References of "Fillet, Marianne"
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See detailSimultaneous analysis of nucleobases, nucleosides and ginsenosides in ginseng extracts using supercritical fluid chromatography coupled with single quadrupole mass spectrometry
Huang, Yang ULiege; Zhang, Tingting; Zhao, Yumei et al

in Journal of Pharmaceutical and Biomedical Analysis (2017), 144(213), 219

Nucleobases, nucleosides and ginsenosides, which have a significant impact on the physiological activity of organisms, are reported to be the active components of ginseng, while they are less present in ... [more ▼]

Nucleobases, nucleosides and ginsenosides, which have a significant impact on the physiological activity of organisms, are reported to be the active components of ginseng, while they are less present in ginseng extracts. Few analytical methods have been developed so far to simultaneously analyze these three classes of compounds with different polarities present in ginseng extracts. In the present study, a simple and efficient analytical method was successfully developed for the simultaneous separation of 17 nucleobases, nucleosides and ginsenosides in ginseng extracts using supercritical fluid chromatography coupled with single quadrupole mass spectrometry (SFC-MS). The effect of various experimental factors on the separation performance, such as the column type, temperature and backpressure, the type of modifier and additive, and the concentration of make-up solvent were systematically investigated. Under the selected conditions, the developed method was successfully applied to the quality evaluation of 14 batches of ginseng extracts from different origins. The results obtained for the different batches indicate that this method could be employed for the quality assessment of ginseng extracts [less ▲]

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See detailLc-chip versus UHPLC-tandem mass spectrometry for the quantitation of estetrol and estradiol without derivatization after whole blood microsampling
Nys, Gwenaël ULiege; Servais, Anne-Catherine ULiege; Pequeux, Christel ULiege et al

Conference (2017, March 29)

the aim of this work was to conduct a PK study on mice to select the most appropriate administration route for E2 and E4 formulations. To achieve this goal, a reference method for the quantitation of both ... [more ▼]

the aim of this work was to conduct a PK study on mice to select the most appropriate administration route for E2 and E4 formulations. To achieve this goal, a reference method for the quantitation of both estrogens after whole blood microsampling was developed and validated on a UHPLC-MS/MS system. This reference method was later transferred on LC-chip device and both methods were compared in terms of analytical parameters such as response function, accuracy, precision, trueness and limit of quantification. [less ▲]

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See detailDevelopment and validation of a fast SFC method for the analysis of flavonoids in plant extracts
Huang, Yang ULiege; Feng, Ying; Tang, Guangyun et al

in Journal of Pharmaceutical and Biomedical Analysis (2017), 140

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See detailBioavailability enhancement of itraconazole-based solid dispersions produced by hot melt extrusion in the framework of the Three Rs rule
Thiry, Justine ULiege; Kok, Miranda ULiege; Collard, Laurence ULiege et al

in European Journal of Pharmaceutical Sciences (2017), 99

Solid dispersion formulations made of itraconazole (ITZ) and Soluplus® (polyethylene glycol, polyvinyl acetate and polyvinylcaprolactame-based graft copolymer abbreviated SOL) were produced using hot melt ... [more ▼]

Solid dispersion formulations made of itraconazole (ITZ) and Soluplus® (polyethylene glycol, polyvinyl acetate and polyvinylcaprolactame-based graft copolymer abbreviated SOL) were produced using hot melt extrusion. Since ITZ possesses a water solubility of less than 1 ng/mL, the aim of this work was to enhance the aqueous solubility of ITZ, and thereby improve its bioavailability. The three formulations consisted of a simple SOL/ITZ amorphous solid dispersion (ASD), an optimized SOL/ITZ/AcDiSol® (super-disintegrant) ASD and an equimolar inclusion complex of ITZ in hydroxypropyl-β-cyclodextrin (substitution degree = 0.63, CD) with SOL. The three formulations were compared in vitro and in vivo to the marketed product Sporanox®. The in vitro enhancement of dissolution rate was evaluated using a biphasic dissolution test. In vitro dissolution results showed that all three formulations had a higher percentage of ITZ released than Sporanox® with the following ranking: SOL/ITZ/CD > SOL/ITZ/AcDiSol® > SOL/ITZ > Sporanox®. The bioavailability of these four formulations was evaluated in rats. The bioanalytical method was optimized so that only 10 μL of blood was withdrawn from the rats using specific volumetric absorptive microsampling devices. This enabled to keep the same rats during the whole study, which was in accordance with the Three Rs rules (reduction, refinement and replacement). Furthermore, this technique allowed the suppression of inter-individual variability. Higher Cmax and AUC were obtained after the administration of all three formulations compared to the levels after the use of Sporanox® as follows: SOL/ITZ/AcDiSol® > SOL/ITZ/CD > SOL/ITZ > Sporanox®. The inversion in the ranking between SOL/ITZ/CD and SOL/ITZ/AcDiSol® made impossible the establishment of an in vitro–vivo correlation. Indeed, very different release rates were obtained in vitro and in vivo for the two optimized formulations. These results suggest that ITZ would be protected inside the core of the SOL micelles even during the absorption step at the intestine, while some agents present in the intestinal fluids could displace ITZ from the hydrophobic cavity of CD by competition. [less ▲]

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See detailVolumetric absorptive microsampling: Current advances and applications.
Kok, Miranda ULiege; Fillet, Marianne ULiege

in Journal of Pharmaceutical & Biomedical Analysis (2017)

Recently, volumetric absorptive microsampling (VAMS) has been introduced for the sampling of biological fluids, and more particularly whole blood, on a porous hydrophilic tip. VAMS enables the collection ... [more ▼]

Recently, volumetric absorptive microsampling (VAMS) has been introduced for the sampling of biological fluids, and more particularly whole blood, on a porous hydrophilic tip. VAMS enables the collection of small, accurate and precise blood volumes (10 or 20muL) regardless of the hematocrit. After drying, the samples can be stored or directly analyzed. The stability of various compounds in dried samples supported on VAMS tips varies from one day to a few months at room temperature, and increases at lower temperatures. The complete tip is used during a simple and straightforward sample preparation. Compounds can be extracted with a variety of solvents, and thereafter directly analyzed. A design of experiments is recommended to determine the optimal extraction conditions for a reproducible recovery. The recovery of compounds might be influenced by the hematocrit. In the last two years, various pharmacokinetic and therapeutic drug monitoring studies have been conducted with VAMS. This review covers the general aspects related with the use of VAMS and its applicability is demonstrated through examples. [less ▲]

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See detailPartial filling affinity capillary electrophoresis as a useful tool for fragment-based drug discovery: A proof of concept on thrombin.
Farcas, E.; Bouckaert, C.; Servais, Anne-Catherine ULiege et al

in Analytica Chimica Acta (2017), 984

With the emergence of more challenging targets, a relatively new approach, fragment-based drug discovery (FBDD), proved its efficacy and gained increasing importance in the pharmaceutical industry. FBDD ... [more ▼]

With the emergence of more challenging targets, a relatively new approach, fragment-based drug discovery (FBDD), proved its efficacy and gained increasing importance in the pharmaceutical industry. FBDD identifies low molecular-weight (MW) ligands (fragments) that bind to biologically important macromolecules, then a structure-guided fragment growing or merging approach is performed, contributing to the quality of the lead. However, to select the appropriate fragment to be evolved, sensitive analytical screening methods must be used to measure the affinity in the muM or even mM range. In this particular context, we developed a robust and selective partial filling affinity CE (ACE) method for the direct binding screening of a small fragment library in order to identify new thrombin inhibitors. To demonstrate the accuracy of our assay, the complex dissociation constants of three known thrombin inhibitors, namely benzamidine, p-aminobenzamidine and nafamostat were determined and found to be in good concordance with the previously reported values. Finally, the screening of a small library was performed and demonstrated the high discriminatory power of our method towards weak binders compared to classical spectrophotometric activity assay, proving the interest of our method in the context of FBDD. [less ▲]

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See detailSampling only ten microliters of whole blood for the quantification of poorly soluble drugs: Itraconazole as case study
Thiry, Justine ULiege; Evrard, Brigitte ULiege; Nys, Gwenaël ULiege et al

in Journal of Chromatography. A (2017), 1479

Nowadays in animal studies, it is important to comply with the so-called Three Rs rule by replacing or reducing the number of tested animals. Volumetric absorptive microsampling (VAMS) can be used to ... [more ▼]

Nowadays in animal studies, it is important to comply with the so-called Three Rs rule by replacing or reducing the number of tested animals. Volumetric absorptive microsampling (VAMS) can be used to collect small quantities (10 or 20 µL) of whole blood, thereby limiting the amount of animals needed. In this study, a quantitative method was developed and subsequently validated for the poorly soluble drug itraconazole (ITZ) using VAMS and ultra-high performance liquid chromatography (UHPLC) coupled to tandem mass spectrometry (MS). A proof of concept study showed that the optimized method is applicable to test the bioavailability of drug formulations containing ITZ. Using VAMS, smaller blood volumes can be taken per sampling point (10-20 µL instead of the conventional 0.2-0.5 mL) avoiding the sacrifice of animals. Moreover, the same rats can be used to compare different drug formulations which strengthens the validity of the results. In long-term bioavailability studies, it is necessary to guarantee the stability of the tested drugs supported on VAMS devices. In this study, we show that ITZ was only stable for 24 hours after collection with VAMS, but for at least two weeks by the storage of extracted samples at -80°C. [less ▲]

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See detailQuantitation and biospecific identification of virus-like particles of human papillomavirus by capillary electrophoresis.
Bettonville, Virginie ULiege; Nicol, Jerome T. J.; Furst, Tania et al

in Talanta (2017), 175

Capillary electrophoresis (CE) for HPV-VLP quantitation is a very interesting alternative technique compared to those currently used in viral analysis, such as SDS-PAGE, Western blot or protein assay that ... [more ▼]

Capillary electrophoresis (CE) for HPV-VLP quantitation is a very interesting alternative technique compared to those currently used in viral analysis, such as SDS-PAGE, Western blot or protein assay that are destructive and semi-quantitative or non specific. In this study, the quantitative performance of the CE method was evaluated. A main issue in virus quantitation is the absence of reference material. Therefore, the concentration of a HPV16-VLP sample produced in the laboratory was determined using ELISA with Gardasil(R), after adjuvant dissolution, as reference material and conformational H16.V5 antibody. HPV16-VLP concentration was found to influence particles electrophoretic mobility until a plateau was reached for concentrations </= 50microgml-1. As zeta potential is directly proportional to the electrophoretic mobility, it was measured at different HPV-VLP concentrations and the results were in complete accordance with the measured electrophoretic mobilities. The concentration dependence of the electrophoretic mobility could be explained by an overlap of the electrical double layers of adjacent particles. The HPV16-VLP peak identity was demonstrated unequivocally by the study of HPV16-VLP/H16.V5 antibody complex formation using affinity CE. Finally, the CE method was successfully validated following the ICH Q2R1 guidelines. To overcome the sample heterogeneity issue, a well-designed sample preparation was used. Considering sample complexity, validation results were satisfactory with maximum repeatability and intermediate precision RSD of 12.2% and a maximum relative bias of 1.4%. [less ▲]

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See detailValidation of a new method by nano-liquid chromatography on chip tandem mass spectrometry for combined quantitation of C3f and the V65 vitronectin fragment as biomarkers of diagnosis and severity of osteoarthritis.
Cobraiville, Gael; Fillet, Marianne ULiege; Sharif, Mohammed et al

in Talanta (2017), 169

Microfluidic liquid chromatography coupled to a nanoelectrospray source ion trap mass spectrometry was used for the absolute and simultaneous quantitation of C3f and the V65 vitronectin fragment in serum ... [more ▼]

Microfluidic liquid chromatography coupled to a nanoelectrospray source ion trap mass spectrometry was used for the absolute and simultaneous quantitation of C3f and the V65 vitronectin fragment in serum. The method was first carefully optimized and then validated in serum biological matrix. Stable isotopes for the two biomarkers of interest were used as stable isotope labeled peptide standards. A weighted 1/x2 quadratic regression for C3f and a weighted 1/x quadratic regression for the V65 vitronectin peptide were selected for calibration curves. Trueness (with a relative bias <10%), precision (repeatability and intermediate precision <15%) and accuracy (risk <15%) of the method were successfully demonstrated. The linearity of results was validated in the concentration range of 2.5-200ng/mL for C3f and 2.5-100ng/mL for the V65 vitronectin fragment. Serum samples (n=147) classified in 7 groups [(healthy volunteers, OA with 5 grades of severity and rheumatoid arthritis (RA) patients] were analyzed with our new quantitative method. Our data confirm that C3f and the V65 vitronectin fragment are biomarkers of OA severity, but also that C3f fragment is further related to OA severity whereas the V65 vitronectin fragment is more related to early OA detection. [less ▲]

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See detail(+) or (-)-1-(9-fluorenyl)ethyl chloroformate as chiral derivatizing agent: A review.
Moldovan, Radu-Cristian ULiege; Bodoki, Ede; Servais, Anne-Catherine ULiege et al

in Journal of Chromatography. A (2017), 1513

Over the last 30years, (+/-)-1-(9-fluorenyl)ethyl chloroformate ((+/-)-FLEC) was used as a chiral derivatizing agent in various analytical applications involving a wide range of endogenous, pharmaceutical ... [more ▼]

Over the last 30years, (+/-)-1-(9-fluorenyl)ethyl chloroformate ((+/-)-FLEC) was used as a chiral derivatizing agent in various analytical applications involving a wide range of endogenous, pharmaceutical and environmentally relevant molecules. This comprehensive review aims to present all the significant aspects related to the state of the art in FLEC labeling and subsequent chiral separation of the resulting diastereomers using LC, SFC and CE techniques. [less ▲]

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See detailSimultaneous analysis of nucleobases, nucleosides and ginsenosides in ginseng extracts using supercritical fluid chromatography coupled with single quadrupole mass spectrometry.
Huang, Yang; Zhang, Tingting; Zhao, Yumei et al

in Journal of Pharmaceutical & Biomedical Analysis (2017)

Nucleobases, nucleosides and ginsenosides, which have a significant impact on the physiological activity of organisms, are reported to be the active components of ginseng, while they are less present in ... [more ▼]

Nucleobases, nucleosides and ginsenosides, which have a significant impact on the physiological activity of organisms, are reported to be the active components of ginseng, while they are less present in ginseng extracts. Few analytical methods have been developed so far to simultaneously analyze these three classes of compounds with different polarities present in ginseng extracts. In the present study, a simple and efficient analytical method was successfully developed for the simultaneous separation of 17 nucleobases, nucleosides and ginsenosides in ginseng extracts using supercritical fluid chromatography coupled with single quadrupole mass spectrometry (SFC-MS). The effect of various experimental factors on the separation performance, such as the column type, temperature and backpressure, the type of modifier and additive, and the concentration of make-up solvent were systematically investigated. Under the selected conditions, the developed method was successfully applied to the quality evaluation of 14 batches of ginseng extracts from different origins. The results obtained for the different batches indicate that this method could be employed for the quality assessment of ginseng extracts. [less ▲]

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See detailDevelopment and validation of a fast SFC method for the analysis of flavonoids in plant extracts.
Huang, Yang; Feng, Ying; Tang, Guangyun et al

in Journal of Pharmaceutical & Biomedical Analysis (2017), 140

Flavonoids from plants always show a wide range of biological activities. In the present study, a rapid and highly efficient supercritical fluid chromatography (SFC) method was developed for the ... [more ▼]

Flavonoids from plants always show a wide range of biological activities. In the present study, a rapid and highly efficient supercritical fluid chromatography (SFC) method was developed for the separation of 12 flavonoids. After careful optimization, the 12 flavonoids were baseline separated on a ZORBAX RX-SIL column using gradient elution. A 0.1% phosphoric acid solution in methanol was found to be the most suitable polar mobile phase component for the separation of flavonoids. From the viewpoint of retention and resolution, a backpressure of 200bar and a temperature of 40 degrees C were shown to give the best results. Compared with a previously developed reverse phase liquid chromatography method, the SFC method could provide flavonoid separations that were about three times faster, while maintaining good peak shape and comparable peak efficiency. This SFC method was validated and applied to the analysis of five flavonoids (kaempferol, luteolin, quercetin, luteoloside, buddleoside) present in Chrysanthemum morifolium Ramat. from different cultivars (Chuju, Gongju, Hangju, Boju). The results indicated a good repeatability and sensitivity for the quantification of the five analytes with RSDs for overall precision lower than 3%. The limits of detection ranged from 0.73 to 2.34mug/mL, while the limits of quantification were between 2.19 and 5.86mug/mL. The method showed that SFC could be employed as a useful tool for the quality assessment of Traditional Chinese medicines (TCMs) containing flavonoids as active components. [less ▲]

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See detailVolumetric absorptive microsampling: Current advances and applications.
Kok, Miranda ULiege; Fillet, Marianne ULiege

in Journal of Pharmaceutical & Biomedical Analysis (2017)

Recently, volumetric absorptive microsampling (VAMS) has been introduced for the sampling of biological fluids, and more particularly whole blood, on a porous hydrophilic tip. VAMS enables the collection ... [more ▼]

Recently, volumetric absorptive microsampling (VAMS) has been introduced for the sampling of biological fluids, and more particularly whole blood, on a porous hydrophilic tip. VAMS enables the collection of small, accurate and precise blood volumes (10 or 20muL) regardless of the hematocrit. After drying, the samples can be stored or directly analyzed. The stability of various compounds in dried samples supported on VAMS tips varies from one day to a few months at room temperature, and increases at lower temperatures. The complete tip is used during a simple and straightforward sample preparation. Compounds can be extracted with a variety of solvents, and thereafter directly analyzed. A design of experiments is recommended to determine the optimal extraction conditions for a reproducible recovery. The recovery of compounds might be influenced by the hematocrit. In the last two years, various pharmacokinetic and therapeutic drug monitoring studies have been conducted with VAMS. This review covers the general aspects related with the use of VAMS and its applicability is demonstrated through examples. [less ▲]

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See detailCapillary electrophoresis in the context of drug discovery.
Farcas, Elena ULiege; Pochet, Lionel; Crommen, Jacques ULiege et al

in Journal of Pharmaceutical & Biomedical Analysis (2017)

Capillary Electrophoresis is a very efficient and resolutive separation technique used for many years in the analytical field. Despite all its assets, CE remains poorly used in drug discovery. This can be ... [more ▼]

Capillary Electrophoresis is a very efficient and resolutive separation technique used for many years in the analytical field. Despite all its assets, CE remains poorly used in drug discovery. This can be explained by the relatively low number of experienced CE practitioners, the maturity of HPLC in the pharmaceutical industry and some intrinsic limitations of the technique. The objective of this review is to focus our attention on recent developments of this technique in three different drug discovery areas: bioassays, drug-plasma interactions and drug metabolism studies. These developments were based on two important abilities of CE: the capacity to measure non-covalent interactions in solution and the ability to use a portion of the capillary as a reactor while the rest of the capillary is used for the separation of the product of the reaction. [less ▲]

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See detailSingle and dual cyclodextrins systems for the enantiomeric and diastereoisomeric separations of structurally related dihydropyridone analogues.
Delplanques, Thibaut; Boulahjar, Rajaa; Charton, Julie et al

in Electrophoresis (2017)

Cyclodextrin capillary electrophoresis methods (CD-CZE) were developed for complete enantiomeric and diastereoisomeric separations of a series of ten dihydropyridone analogues, of which eight were neutral ... [more ▼]

Cyclodextrin capillary electrophoresis methods (CD-CZE) were developed for complete enantiomeric and diastereoisomeric separations of a series of ten dihydropyridone analogues, of which eight were neutral, one was anionic and one was cationic. Ten different systems comprising one or two cyclodextrins were found to successfully separate the isomers thanks to a screening approach. Among the tested cyclodextrins, HS-gamma-CD, either in a single or in a dual system, in a phosphate buffer using capillaries dynamically coated with polyethylene oxide (PEO), and SBE-beta-CD, either in a single or in a dual system, in a borate buffer using uncoated capillaries, were the most selective selectors. The effects of different parameters such as the nature and concentration of the cyclodextrins, nature and concentration of the buffer, and voltage were examined. The precision and limits of detection and quantification were evaluated for the optimized methods. This article is protected by copyright. All rights reserved. [less ▲]

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See detailStudy of virus-like particles of human papillomavirus in capillary electrophoresis
Bettonville, Virginie ULiege; Nicol, Jérôme; Furst, Tania et al

Poster (2017)

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See detailRIP3 antagonizes a TSC2-mediated pro-survival pathway in glioblastoma cell death.
Fettweis, Grégory ULiege; Di Valentin, Emmanuel ULiege; L'homme, Laurent et al

in Biochimica et Biophysica Acta (2017)

Glioblastomas are the deadliest type of brain cancer and are frequently associated with poor prognosis and a high degree of recurrence despite removal by surgical resection and treatment by chemo- and ... [more ▼]

Glioblastomas are the deadliest type of brain cancer and are frequently associated with poor prognosis and a high degree of recurrence despite removal by surgical resection and treatment by chemo- and radio-therapy. Photodynamic therapy (PDT) is a treatment well known to induce mainly necrotic and apoptotic cell death in solid tumors. 5-Aminolevulinic acid (5-ALA)-based PDT was recently shown to sensitize human glioblastoma cells (LN-18) to a RIP3 (Receptor Interacting Protein 3)-dependent cell death which is counter-acted by activation of autophagy. These promising results led us to investigate the pathways involved in cell death and survival mechanisms occurring in glioblastoma following PDT. In the present study, we describe a new TSC2 (Tuberous Sclerosis 2)-dependent survival pathway implicating MK2 (MAPKAPK2) kinase and 14-3-3 proteins which conducts to the activation of a pro-survival autophagy. Moreover, we characterized a new RIP3/TSC2 complex where RIP3 is suggested to promote cell death by targeting TSC2-dependent survival pathway. These results highlight (i) a new role of TSC2 to protect glioblastoma against PDT-induced cell death and (ii) TSC2 and 14-3-3 as new RIP3 partners. [less ▲]

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