary coils and standard HPLC connectors in upper undergraduate chemistry labs. Fundamental principles and concepts, as well as practical tips for the rapid deployment of microfluidics are presented. In-line membrane separation, segmented-flow regime, high temperature experiments, and in-line analytical techniques are illustrated with the preparation of inorganic nanoparticles (silver, gold, cadmium selenide or telluride) in microreactors. Besides microfluidics, analytical techniques for nanoparticle analysis are also illustrated. [less ▲]

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See detailPerinatal programming of depressive-like behavior by inflammation in adult offspring mice whose mothers were fed polluted eels: Gender selective effects
Soualed, Nidhal; Dridi, Imen; Eppe, Gauthier ULiege et al

in Brain, Behavior & Immunity (2017), 63

Several lines of evidence indicate that early-life inflammation may predispose to mental illness, including depression, in later-life. We investigated the impact of perinatal exposure to polluted eels on ... [more ▼]

Several lines of evidence indicate that early-life inflammation may predispose to mental illness, including depression, in later-life. We investigated the impact of perinatal exposure to polluted eels on neonatal, postnatal, and adult brain inflammation, and on the resignation behavior of male and female adult offspring mice. The effects of maternal standard diet (laboratory food) were compared to the same diet enriched with low, intermediate, or highly polluted eels. Brain inflammatory markers including cytokines were assessed in offspring mice on the day of birth (i.e., on the postnatal day–PND 1), upon weaning (PND 21) and at adulthood (PND 100). Plasma myeloperoxidase and corticosterone levels were evaluated at PND 100. Immobility behavior of offspring was assessed in adulthood (i.e., at PNDs 95–100), using the tail suspension and forced swimming tests. Chronic brain inflammation was found in male and female offspring mice compared to controls, as assessed at PNDs 1, 21, and 100. The level of myeloperoxidase was found to be significantly higher in both adult males and females vs. control offspring. However, high corticosterone levels were only found in male offspring mice that were perinatally exposed to eels, suggesting a gender-selective dysregulation of the adult hypothalamicpituitaryadrenal (HPA) axis. Gender-specific differences were also detected in adulthood in regard to offspring resignation behavior. Thus, compared to controls, males, but not females, whose mothers were fed eels during pregnancy and lactation exhibited a depressive-like behavior in adult age in both behavioral models of depression. Depressive symptoms were more pronounced in male mice perinatally exposed to either intermediate or highly polluted eels than those exposed to only lowly polluted eels. Our results indicate that early-life inflammatory insult is a plausible causative factor that induce the depressive phenotype exhibited by male adult offspring mice, most likely through a gender-specific HPA axis enhanced activation. [less ▲]

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See detailGuidance Document on Measurement Uncertainty for Laboratories performing PCDD/F and PCB analysis using Isotope Dilution Mass Spectrometry
Eppe, Gauthier ULiege; Schaechtele, Alexander; Haedrich, Johannes et al

Report (2017)

This document on measurement uncertainty was developed within the network of the European Union Reference Laboratory (EURL) for Dioxins and PCBs in Feed and Food and the respective National Reference ... [more ▼]

This document on measurement uncertainty was developed within the network of the European Union Reference Laboratory (EURL) for Dioxins and PCBs in Feed and Food and the respective National Reference Laboratories (NRLs) of member states. Detailed guidance is given on the evaluation of measurement uncertainty in the quantitative analysis of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) and polychlorinated biphenyls (PCBs), to assist laboratories performing official feed and food control within the European Union, especially National Reference Laboratories (NRLs) and Official Laboratories (OFLs). It provides useful key elements contributing to further harmonization of compliance assessment and outlines practical aspects related to measurement uncertainty estimation. A new concept placing special emphasis on the inclusion of current method performance data is presented. The concept covers the full analytical process from sample receipt at the laboratory through sample storage, preparation and analysis, to data processing and reporting. In particular, it focuses on the role of analytical variability generally known as "measurement uncertainty" (MU) in the interpretation of analytical results for assessment of their compliance with a specification. Effects from sampling [EURACHEM/CITAC 2007, /18/] and transport also contributing to MU are acknowledged but not treated within the scope of this document. Two selected approaches for measurement uncertainty estimation are proposed for the determination of PCDD/Fs and PCBs in food and feed by gas chromatography-mass spectrometry (GC-MS) using internal standard stable isotope labelled analogues. An empirical, or “top-down”, approach combines contributions from intermediate (intra-laboratory) precision and trueness (expressed as bias) to estimate measurement uncertainty, both for individual congeners and for sum parameters. The working group recommends the use of the empirical approach as described in this document as the main option for MU estimation, because it is designed and developed to cover the whole analytical process and also includes the opportunity to reassess or update MU on a regular basis. However, an alternative methodology based on a semi-empirical approach following the EURACHEM/CITAC guide [EURACHEM/CITAC 2012, /12/] is also presented. It has been designed for laboratories new to this type of analysis that have generated data from initial validation studies. In this case the semi-empirical approach may be a good starting point, however the authors recommend implementing the empirical or top-down approach once enough data have been gathered. [less ▲]

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See detailEffect of the Extraction Technique, Heating Time and Cryogenic Grinding (N2 at -196°C) on the Composition of Cumin Seeds Volatile Oil
Mékaoui, R; Benkaci-Ali, Farid; Scholl, Georges ULiege et al

in Journal of Essential Oil-Bearing Plants [=JEOBP] (2016), 19(8), 1903-1919

Two techniques of extraction of essential oils (Steam distillation assisted by microwave (SDAM) and hydrodistillation assisted by microwave (HDAM)) are respectively advanced steam distillation (SD) and ... [more ▼]

Two techniques of extraction of essential oils (Steam distillation assisted by microwave (SDAM) and hydrodistillation assisted by microwave (HDAM)) are respectively advanced steam distillation (SD) and hydrodistillation techniques (HD), in which a microwave oven is used in the extraction process. They are considered as accelerated techniques extraction performed at atmospheric pressure. The cryogrinding (CG) showed a difference on the yields and aromatic profile comparing to the sample grinding. Isolation and concentration of volatile compounds are performed by a single stage for the extraction of volatile oil from Algerian (Sahara) Cuminum cyminum seeds (CCS). The chemical composition of the essential oil of this plant as a function of extraction time was also studied. The major components and family classes showed a significant variation with the extraction time. Gas chromatography (GC), GCxGC-mass spectrometry (GCxGC-MS)] were utilised for qualitative and quantitative analysis of essential oils extracted by these two methods. The major compounds are cumin aldehyde (HDAM-CG: 20.50-53.35 %, SDAM-CG: 21.68 66.6 %), p-cymene (HDAM-CG: 14.1-37.54 %, SDAM-CG: 6.06-20.18 %), β-pinene (HDAM-CG: 4.53-14.74 %, SDAM-CG: 4.3-32.65 %) and γ-terpinene (HDAM-CG: 1.26-14.70 %, SDAM-CG: 5.13-18.23 %). [less ▲]

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See detailIntegrated microfluidic device for the synthesis of SERS substrates
Emonds-Alt, Gauthier ULiege; Malherbe, Cédric ULiege; Monbaliu, Jean-Christophe ULiege et al

Poster (2016, December 19)

The goal of this work is to develop a quantitative analytical method for the glyphosate and its major metabolite the aminomethylphosphonic acid (AMPA) by coupling microfluidics with surface enhanced Raman ... [more ▼]

The goal of this work is to develop a quantitative analytical method for the glyphosate and its major metabolite the aminomethylphosphonic acid (AMPA) by coupling microfluidics with surface enhanced Raman spectroscopy (SERS). This work is divided into 4 axes : (a) bimetallic nanoparticles synthesis in a microreactor, (b) nanoparticles functionnalisation, (c) SERS quantification of glyphosate/AMPA and (d) miniature prototype development composed of axes a to c. The first section aims at the synthesis of bimetallic nanoparticles (Au-Ag, Au-Cu and Ag-Cu) in a microfluidic device. This microfluidic device integrates a first section for the synthesis of monometallic nanoparticles (core) and a second section for the reductive deposition of a second metal (shell). The second axe of this work deals with the functionnalisation of nanoparticles to improve the selectivity of this method for the selected analytes. Two types of functionnalisation are studied : PEGylation (a) with multi-arm PEG ending with -SH and/or (b) with linear heterobifunctionnal PEG. The third axe consists in measuring quantitatively glyphosate and AMPA in different matrices, such as water, urine and fruit juice. Finally, the forth axe deals with the development of a portable detection system to perform on-site analysis. This prototype integrates the microfluidic device for nanoparticles synthesis, their functionnalisation, an injection port followed by a mixing section for the sample and an integrated Raman spectrometer for in-line analysis. [less ▲]

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See detailRaman imaging for diagnostic application
Malherbe, Cédric ULiege; Gilbert, Bernard ULiege; Eppe, Gauthier ULiege

Poster (2016, December 19)

Specific dynamic biochemical compositions and molecular structures characterise healthy cells and tissues. This also stands for pathologies or cellular abnormalities which are accompanied by biochemical ... [more ▼]

Specific dynamic biochemical compositions and molecular structures characterise healthy cells and tissues. This also stands for pathologies or cellular abnormalities which are accompanied by biochemical and molecular changes. Raman spectroscopy can provide unique inputs to correlate the molecular composition and its variations with the diagnosis. In addition, the presence of metal nanoparticles in the molecule vicinity induces a remarkable enhancement (up to 1000000 times) of the Raman signal of small molecules (known as SERS effect). It opens towards applications in the field of trace analysis. In preparation for clinical applications, we evaluate, by Raman mapping, the signal detected from a SERS target deposited on solid state support. [less ▲]

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See detailThe performance of atmospheric pressure gas chromatography–tandem mass spectrometry compared to gas chromatography–high resolution mass spectrometry for the analysis of polychlorinated dioxins and PCBs in food and feed samples
ten Dam, Guillaume; Pussente, Igor; Scholl, Georges ULiege et al

in Journal of Chromatography. A (2016), 1477

Recently, gas chromatography tandem mass spectrometry (GC–MS/MS) has been added in EuropeanUnion (EU) legislation as an alternative to magnetic sector high resolution mass spectrometry (HRMS) for the ... [more ▼]

Recently, gas chromatography tandem mass spectrometry (GC–MS/MS) has been added in EuropeanUnion (EU) legislation as an alternative to magnetic sector high resolution mass spectrometry (HRMS) for the analysis of dioxins and dioxin like polychlorinated biphenyls (dl-PCB) in food and feed. In this study the performance of APGC–MS/MS compared to GC–HRMS is investigated and compared with EU legislation. The study includes the legislative parameters, relative intermediate precision standard devia-tion (SRw,rel), trueness, sensitivity, linear range and ion ratio tolerance. In addition, over 200 real samplesof large variety and spanning several orders of magnitude in concentration were analyzed by both techniques and the selectivity was evaluated by comparing chromatograms. The SRw,rel and trueness were evaluated using (in-house) reference samples and fulfill to EU legislation, though the SRw,rel was better with GC–HRMS. The sensitivity was considerably better than of GC–HRMS while the linear range was similar. Ion ratios were mostly within the tolerable range of ±15%. A (temporary unresolved) systematic deviation in ion ratio was observed for several congeners, yet this did not lead to exceeding of the maxi-mum ion ratio limits. The APGC–MS/MS results for the non-dioxin-like-PCBs (ndl-PCBs) were negatively biased, particularly for PCB138 and 153 in contaminated samples. The selectivity of APGC–MS/MS was lower for several matrices. Particularly for contaminated samples, interfering peaks were observed in the APGC chromatograms of the native compounds (dioxins) and labeled internal standards (PCBs). These can lead to biased results and ultimately to false positive samples. It was concluded that the determination of dioxins and PCBs using APGC–MS/MS meets the requirements set by the European Commission. However, due to generally better selectivity and SRw,rel, GC–HRMS is the preferred method for monitoring purposes. [less ▲]

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