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28 results on '"Aurélie Fildier"'

1. Validation of the Chemical and Biological Steps Required Implementing an Advanced Multi-Omics Approach for Assessing the Fate and Impact of Contaminants in Lagoon Sediments

Author

Anouar Mejait, Aurélie Fildier, Barbara Giroud, Gaëlle Daniele, Laure Wiest, Delphine Raviglione, Jules Kotarba, Eve Toulza, Triana Ramirez, Alexia Lanseman, Camille Clerissi, Emmanuelle Vulliet, Christophe Calvayrac, and Marie-Virginie Salvia

Subjects
contaminants, fate, impact, lagoons, metabolomics, metabarcoding, Microbiology, QR1-502
Abstract

The increasing use of chemicals requires a better understanding of their presence and dynamics in the environment, as well as their impact on ecosystems. The aim of this study was to validate the first steps of an innovative multi-omics approach based on metabolomics and 16S metabarcoding data for analyses of the fate and impact of contaminants in Mediterranean lagoons. Semi-targeted analytical procedures for water and sediment matrices were implemented to assess chemical contamination of the lagoon: forty-six compounds were detected, 28 of which could be quantified in water (between 0.09 and 47.4 ng/L) and sediment (between 0.008 and 26.3 ng/g) samples using the UHPLC-MS/MS instrument. In addition, a non-targeted approach (UHPLC-HRMS) using four different sample preparation protocols based on solid/liquid extractions or an automated pressurized fluid extraction system (EDGE®) was carried out to determine the protocol with the best metabolome coverage, efficiency and reproducibility. Solid/liquid extraction using the solvent mixture acetonitrile/methanol (50/50) was evaluated as the best protocol. Microbial diversity in lagoon sediment was also measured after DNA extraction using five commercial extraction kits. Our study showed that the DNeasy PowerSoil Pro Qiagen kit (Promega, USA) was the most suitable for assessing microbial diversity in fresh sediment.

Published
2024
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2. Inter-laboratory mass spectrometry dataset based on passive sampling of drinking water for non-target analysis

Author

Bastian Schulze, Denice van Herwerden, Ian Allan, Lubertus Bijlsma, Nestor Etxebarria, Martin Hansen, Sylvain Merel, Branislav Vrana, Reza Aalizadeh, Bernard Bajema, Florian Dubocq, Gianluca Coppola, Aurélie Fildier, Pavla Fialová, Emil Frøkjær, Roman Grabic, Pablo Gago-Ferrero, Thorsten Gravert, Juliane Hollender, Nina Huynh, Griet Jacobs, Tim Jonkers, Sarit Kaserzon, Marja Lamoree, Julien Le Roux, Teresa Mairinger, Christelle Margoum, Giuseppe Mascolo, Emmanuelle Mebold, Frank Menger, Cécile Miège, Jeroen Meijer, Régis Moilleron, Sapia Murgolo, Massimo Peruzzo, Martijn Pijnappels, Malcolm Reid, Claudio Roscioli, Coralie Soulier, Sara Valsecchi, Nikolaos Thomaidis, Emmanuelle Vulliet, Robert Young, and Saer Samanipour

Subjects
Science
Abstract

Measurement(s) chemical • drinking water Technology Type(s) high resolution mass spectrometry • non-target analysis • Interlaboratory Factor Type(s) method Sample Characteristic - Environment laboratory environment Machine-accessible metadata file describing the reported data: https://doi.org/10.6084/m9.figshare.15028665

Published
2021
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3. An optimized LC-HRMS untargeted metabolomics workflow for multi-matrices investigations in the three-spined stickleback.

Author

Emmanuelle Lebeau-Roche, Gaëlle Daniele, Aurélie Fildier, Cyril Turies, Odile Dedourge-Geffard, Jean-Marc Porcher, Alain Geffard, and Emmanuelle Vulliet

Subjects
Medicine, Science
Abstract

Environmental metabolomics has become a growing research field to understand biological and biochemical perturbations of organisms in response to various abiotic or biotic stresses. It focuses on the comprehensive and systematic analysis of a biologic system's metabolome. This allows the recognition of biochemical pathways impacted by a stressor, and the identification of some metabolites as biomarkers of potential perturbations occurring in a body. In this work, we describe the development and optimization of a complete reliable methodology based on liquid chromatography coupled to high resolution mass spectrometry (LC-HRMS) for untargeted metabolomics studies within a fish model species, the three-spined stickleback (Gasterosteus aculeatus). We evaluated the differences and also the complementarities between four different matrices (brain, gills, liver and whole fish) to obtain metabolome information. To this end, we optimized and compared sample preparation and the analytical method, since the type and number of metabolites detected in any matrix are closely related to these latter. For the sample preparation, a solid-liquid extraction was performed on a low quantity of whole fish, liver, brain, or gills tissues using combinations of methanol/water/heptane. Based on the numbers of features observed in LC-HRMS and on the responses of analytical standards representative of different metabolites groups (amino acids, sugars…), we discuss the influence of the nature, volume, and ratio of extraction solvents, the sample weight, and the reconstitution solvent. Moreover, the analytical conditions (LC columns, pH and additive of mobile phases and ionization modes) were also optimized so as to ensure the maximum metabolome coverages. Thus, two complementary chromatographic procedures were combined in order to cover a broader range of metabolites: a reversed phase separation (RPLC) on a C18 column followed by detection with positive ionization mode (ESI+) and a hydrophilic interaction chromatography (HILIC) on a zwitterionic column followed by detection with negative ionization mode (ESI-). This work provides information on brain, gills, liver, vs the whole body contribution to the stickleback metabolome. These information would help to guide ecotoxicological and biomonitoring studies.

Published
2021
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4. Phytochemical and Biological Investigation of Two Diplotaxis Species Growing in Tunisia: D. virgata & D. erucoides

Author

Nizar Ben Salah, Hervé Casabianca, Hichem Ben Jannet, Sophie Chenavas, Corinne Sanglar, Aurélie Fildier, and Nabiha Bouzouita

Subjects
D. erucoides, D. virgata, flavonoids, fatty acids, NMR, antioxidant activity, antimicrobial activity, Organic chemistry, QD241-441
Abstract

A phytochemical investigation of Diplotaxis virgata D.C. and D. erucoides (L.) D.C. (Brassicaceae) offered to the isolation of two new flavonoids isorhamnetin-3-O-α-l-glucopyranoside (1) and rhamnetin-3,3ʹ-di-O-β-d-glucopyranoside (2), respectively. Their structures have been elucidated from the extended spectroscopic methods, including 1D- and 2D-NMR, UV and mass spectrometry analysis and by comparison with literature data. The fatty acid composition of the hexane extracts of the two species was also investigated by using GC-MS. The antioxidant activity of ethanol, ethyl acetate, n-butanol extracts and the isolated compounds from the two species was evaluated using DPPH and ABTS+ scavenging assays. All the tested samples showed an efficient radical scavenging ability, with IC50 values ranging from 16–40 µg/mL for the DPPH and from 17–44 µg/mL for the ABTS+ assays. In addition, the antibacterial activity of the prepared extracts and compounds 1 and 2, determined by well diffusion agar method against two Gram positive and five Gram negative bacteria, was evaluated and the results showed significant effects against all strains used.

Published
2015
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5. Doping control using high and ultra-high resolution mass spectrometry based non-targeted metabolomics-a case study of salbutamol and budesonide abuse.

Author

Agneta Kiss, Marianna Lucio, Aurélie Fildier, Corinne Buisson, Philippe Schmitt-Kopplin, and Cécile Cren-Olivé

Subjects
Medicine, Science
Abstract

We have detected differences in metabolite levels between doped athletes, clean athletes, and volunteers (non athletes). This outcome is obtained by comparing results of measurements from two analytical platforms: UHPLC-QTOF/MS and FT-ICR/MS. Twenty-seven urine samples tested positive for glucocorticoids or beta-2-agonists and twenty samples coming from volunteers and clean athletes were analyzed with the two different mass spectrometry approaches using both positive and negative electrospray ionization modes. Urine is a highly complex matrix containing thousands of metabolites having different chemical properties and a high dynamic range. We used multivariate analysis techniques to unravel this huge data set. Thus, the several groups we created were studied by Principal Components Analysis (PCA) and Partial Least Square regression (PLS-DA and OPLS) in the search of discriminating m/z values. The selected variables were annotated and placed on pathway by using MassTRIX.

Published
2013
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7. La spectrométrie de masse haute résolution pour la recherche de micropolluants organiques dans l’environnement

Author

Guillaume Couturier, Virginie Boiteux, M. Esperanza, Anne Piram, Caroline Gardia-Parege, Emilie Caupos, Patrick Candido, C. Soulier, Marie-Hélène Devier, Xavier Dauchy, Christelle Margoum, Gaëla Leroy, N. Noyon, J. Le Roux, Mathilde Chachignon, Sophie Lissalde, Robin Guibal, François Lestremau, Emmanuelle Vulliet, and Aurélie Fildier

Subjects
Fluid Flow and Transfer Processes, 13. Climate action, 0207 environmental engineering, Ocean Engineering, 02 engineering and technology, 010501 environmental sciences, 020701 environmental engineering, General Agricultural and Biological Sciences, 01 natural sciences, 0105 earth and related environmental sciences, Water Science and Technology
Abstract

L’analyse non ciblée connaît une forte période de croissance dans le domaine de l’analyse environnementale, car elle ouvre le champ des investigations de la qualité des milieux à un très grand nombre de composés. Cet article consiste en un retour d’expérience de 12 laboratoires français sur les pratiques et les précautions à considérer lors de la réalisation d’analyses non ciblées, en particulier pour la recherche de composés suspects dans les échantillons issus des milieux aquatiques. En effet, si cette technique apporte des informations nouvelles et très prometteuses, elle n’en reste pas moins une technique complexe qu’il convient d’utiliser avec de nombreuses précautions pour assurer des résultats de qualité. La réflexion commune entreprise dans le groupe de laboratoires, a permis de synthétiser des informations techniques afin de présenter les enjeux de cette méthodologie d’intérêt majeur en analyse environnementale de façon simple et accessible aux laboratoires, demandeurs d’analyse ou toute personne intéressée par ce type d’approche. Les verrous liés à la spécificité des analyses non ciblées, au développement de méthodes et au rendu de résultats ont été développés pour fournir des clés de compréhension pour les laboratoires et les utilisateurs de résultats. Ce travail s’attache ainsi à être un guide de découverte de la technique pour les personnes désireuses de voir ce que peut apporter l’analyse non ciblée, mais également un guide de bonnes pratiques pour celles et ceux qui acquièrent ou qui analysent des données issues de ces techniques.

Published
2021

8. Inter-laboratory mass spectrometry dataset based on passive sampling of drinking water for non-target analysis

Author

Claudio Roscioli, C. Soulier, Marja H. Lamoree, Bernard Bajema, Griet Jacobs, R. Moilleron, Aurélie Fildier, Gianluca Coppola, Pavla Fialová, Julien Le Roux, Cecile Miege, Bastian Schulze, Lubertus Bijlsma, Martijn Pijnappels, Tim Jonkers, Saer Samanipour, Sapia Murgolo, Roman Grabic, Frank Menger, Robert B. Young, Emmanuelle Mebold, Emmanuelle Vulliet, Massimo Peruzzo, Juliane Hollender, Teresa Mairinger, Christelle Margoum, Sylvain Merel, Sarit Kaserzon, Giuseppe Mascolo, Nikolaos S. Thomaidis, Branislav Vrana, Pablo Gago-Ferrero, Ian Allan, Reza Aalizadeh, Denice van Herwerden, Jeroen Meijer, Sara Valsecchi, Nestor Etxebarria, Malcolm J. Reid, Thorsten Klaus Otto Gravert, Florian Dubocq, Martin Ejnar Hansen, Nina Huynh, Emil Frøkjær, HIMS Other Research (FNWI), University of Queensland [Brisbane], University of Amsterdam [Amsterdam] (UvA), Norwegian Institute for Water Research (NIVA), Universitat Jaume I, University of the Basque Country/Euskal Herriko Unibertsitatea (UPV/EHU), Aarhus University [Aarhus], Riverly (Riverly), Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Research Centre for Toxic Compounds in the Environment [Brno] (RECETOX / MUNI), Faculty of Science [Brno] (SCI / MUNI), Masaryk University [Brno] (MUNI)-Masaryk University [Brno] (MUNI), National and Kapodistrian University of Athens (NKUA), Vitens NV, Örebro University, Eurolab Srl, TRACES - Technologie et Recherche en Analyse Chimique pour l'Environnement et la Santé, Institut des Sciences Analytiques (ISA), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), UNIVERSITY OF SOUTH BOHEMIA CESKE BUDEJOVICE CZE, Partenaires IRSTEA, Institut national de recherche en sciences et technologies pour l'environnement et l'agriculture (IRSTEA)-Institut national de recherche en sciences et technologies pour l'environnement et l'agriculture (IRSTEA), Instituto Catalán de Investigación del Agua - ICRA (SPAIN) (ICRA), Swiss Federal Insitute of Aquatic Science and Technology [Dübendorf] (EAWAG), École des Ponts ParisTech (ENPC), Flemish Institute for Technological Research (VITO), Vrije Universiteit Amsterdam [Amsterdam] (VU), Laboratoire Eau Environnement et Systèmes Urbains (LEESU), École des Ponts ParisTech (ENPC)-Université Paris-Est Créteil Val-de-Marne - Paris 12 (UPEC UP12), Universität für Bodenkultur Wien = University of Natural Resources and Life [Vienne, Autriche] (BOKU), Istituto di Ricerca Sulle Acque, Università degli studi di Bari Aldo Moro = University of Bari Aldo Moro (UNIBA), Enveloppes fluides : de la ville à l'exobiologie (EFLUVE (UMS_3563)), Institut national des sciences de l'Univers (INSU - CNRS)-École des Ponts ParisTech (ENPC)-Université Paris-Est Créteil Val-de-Marne - Paris 12 (UPEC UP12)-Centre National de la Recherche Scientifique (CNRS)-Université Paris Cité (UPCité), Swedish University of Agricultural Sciences (SLU), Rijkswaterstaat [Delft], INSTITUTO DI RICERCA SULLE ACQUE ITA, Bureau de Recherches Géologiques et Minières (BRGM) (BRGM), Colorado State University [Fort Collins] (CSU), NORMAN network, Danish Environmental Protection Agency : MST-667-00207, Aarhus University Research Foundation : AUFF-T-2017-FLS-7-4, University of the Basque Country [Bizkaia] (UPV/EHU), Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), University of Natural Resources and Life Sciences (BOKU), Università degli studi di Bari Aldo Moro (UNIBA), Institut national des sciences de l'Univers (INSU - CNRS)-École des Ponts ParisTech (ENPC)-Université Paris-Est Créteil Val-de-Marne - Paris 12 (UPEC UP12)-Centre National de la Recherche Scientifique (CNRS)-Université de Paris (UP), E&H: Environmental Chemistry and Toxicology, and AIMMS

Subjects
Statistics and Probability, Data Descriptor, Computer science, Science, 010501 environmental sciences, Library and Information Sciences, computer.software_genre, 01 natural sciences, Education, Workflow, Set (abstract data type), spectrometry, Non target, Resource (project management), [CHIM.ANAL]Chemical Sciences/Analytical chemistry, 0105 earth and related environmental sciences, Mass spectrometry, [SDE.IE]Environmental Sciences/Environmental Engineering, Drinking Water, 010401 analytical chemistry, Quality control, Environmental monitoring, 6. Clean water, 0104 chemical sciences, Computer Science Applications, Benchmarking, Benchmark (computing), Computer-aided, mass, Data mining, COLLABORATIVE TRIAL, POLLUTANTS, IDENTIFICATION, CONTAMINANTS, ENVIRONMENT, MIXTURES, PLATFORM, SUSPECT, Statistics, Probability and Uncertainty, SDG 6 - Clean Water and Sanitation, Laboratories, computer, Algorithms, Passive sampling, Information Systems
Abstract

Non-target analysis (NTA) employing high-resolution mass spectrometry is a commonly applied approach for the detection of novel chemicals of emerging concern in complex environmental samples. NTA typically results in large and information-rich datasets that require computer aided (ideally automated) strategies for their processing and interpretation. Such strategies do however raise the challenge of reproducibility between and within different processing workflows. An effective strategy to mitigate such problems is the implementation of inter-laboratory studies (ILS) with the aim to evaluate different workflows and agree on harmonized/standardized quality control procedures. Here we present the data generated during such an ILS. This study was organized through the Norman Network and included 21 participants from 11 countries. A set of samples based on the passive sampling of drinking water pre and post treatment was shipped to all the participating laboratories for analysis, using one pre-defined method and one locally (i.e. in-house) developed method. The data generated represents a valuable resource (i.e. benchmark) for future developments of algorithms and workflows for NTA experiments., Measurement(s)chemical • drinking waterTechnology Type(s)high resolution mass spectrometry • non-target analysis • InterlaboratoryFactor Type(s)methodSample Characteristic - Environmentlaboratory environment Machine-accessible metadata file describing the reported data: 10.6084/m9.figshare.15028665

Published
2021

9. Ecotoxicological risk assessment of contaminants of emerging concern identified by 'suspect screening' from urban wastewater treatment plant effluents at a territorial scale

Author

Elisabeth Sibeud, Matthieu Hervé, Christine Libert, Myriam Hammada, Yves Perrodin, Aurélie Fildier, Antoine Gosset, Philippe Polomé, Emmanuelle Vulliet, Laure Wiest, Barbara Giroud, Groupe d'analyse et de théorie économique (GATE Lyon Saint-Étienne), École normale supérieure - Lyon (ENS Lyon)-Université Lumière - Lyon 2 (UL2)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Université Jean Monnet [Saint-Étienne] (UJM)-Centre National de la Recherche Scientifique (CNRS), Équipe 5 - Impact des Aménagements et des Polluants sur les HYdrosystèmes (IAPHY), Laboratoire d'Ecologie des Hydrosystèmes Naturels et Anthropisés (LEHNA), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-École Nationale des Travaux Publics de l'État (ENTPE)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-École Nationale des Travaux Publics de l'État (ENTPE)-Centre National de la Recherche Scientifique (CNRS), TRACES - Technologie et Recherche en Analyse Chimique pour l'Environnement et la Santé, Institut des Sciences Analytiques (ISA), Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), This work was supported by the Lyon Urban School, through a funding grant from the French National Research Agency (Programme Investissements d'Avenir (ANR-17-CONV-0004)). This study also received scientifical, technical, and financial support from the French Ministry of Ecology (through the ENTPE), the Greater Lyon and the University Lyon 2.This work was performed within the framework of the EUR H2O'Lyon (ANR-17-EURE-0018) of Université de Lyon (UdL), within the program 'Investissements d'Avenir' operated by the French National Research Agency (ANR)., Groupe d'Analyse et de Théorie Economique Lyon - Saint-Etienne (GATE Lyon Saint-Étienne), École normale supérieure de Lyon (ENS de Lyon)-Université Lumière - Lyon 2 (UL2)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Université Jean Monnet - Saint-Étienne (UJM)-Centre National de la Recherche Scientifique (CNRS), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), ANR-17-EURE-0018,H2O'LYON,School of Integrated Watershed Sciences(2017), ANR-17-CONV-0004,LUS,Lyon Urban School(2017), Centre National de la Recherche Scientifique (CNRS)-Université de Lyon-Université Jean Monnet [Saint-Étienne] (UJM)-Université Claude Bernard Lyon 1 (UCBL), and Université de Lyon-Université Lumière - Lyon 2 (UL2)-École normale supérieure - Lyon (ENS Lyon)

Subjects
Environmental Engineering, 010504 meteorology & atmospheric sciences, 010501 environmental sciences, Wastewater, 01 natural sciences, Risk Assessment, Waste Disposal, Fluid, Water Purification, Environmental health, Environmental Chemistry, Predicted no-effect concentration, Waste Management and Disposal, Effluent, 0105 earth and related environmental sciences, Cocktail effect, Scale (chemistry), Ecotoxicological risk, Urban wastewater, Contaminants of Emerging Concern, Pesticide, Contamination, Pollution, 6. Clean water, 13. Climate action, Ecotoxicological risk assessment, Pharmaceutical, Environmental science, Sewage treatment, [SDV.TOX.ECO]Life Sciences [q-bio]/Toxicology/Ecotoxicology, [SDE.BE]Environmental Sciences/Biodiversity and Ecology, Risk assessment, Water Pollutants, Chemical, Environmental Monitoring, Suspect-screening
Abstract

Urban wastewater treatment plants (WWTP) are a major vector of highly ecotoxic contaminants of emerging concern (CECs) for urban and sub-urban streams. Ecotoxicological risk assessments (ERAs) provide essential information to public environmental authorities. Nevertheless, ERAs are mainly performed at very local scale (one or few WWTPs) and on pre-selected list of CECs. To cope with these limits, the present study aims to develop a territorial-scale ERA on CECs previously identified by a "suspect screening" analytical approach (LC-QToF-MS) and quantified in the effluents of 10 WWTPs of a highly urbanized territory during three periods of the year. Among CECs, this work focused on pharmaceutical residue and pesticides. ERA was conducted following two complementary methods: (1) a single substance approach, based on the calculation for each CEC of risk quotients (RQs) by the ratio of Predicted Environmental Concentration (PEC) and Predicted No Effect Concentration (PNEC), and (2) mixture risk assessment ("cocktail effect") based on a concentration addition model (CA), summing individual RQs. Chemical results led to an ERA for 41 CEC (37 pharmaceuticals and 4 pesticides) detected in treated effluents. Single substance ERA identified 19 CECs implicated in at least one significant risk for streams, with significant risks for DEET, diclofenac, lidocaine, atenolol, terbutryn, atorvastatin, methocarbamol, and venlafaxine (RQs reaching 39.84, 62.10, 125.58, 179.11, 348.24, 509.27, 1509.71 and 3097.37, respectively). Mixture ERA allowed the identification of a risk (RQmix > 1) for 9 of the 10 WWTPs studied. It was also remarked that CECs leading individually to a negligible risk could imply a significant risk in a mixture. Finally, the territorial ERA showed a diversity of risk situations, with the highest concerns for 3 WWTPs: the 2 biggest of the territory discharging into a large French river, the Rhone, and for the smallest WWTP that releases into a small intermittent stream.

Published
2021

10. In Vivo Characterization of the Toxicological Properties of DPhP, One of the Main Degradation Products of Aryl Phosphate Esters

Author

Béatrice Fervers, Julie Deverchère, Lea Payen-Gay, Jessica Garcia, Thierry Granjon, Samia Ruby, Jesús Marín-Sáez, Arnaud Vigneron, Claire Bardel-Danjean, Emmanuelle Vulliet, Myriam Abdallah, Aurélie Fildier, Alain Puisieux, Barbara Giroud, Audrey Buleté, Sébastien Ibanez, Loic Spinner, Centre de Recherche en Cancérologie de Lyon (UNICANCER/CRCL), Centre Léon Bérard [Lyon]-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS), Research Centre for Agricultural and Food Biotechnology (BITAL), University of Almería, TRACES - Technologie et Recherche en Analyse Chimique pour l'Environnement et la Santé, Institut des Sciences Analytiques (ISA), Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Biochemistry, pharmacotoxicology, and molecular biology department, Hospices Civils de Lyon, centre hospitalier Lyon Sud, Chimie Organique 2-Glycochimie (CO2GLYCO), Institut de Chimie et Biochimie Moléculaires et Supramoléculaires (ICBMS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Institut de Chimie du CNRS (INC)-École Supérieure Chimie Physique Électronique de Lyon-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Institut de Chimie du CNRS (INC)-École Supérieure Chimie Physique Électronique de Lyon-Centre National de la Recherche Scientifique (CNRS), Départment of biostatistics, Hospices Civils de Lyon, Laboratoire de Biométrie et Biologie Evolutive - UMR 5558 (LBBE), Université de Lyon-Université de Lyon-Institut National de Recherche en Informatique et en Automatique (Inria)-VetAgro Sup - Institut national d'enseignement supérieur et de recherche en alimentation, santé animale, sciences agronomiques et de l'environnement (VAS)-Centre National de la Recherche Scientifique (CNRS), Ligue contre le cancer (comité du Rhône), Association pour la Recherche contre le Cancer (projets n°SFI20121205395, PJA20141201758, PJA20171206303), Université de Lyon (Projet Bonus Qualité Recherche), Bussy, Agnès, Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université de Lyon-Université de Lyon-École Supérieure de Chimie Physique Électronique de Lyon (CPE)-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), and Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Health, Toxicology and Mutagenesis, [SDV]Life Sciences [q-bio], Pharmacology, 010501 environmental sciences, 01 natural sciences, 03 medical and health sciences, chemistry.chemical_compound, 0302 clinical medicine, Downregulation and upregulation, In vivo, Lipid droplet, Ketogenesis, [CHIM] Chemical Sciences, Organic chemistry, [CHIM]Chemical Sciences, 030212 general & internal medicine, ComputingMilieux_MISCELLANEOUS, 030304 developmental biology, 0105 earth and related environmental sciences, 0303 health sciences, Fatty acid metabolism, Catabolism, Aryl, Research, technology, industry, and agriculture, Public Health, Environmental and Occupational Health, Phosphate, [SDV] Life Sciences [q-bio], chemistry, 13. Climate action, DPHP, Degradation (geology)
Abstract

BackgroundAryl phosphate esters (APEs), a main class of organophosphorus ester molecules, are widely used and commonly present in the environment. Health hazards associated with these compounds remain largely unknown and the effects of diphenyl phosphate (DPhP), one of their most frequent derivatives in human samples, are poorly characterised.ObjectiveOur aim was to investigate whether DPhP per se may represent a more relevant marker of exposure to APEs and determine its potential deleterious biological effects in chronically exposed mice.MethodsConventional animals (FVB mice) were acutely (intravenous or oral gavage) or chronically (0.1 mg.mL-1, 1 mg.mL-1, 10 mg.mL-1 in drink water) exposed to relevant doses of DPhP or triphenyl phosphate (TPhP), one of its main precursors in the environment. Both molecules were measured in blood and other relevant tissues by liquid chromatography-mass spectrometry (LC-MS). Biological effects of chronic DPhP exposure were addressed through liver multi-omics analysis combining mRNA extraction and sequencing to high resolution LC-MS to determine the corresponding metabolic profile. Deep statistical exploration was performed to extract correlated information, guiding further physiological analyses (immunohistochemistry (IHC) and animal growth measurement).ResultsAcute and chronic exposure to DPhP led to significant levels of this molecule in blood and other tissues, an effect missing with TPhP. Multi-omics analysis confirmed the existence of biological effects of DPhP, even at a very low dose of 0.1 mg.mL-1 in drinking water. Chemical structural homology and pathway mapping demonstrated a clear reduction of the fatty-acid catabolic processes centred on acylcarnitine and mitochondrial β-oxidation. Interestingly, mRNA expression confirmed and extended these observations by demonstrating at all tested doses the overall repression of genes involved in lipid catabolic processes and regulated by PPARα, a master regulator of β-oxidation and its associated ketogenesis. IHC analysis confirmed the alteration of these pathways by showing a specific downregulation of Hmgcs2, a kernel target gene of PPARα, at all doses tested, and surprisingly, a strong reduction of the lipid droplet content only at the highest dose. Overall, DPhP absorption led to weight loss, which was significant using the highest dose.ConclusionsOur results suggest that in mice, the effects of chronic exposure to DPhP, even at a low dose, are not negligible. Fatty acid metabolism in the liver in particular is essential for controlling fast and feast periods with adverse consequences on the overall physiology. Therefore, the impact of DPhP on circulating fat, cardiovascular and metabolic disease incidence deserves, in light of our results, further investigations.

Published
2020

11. NORMAN guidance on suspect and non-target screening in environmental monitoring

Author

Juliane Hollender, Emma L. Schymanski, Lutz Ahrens, Nikiforos Alygizakis, Frederic Béen, Lubertus Bijlsma, Andrea M. Brunner, Alberto Celma, Aurelie Fildier, Qiuguo Fu, Pablo Gago-Ferrero, Ruben Gil-Solsona, Peter Haglund, Martin Hansen, Sarit Kaserzon, Anneli Kruve, Marja Lamoree, Christelle Margoum, Jeroen Meijer, Sylvain Merel, Cassandra Rauert, Pawel Rostkowski, Saer Samanipour, Bastian Schulze, Tobias Schulze, Randolph R. Singh, Jaroslav Slobodnik, Teresa Steininger-Mairinger, Nikolaos S. Thomaidis, Anne Togola, Katrin Vorkamp, Emmanuelle Vulliet, Linyan Zhu, and Martin Krauss

Subjects
Non-target screening, Suspect screening, High-resolution mass spectrometry, Sample preparation, Organic contaminants, Chromatography, Environmental sciences, GE1-350, Environmental law, K3581-3598
Abstract

Abstract Increasing production and use of chemicals and awareness of their impact on ecosystems and humans has led to large interest for broadening the knowledge on the chemical status of the environment and human health by suspect and non-target screening (NTS). To facilitate effective implementation of NTS in scientific, commercial and governmental laboratories, as well as acceptance by managers, regulators and risk assessors, more harmonisation in NTS is required. To address this, NORMAN Association members involved in NTS activities have prepared this guidance document, based on the current state of knowledge. The document is intended to provide guidance on performing high quality NTS studies and data interpretation while increasing awareness of the promise but also pitfalls and challenges associated with these techniques. Guidance is provided for all steps; from sampling and sample preparation to analysis by chromatography (liquid and gas—LC and GC) coupled via various ionisation techniques to high-resolution tandem mass spectrometry (HRMS/MS), through to data evaluation and reporting in the context of NTS. Although most experience within the NORMAN network still involves water analysis of polar compounds using LC–HRMS/MS, other matrices (sediment, soil, biota, dust, air) and instrumentation (GC, ion mobility) are covered, reflecting the rapid development and extension of the field. Due to the ongoing developments, the different questions addressed with NTS and manifold techniques in use, NORMAN members feel that no standard operation process can be provided at this stage. However, appropriate analytical methods, data processing techniques and databases commonly compiled in NTS workflows are introduced, their limitations are discussed and recommendations for different cases are provided. Proper quality assurance, quantification without reference standards and reporting results with clear confidence of identification assignment complete the guidance together with a glossary of definitions. The NORMAN community greatly supports the sharing of experiences and data via open science and hopes that this guideline supports this effort.

Published
2023
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12. Untargeted analysis of nanoLC-HRMS data by ANOVA-PCA to highlight metabolites in Gammarus fossarum after in vivo exposure to pharmaceuticals

Author

Aurélie Fildier, Claire Bordes, Emmanuelle Vulliet, Audrey Buleté, Jeanne Garric, Christelle Bonnefoy, Chemometrics and Theoretical Chemistry - Chimiométrie et chimie théorique, Institut des Sciences Analytiques (ISA), École normale supérieure - Lyon (ENS Lyon)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-École normale supérieure - Lyon (ENS Lyon)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), TRACES - Technologie et Recherche en Analyse Chimique pour l'Environnement et la Santé, RiverLy (UR Riverly), Institut national de recherche en sciences et technologies pour l'environnement et l'agriculture (IRSTEA), French EC2CO program INSU-CNRS, Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), and Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL)

Subjects
Male, 02 engineering and technology, Mass spectrometry, 01 natural sciences, River water, Mass Spectrometry, Analytical Chemistry, Chemometrics, Metabolomics, In vivo, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Animals, Humans, Nanotechnology, [CHIM]Chemical Sciences, Amphipoda, ComputingMilieux_MISCELLANEOUS, Principal Component Analysis, Chromatography, Oxazepam, Chemistry, 010401 analytical chemistry, Factorial experiment, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Carbamazepine, Gammarus fossarum, [SDE]Environmental Sciences, Female, Analysis of variance, 0210 nano-technology, Chromatography, Liquid
Abstract

In Western Europe, river water quality can be assessed using sentinel species such as the amphipod Gammarus fossarum. In this work of environmental metabolomics, the objective was to develop suitable chemometrics methods, using a limited number of individuals, to assess the modification of the metabolism of G. fossarum exposed to two human pharmaceuticals. Males and females gammarids were exposed to a mixture of the anxiolytic oxazepam and the antiepileptic carbamazepine (1000 ng L−1) for 14 days under laboratory conditions according to a full factorial design 2² (repeated 5 times). They were analyzed at the single individual scale using a method including a μQuEChERS type extraction followed by a nanoliquid chromatography analysis coupled to high-resolution mass spectrometry. The molecular fingerprints obtained were investigated using XCMS. Several corrections of experimental drifts (by using lock mass and Quality Control samples) were tested prior to using APCA + method for the exploitation of the unbalanced designed data. Signal reproducibility was greatly improved by the lock mass normalisation. From the experimental design, a significant effect of both experimental factors “exposure to the mixture” and “gammarid gender” on the signals measured were highlighted by APCA+. Finally, the results obtained made it possible to identify variables responsible for each of the factor effects.

Published
2019

13. Use of passive sampling and high resolution mass spectrometry using a suspect screening approach to characterise emerging pollutants in contaminated groundwater and runoff

Author

Emmanuelle Vulliet, Florian Mermillod-Blondin, Lucie Pinasseau, Aurélie Fildier, Gary R. Fones, Graham A. Mills, Laurence Volatier, Laure Wiest, TRACES - Technologie et Recherche en Analyse Chimique pour l'Environnement et la Santé, Institut des Sciences Analytiques (ISA), Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Laboratoire d'Ecologie des Hydrosystèmes Naturels et Anthropisés (LEHNA), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-École Nationale des Travaux Publics de l'État (ENTPE)-Centre National de la Recherche Scientifique (CNRS), School of Earth and Environmental Sciences [Portsmouth], University of Portsmouth, School of Pharmacy and Biomedical Sciences, École normale supérieure - Lyon (ENS Lyon)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-École normale supérieure - Lyon (ENS Lyon)-Université Claude Bernard Lyon 1 (UCBL), Centre National de la Recherche Scientifique (CNRS)-Institut National de la Recherche Agronomique (INRA)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-École Nationale des Travaux Publics de l'État (ENTPE), Centre National de la Recherche Scientifique (CNRS)-Université de Lyon-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-École normale supérieure - Lyon (ENS Lyon)-Centre National de la Recherche Scientifique (CNRS)-Université de Lyon-Université Claude Bernard Lyon 1 (UCBL), and Université de Lyon-École normale supérieure - Lyon (ENS Lyon)

Subjects
Pollution, Environmental Engineering, 010504 meteorology & atmospheric sciences, media_common.quotation_subject, Stormwater, 010501 environmental sciences, 01 natural sciences, Stormwater runoff Stormwater infiltration basins Passive sampling High resolution mass spectrometry Polar pharmaceuticals and pesticides Suspect screening, Groundwater pollution, Environmental Chemistry, [CHIM]Chemical Sciences, Waste Management and Disposal, 0105 earth and related environmental sciences, media_common, Pollutant, geography, geography.geographical_feature_category, Environmental engineering, Contamination, 6. Clean water, Environmental Management, 13. Climate action, Environmental science, [SDE.BE]Environmental Sciences/Biodiversity and Ecology, Surface runoff, Groundwater, Water well
Abstract

International audience; Groundwater systems are being increasingly used to provide potable and other water supplies. Due to human activities, a range of organic pollutants is often detected in groundwater. One source of groundwater contamination is via stormwater infiltration basins, however, there is little information on the types of compounds present in these collection systems and their influence on the underlying groundwater. We developed an analytical strategy based on the use of passive sampling combined with liquid chromatography/high resolution quadrupole-time-of-flight mass spectrometry for screening for the presence of pesticide and pharmaceutical compounds in groundwater and stormwater runoff. Empore™ disk-based passive samplers (SDB-RPS and SDB-XC sorbents) were exposed, using for the first time a new specially designed deployment rig, for 10 days during a rainfall event in five different stormwater infiltration systems around Lyon, France. Stormwater runoff and groundwater (via a well, upstream and downstream of each basin) was sampled. Exposed Empore™ disks were solvent extracted (acetone and methanol) and the extracts analysed using a specific suspect compound screening workflow. High resolution mass spectrometry coupled with a suspect screening approach was found to be a useful tool as it allows a more comprehensive analysis than with targeted screening whilst being less time consuming than non-targeted screening. Using this analytical approach, 101 suspect compounds were tentatively identified, with 40 of this set being subsequently confirmed. The chemicals detected included fungicides, herbicides, insecticides, indicators of human activity, antibiotics, antiepileptics, antihypertensive and non-steroidal anti-inflammatory drugs as well as their metabolites. Polar pesticides were mainly detected in groundwater and pharmaceuticals were more frequently found in runoff. In terms of detection frequency of the pollutants, groundwater impacted by infiltration was found not to be significantly more contaminated than non-impacted groundwater.

Published
2019

14. Non-target strategies by HRMS to evaluate fluidized micro-grain activated carbon as a tertiary treatment of wastewater

Author

Yves Coquet, Aurélie Fildier, Johnny Gasperi, Audrey Buleté, Vincent Rocher, Emmanuelle Vulliet, Alexandre Bergé, Romain Mailler, Fabrice Nauleau, TRACES - Technologie et Recherche en Analyse Chimique pour l'Environnement et la Santé, Institut des Sciences Analytiques (ISA), Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), SIAAP - Direction du Développement et de la Prospective, SIAAP, laboratoire Eau Environnement et Systèmes Urbains (LEESU), AgroParisTech-École des Ponts ParisTech (ENPC)-Université Paris-Est Créteil Val-de-Marne - Paris 12 (UPEC UP12), SAUR - Direction de la Recherche et Développement, SAUR, Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), and Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Environmental Engineering, Health, Toxicology and Mutagenesis, 0208 environmental biotechnology, 02 engineering and technology, 010501 environmental sciences, Wastewater, 01 natural sciences, Antiviral Agents, Mass Spectrometry, Water Purification, Non target, medicine, Environmental Chemistry, [CHIM]Chemical Sciences, Pesticides, Effluent, Antihypertensive Agents, 0105 earth and related environmental sciences, Analgesics, Chemistry, Public Health, Environmental and Occupational Health, General Medicine, General Chemistry, Pesticide, Contamination, Pulp and paper industry, Pollution, 6. Clean water, Antidepressive Agents, 020801 environmental engineering, Tertiary treatment High-resolution mass spectrometry Refractory compounds Micropollutants μGAC Non target, Pharmaceutical Preparations, Fluidized bed, Charcoal, [SDE]Environmental Sciences, Sewage treatment, Water Pollutants, Chemical, Activated carbon, medicine.drug
Abstract

The authors gratefully acknowledge Céline Briand (SIAAP) for her technical assistance during the sampling campaigns and daily operation of the pilot system.; International audience; Among the release solutions for reducing the discharge of organic and persistent contaminants in the aquatic environment, the use of a tertiary treatment in addition to existing conventional wastewater treatment processes is considered. The use of micro-grain activated carbon in a fluidized bed is a promising technique investigated in this study. The effluents from a large-scale pilot system were analyzed by liquid chromatography coupled with high-resolution mass spectrometry (QToF). Several strategies were deployed, namely molecular fingerprint comparison, suspected and non-target analyses, identification of refractory compounds to treatment, and finally, quantification of identified compounds. The evaluation of the molecular fingerprints provided evidence of the overall effect of the tertiary treatment on the treated wastewater quality. The suspected approach highlighted the presence of 83 pharmaceuticals and pesticides as well as transformation products in the effluents. The non-target approaches also highlighted compounds refractory to tertiary treatment, such as illicit drugs or some pharmaceuticals. The identification and quantification of identified compounds underscored the suitability of micro-grain activated carbon in eliminating many classes of pharmaceuticals with various physicochemical properties, such as anti-hypertensive, analgesic, anti-viral, antidepressant and even various pesticides.

Published
2018

15. Non-targeted investigation of benthic invertebrates ( Chironomus riparius ) exposed to wastewater treatment plant effluents using nanoliquid chromatography coupled to high-resolution mass spectrometry

Author

Jeanne Garric, Aurélie Fildier, Alexandra Berlioz-Barbier, Emmanuelle Vulliet, Audrey Buleté, TRACES - Technologie et Recherche en Analyse Chimique pour l'Environnement et la Santé, Institut des Sciences Analytiques (ISA), Centre National de la Recherche Scientifique (CNRS)-Université de Lyon-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-École normale supérieure - Lyon (ENS Lyon)-Centre National de la Recherche Scientifique (CNRS)-Université de Lyon-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-École normale supérieure - Lyon (ENS Lyon), Milieux aquatiques, écologie et pollutions (UR MALY), Institut national de recherche en sciences et technologies pour l'environnement et l'agriculture (IRSTEA), The authors gratefully acknowledge the Persistent Systems France Company for the development of our home-made annotation software, Bruker Daltonics® for its technical support and the French National Center of Scientific Research (CNRS) and the Rhône-Alpes research group on infrastructures and water (GRAIE) for the thesis funding., Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), and Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)

Subjects
Environmental Engineering, Insecta, Health, Toxicology and Mutagenesis, ved/biology.organism_classification_rank.species, 010501 environmental sciences, Wastewater, Quechers, Mass spectrometry, 01 natural sciences, Chironomidae, Mass Spectrometry, chemistry.chemical_compound, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Metabolome, Environmental Chemistry, Animals, Metabolomics, Nanotechnology, Water Pollutants, Effluent, 0105 earth and related environmental sciences, Chironomus riparius, Chromatography, ved/biology, 010401 analytical chemistry, fungi, Public Health, Environmental and Occupational Health, General Medicine, General Chemistry, Pollution, Invertebrates, 6. Clean water, 0104 chemical sciences, chemistry, 13. Climate action, Benthic zone, Larva, [SDE]Environmental Sciences, Sewage treatment, Xenobiotic, Chromatography, Liquid
Abstract

International audience; Nanoliquid chromatography (nanoLC) was coupled to high-resolution mass spectrometry (HRMS) to perform a non-targeted investigation on benthic invertebrates, Chironomus riparius exposed to wastewater treatment plant (WWTP) effluents. Insect larvae represent a complex and low-weight matrix that required the use of a miniaturized Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method of extraction followed by nanoLC-HRMS to perform the analysis. The optimization of this coupling in terms of separation conditions including trapping step, detection conditions and data treatment provided reproducible fingerprints on insect larvae exposed to WWTP effluents with both in situ and ex-situ approaches. Statistical treatments such as principal component analysis highlighted the impact of WWTP effluents on the metabolome of insect larvae and showed the influence of exposure conditions. The identification of discriminating signals (m/z, tR) matched with several potential endogenous biomarkers. These are mainly fatty acids, indicating a change in lipid metabolism that can be correlated with exposure to WWTP effluents. Several xenobiotics have also been detected, including ibuprofen and propranolol, whose identities have been confirmed by analytical standards. This work demonstrates the effectiveness and sensitivity of nanoLC-HRMS based environmental non-targeted approaches in ecotoxicological studies and provides the first profiling data for a very small aquatic invertebrate.

Published
2018

16. Phytochemical and Biological Investigation of Two Diplotaxis Species Growing in Tunisia: D. virgata & D. erucoides

Author

Hichem Ben Jannet, Nabiha Bouzouita, Nizar Ben Salah, Corinne Sanglar, Aurélie Fildier, Hervé Casabianca, Sophie Chenavas, Lab Chim Organ & Struct Synth & Anal Physiochim, Université de Tunis El Manar (UTM), PNBS - Produits naturels et biosourcés - Natural & Bio-based Products, Institut des Sciences Analytiques (ISA), Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Chimie Hétérocyclique, Produits Naturels et Réactivité [Monastir] (CHPNR), Département de Chimie [Monastir], Faculté des Sciences de Monastir (FSM), Université de Monastir - University of Monastir (UM)-Université de Monastir - University of Monastir (UM)-Faculté des Sciences de Monastir (FSM), Université de Monastir - University of Monastir (UM)-Université de Monastir - University of Monastir (UM), and TRACES - Technologie et Recherche en Analyse Chimique pour l'Environnement et la Santé

Subjects
Antioxidant, DPPH, medicine.medical_treatment, Phytochemicals, Ethyl acetate, Pharmaceutical Science, antioxidant activity, D. virgata, Antioxidants, Analytical Chemistry, chemistry.chemical_compound, Drug Discovery, Agar, erucoides, ABTS, Molecular Structure, biology, Free Radical Scavengers, Anti-Bacterial Agents, Phytochemical, Chemistry (miscellaneous), D. erucoides, Molecular Medicine, Antibacterial activity, Diplotaxis, Tunisia, food.ingredient, Gram-Positive Bacteria, fatty acids, Article, ABRUZZO, lcsh:QD241-441, food, lcsh:Organic chemistry, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Gram-Negative Bacteria, Botany, medicine, LEAVES, Hexanes, Physical and Theoretical Chemistry, Chromatography, antimicrobial activity, Plant Extracts, EXTRACTS, MEDICINE, Organic Chemistry, virgata, biology.organism_classification, NMR, chemistry, Brassicaceae, flavonoids, HARRA
Abstract

International audience; A phytochemical investigation of Diplotaxis virgata D.C. and D. erucoides (L.) D.C. (Brassicaceae) offered to the isolation of two new flavonoids isorhamnetin-3-O--l-glucopyranoside (1) and rhamnetin-3,3'-di-O--d-glucopyranoside (2), respectively. Their structures have been elucidated from the extended spectroscopic methods, including 1D- and 2D-NMR, UV and mass spectrometry analysis and by comparison with literature data. The fatty acid composition of the hexane extracts of the two species was also investigated by using GC-MS. The antioxidant activity of ethanol, ethyl acetate, n-butanol extracts and the isolated compounds from the two species was evaluated using DPPH and ABTS(+) scavenging assays. All the tested samples showed an efficient radical scavenging ability, with IC50 values ranging from 16-40 mu g/mL for the DPPH and from 17-44 mu g/mL for the ABTS(+) assays. In addition, the antibacterial activity of the prepared extracts and compounds 1 and 2, determined by well diffusion agar method against two Gram positive and five Gram negative bacteria, was evaluated and the results showed significant effects against all strains used.

Published
2015

17. High-Resolution Mass Spectrometry as a Tool To Evaluate the Sample Preparation of Sludge

Author

Alexandre Bergé, Audrey Buleté, Aurélie Fildier, Emmanuelle Vulliet, TRACES - Technologie et Recherche en Analyse Chimique pour l'Environnement et la Santé, Institut des Sciences Analytiques (ISA), Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), and Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)

Subjects
Chromatography, Chemistry, 010401 analytical chemistry, Extraction (chemistry), Analytical chemistry, 010501 environmental sciences, Quechers, Mass spectrometry, 01 natural sciences, 6. Clean water, 0104 chemical sciences, Analytical Chemistry, Solvent, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Targeted screening, Sample preparation, Retention time, Sludge, ComputingMilieux_MISCELLANEOUS, 0105 earth and related environmental sciences
Abstract

This study explored the sample preparation steps based on QuEChERS (quick, easy, cheap, effective, rugged, and safe) of a complex matrix, such as sewage sludge, regarding their impacts on the chemical signatures of the samples obtained via high-resolution mass spectrometry (HRMS). The effects on the HRMS signal of the intrinsic parameters of the QuEChERS method, such as the extraction solvent, the buffer salt, or the purification procedure, have been evaluated. Different strategies have been used to perform these evaluations, such as a comparison of the total number of HRMS signals, a comparison of the targeted screening based on more than 100 compounds, and a comparison of a nontargeted screening based both on the study of the most discriminating couples [mass-to-charge ratio (m/z); retention time (tR)] and on the most intense peaks. Moreover, two specific methods dedicated to the extraction of surfactants and drugs have been added to this comparison to visualize the impact of specific conditions on the ...

Published
2017

18. Isolation and structure elucidation of two new antioxidant flavonoid glycosides and fatty acid composition in Hedysarum carnosum Desf

Author

Hichem Ben Jannet, Nabiha Bouzouita, Corinne Sanglar, Aurélie Fildier, Sophie Chenavas, Ismahen Essaidi, Hervé Casabianca, Nizar Ben Salah, Lab Chim Organ & Struct Synth & Anal Physiochim, Université de Tunis El Manar (UTM), Faculté des Sciences de Monastir (FSM), Université de Monastir - University of Monastir (UM), PNBS - Produits naturels et biosourcés - Natural & Bio-based Products, Institut des Sciences Analytiques (ISA), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), TRACES - Technologie et Recherche en Analyse Chimique pour l'Environnement et la Santé, Laboratoire de Chimie Hétérocyclique, Produits Naturels et Réactivité [Monastir] (CHPNR), Département de Chimie [Monastir], Université de Monastir - University of Monastir (UM)-Université de Monastir - University of Monastir (UM)-Faculté des Sciences de Monastir (FSM), and Université de Monastir - University of Monastir (UM)-Université de Monastir - University of Monastir (UM)

Subjects
Fatty Acid composition, Antioxidant, DPPH, medicine.medical_treatment, Context (language use), 01 natural sciences, chemistry.chemical_compound, Rutin, Antioxidant activity, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, medicine, LEAVES, Organic chemistry, ROOTS, Flavonoids, Chromatography, ABTS, 010405 organic chemistry, 010401 analytical chemistry, EXTRACT, POLYBOTRYS, NMR, 0104 chemical sciences, chemistry, Phytochemical, Hedysarum carnosum, Kaempferol, Quercetin, Agronomy and Crop Science, SAPONINS
Abstract

International audience; The present work constitutes a contribution to the phytochemical investigation of Hedysarum carnosum aiming to search for novel bioactives secondary metabolites. In this context, the fractionation of the butanolic extract of H. carnosum flowers afforded two new flavonoid glycosides quercetin 3-O-beta-D-glucopyranosyl-(1 -> 2)-alpha-L-rhamnopyranosyl-(1 -> 6)-alpha-L-rhamnopyranoside 1 and kaempferol 3-O-beta-D-glucopyranosyl-(1 -> 2)-alpha-L-rhamnopyranosyl-(1 -> 6)-alpha-L-rhamnopyranoside 2 together with a the known rutin 3 indicated for the first time in this species. Their structures were determined on the basis of spectroscopic evidences (UV, HRMS and NMR) and comparison with literature. The fatty acid composition of the hexane extract of this species was also investigated by using GC-MS. The n-butanol extract and the isolates were assessed for their antioxidant potential using DPPH center dot and ABTS(center dot+) scavenging assays and ferric reducing power (FRAP). The n-butanol extract and its fractions exhibited efficient radical scavenging activity with IC50 values ranging from 16 to 37 mu g/mL for the DPPH center dot assay. The obtained results suggest that the isolated compounds 1 and 3 could be promising antioxidant agents.

Published
2016

19. Cyclic and non cyclic aliphatic–aromatic polyesters derived from biomass: Study of structures by MALDI-ToF and NMR

Author

Damien Prim, Hana Ben Abderrazak, Aurélie Fildier, Hatem Ben Romdhane, Hans R. Kricheldorf, Saber Chatti, Sylvain Marque, Institut des Sciences Analytiques (ISA), Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Synthèse, interactions et réactivité en chimie organique et bioorganique (SIRCOB), Université de Versailles Saint-Quentin-en-Yvelines (UVSQ)-Centre National de la Recherche Scientifique (CNRS), Ecole Nationale d'Ingénieurs de Tunis (ENIT), Université de Tunis El Manar (UTM), Institut fur Technische und Makromolekulare Chemie/Fachbereich Chemie TMC, Universität Hamburg (UHH), and Institut National de Recherche et d'Analyse Physico-Chimique (INRAP)

Subjects
Condensation polymer, Materials science, Polymers and Plastics, Polyesters, General Physics and Astronomy, Acid dichlorides, 02 engineering and technology, MALDI-ToF mass spectrometry, 010402 general chemistry, Mole fraction, Mass spectrometry, 01 natural sciences, 6 Dianhydrohexitols, Differential scanning calorimetry, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Polymer chemistry, Materials Chemistry, Alkyl, 4:3, Polycondensation, chemistry.chemical_classification, Organic Chemistry, Polymer, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Polyester, chemistry, 0210 nano-technology, Glass transition
Abstract

International audience; New polyesters were prepared by polycondensation in solution of 1,4:3,6 dianhydrohexitols with various aliphatic-aromatic acid dichlorides which differ by their chain length (m = 6,8,10). They are obtained with yields in the range of between 89% and 95%. In order to obtain these polymers within optimum conditions, a systematic study was conducted on the effect of the parameters involved in the reaction, such as the alkyl chain length of acid dichlorides and the endo or exo positions of hydroxyl function of diols. The resulting polyesters were characterized by different analytical techniques such as NMR (1H and 13C), FT-IR spectrometry, SEC measurements and MALDI-ToF mass spectrometry. Under optimized conditions a high molar fraction of cyclic polyesters was formed. The differential scanning calorimetry (DSC) measurements revealed an amorphous character with glass transition temperatures in the range of 27-45 °C. The polymers are obtained with inherent viscosities in the range of 0.11-0.25 dL/g with a polydispersity index between 1.75 and 1.99.

Published
2011

20. Biosourced Cyclic and Multicyclic Polyesters Based on 1,4:3,6-Dianhydrohexitols: Application to Metal Ions Uptake in Aqueous Media

Author

Hans R. Kricheldorf, Raouf Medimagh, Saber Chatti, Mongia Saïd Zina, Aurélie Fildier, Haythem Bennour, Laboratoire des Substances Naturelles (LR02INRAP10), Institut National de Recherche et d'Analyse Physico-chimique [Ariana, Tunisie] (INRAP), TRACES - Technologie et Recherche en Analyse Chimique pour l'Environnement et la Santé, Institut des Sciences Analytiques (ISA), Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), PNBS - Produits naturels et biosourcés - Natural & Bio-based Products, Institut fur Technische und Makromolekulare Chemie/Fachbereich Chemie TMC, Universität Hamburg (UHH), Laboratoire de Chimie des Materiaux, Faculte ́ des Sciences de Tunis, Universite ́ de Tunis El Manar, Laboratoire de Chimie des Materiaux, and the Tunisian Ministry of Higher Education and Research for financial support together with EGIDE (Project 'PHC Utique' 13G/1211).

Subjects
MALDI-TOF, Condensation polymer, Isosorbide, ADSORPTION, Polymers and Plastics, Metal ions in aqueous solution, Inorganic chemistry, Diol, DICARBOXYLIC-ACID, polyesters, Mass spectrometry, multicyclic, chemistry.chemical_compound, MALDI ToF, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Polymer chemistry, SUCCINIC ACID, Materials Chemistry, Magic angle spinning, medicine, metal uptake, Organic chemistry, POLYCONDENSATION, Physical and Theoretical Chemistry, FREE SAMPLE PREPARATION, POLY(ETHER ESTER)S, Organic Chemistry, MASS-SPECTROMETRY, Condensed Matter Physics, STATE, Polyester, Matrix-assisted laser desorption/ionization, ISOSORBIDE, chemistry, medicine.drug
Abstract

Authors want to thank all INRAP staff for analysis and helpful discussion. M. Mezni is acknowledged for NMR experiments, R. Jebali and N. Chaabane for ICP analysis.; International audience; Isosorbide and isomannide are polycondensed in solution with trimesoyl chloride at a concentration of 0.06 mol L-1 for the synthesis of cyclic and multicyclic polyesters. The feed ratio diol/trimesoyl chloride is varied from 1.0/1.0 to 1.6/1.0. As all obtained polyesters prove insoluble, innovative solvent-free matrix assisted laser desorption ionization time-of-flight mass spectrometry (MALDI ToF MS) is performed for their characterization. The influence of the stereochemistry is shown to be of great importance for the cyclization trend. Both isosorbide and isomannide lead mainly to cyclic and multicyclic structures at a feed ratio of 1.0/1.0 and 1.1/1.0. Isomannide gives higher fractions of multicyclic structures. The products are characterized by complementary techniques such as C-13 cross polarization magic angle spinning nuclear magnetic resonance (C-13 CP-MAS NMR) and differential scanning calorimetry measurements. Application as a cryptands for the uptake of metal ions in aqueous media is followed by inductively coupled plasma atomic emission spectroscopy (ICP AES) analysis and reveal efficient toward large range of metals with tunable selectivity depending on the starting diol.

Published
2015

21. Synthesis and characterization of isosorbide-based α,ω-dihydroxyethersulfone oligomers

Author

Raouf Medimagh, Audrey Buleté, Hans R. Kricheldorf, Saber Chatti, Hatem Ben Romdhane, Aurélie Fildier, Chaouki Belgacem, Laboratoire des Substances Naturelles (LR02INRAP10), Institut National de Recherche et d'Analyse Physico-chimique [Ariana, Tunisie] (INRAP), TRACES - Technologie et Recherche en Analyse Chimique pour l'Environnement et la Santé, Institut des Sciences Analytiques (ISA), Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Institut für Technische und Makromolekulare Chemie, Universität Hamburg (UHH), Laboratoire de Chimie Organique Structurale et Macromoléculaire (LR99ES14), Université de Tunis El Manar (UTM), PNBS - Produits naturels et biosourcés - Natural & Bio-based Products, and Institut fur Technische und Makromolekulare Chemie/Fachbereich Chemie TMC

Subjects
Materials science, Condensation polymer, Isosorbide, Polymers and Plastics, isosorbide, PHASE-TRANSFER CATALYSIS, General Chemical Engineering, DIOLS, Size-exclusion chromatography, DIANHYDROHEXITOLS, Hydroxylation, chemistry.chemical_compound, Differential scanning calorimetry, polyethersulfones, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Materials Chemistry, medicine, Organic chemistry, MICROWAVE, oligomers, chemistry.chemical_classification, MALDI-ToF, POLYURETHANES, General Chemistry, Polymer, Nuclear magnetic resonance spectroscopy, NMR, Monomer, chemistry, ACID, POLYMERS, polycondensation, medicine.drug
Abstract

International audience; Functionalization of bio-based oligomers is a relevant approach in order to allow these materials to replace more conventional and nonbiodegradable polymers in a wider range of applications. This article will report on the hydroxylation of isosorbide-based ethersulfone oligomers. The hydroxy end-group was controlled by the variation of polycondensation parameters. Comparative study was conducted to assess the effect of isosorbide excess and the monomer concentration on structural composition and molecular weights of produced oligomers. Depending on reaction conditions, various products were synthesized, mainly alpha,omega-dihydroxyethersulfone oligomers. The characterization of the synthesized polyethersulfone was demonstrated by MALDI-TOF, NMR spectroscopy, differential scanning calorimetry, and size exclusion chromatography.

Published
2015

22. New biosourced alternated poly(ether)Ester-Amides (PeEA): synthesis and combined NMR/MALDI ToF MS characterization

Author

Sylvain R. A. Marque, Audrey Buleté, Asma Saadaoui, Salma Mghirbi, Aurélie Fildier, Raouf Medimagh, Guy Raffin, Saber Chatti, Damien Prim, Institut National de Recherche et d'Analyse Physico-Chimique (INRAP), Institut Lavoisier de Versailles (ILV), Université de Versailles Saint-Quentin-en-Yvelines (UVSQ)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), TRACES - Technologie et Recherche en Analyse Chimique pour l'Environnement et la Santé, Institut des Sciences Analytiques (ISA), Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), and Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)

Subjects
Condensation polymer, Isosorbide, Materials science, Polymers and Plastics, MALDI ToF mass spectrometry, Ether, chemistry.chemical_compound, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, 4-3, Polymer chemistry, Materials Chemistry, medicine, Organic chemistry, Polycondensation, chemistry.chemical_classification, 6-dianhydrohexitols, Organic Chemistry, Sebacoyl chloride, Nuclear magnetic resonance spectroscopy, Polymer, Matrix-assisted laser desorption/ionization, chemistry, Polymerization, Biobased, Alternated poly(ether)Ester-Amides, medicine.drug
Abstract

International audience; New biosourced alternated poly(ether)Ester-Amides PeEA were prepared by polycondensation in solution or in bulk of unprecedented aminoalcohols based on 1,4:3,6-dianhydrohexitols (DAH) with aromatic and aliphatic diacyl chlorides (sebacoyl, terephtaloyl and isophtaloyl). Optimization of the polymerization in solution has been investigated using MALDI ToF MS and NMR spectroscopy to ascertain the structures and end chain nature of the resulting polymers. The influence of the DAH stereochemistry and the polymerization mode on the structures and thermal properties was demonstrated by MALDI ToF and complementary analytical techniques (DSC and SEC). Isomannide based polymers revealed amorphous but showed higher Tg (around 80 °C for sebacoyl and 180 °C for isophtaloyl) whereas the isosorbide based polymers were semi crystalline. Best properties were obtained in bulk using isomannide based aminoalcohol and sebacoyl chloride (Tg of 82 °C and Mw of 32 kDa, PDI = 1.41).

Published
2014

23. Hyperbranched cyclic and multicyclic poly(etherketone)s by polycondensation of isosorbide and isomannide with 2,6,4′-trifluorobenzophenone and 1,3,5-tris(4-fluorobenzoyl) benzene

Author

Guy Raffin, Saber Chatti, Hans R. Kricheldorf, Aurélie Fildier, Raouf Medimagh, Mongia Saïd Zina, Haythem Bennour, Marie Hangouet, Institut National de Recherche et d'Analyse Physico-Chimique (INRAP), TRACES - Technologie et Recherche en Analyse Chimique pour l'Environnement et la Santé, Institut des Sciences Analytiques (ISA), Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Faculté des Sciences Mathématiques, Physiques et Naturelles de Tunis (FST), Université de Tunis El Manar (UTM), Institut fur Technische und Makromolekulare Chemie/Fachbereich Chemie TMC, and Universität Hamburg (UHH)

Subjects
Condensation polymer, Isosorbide, Polymers and Plastics, Chemistry, Dimethyl sulfoxide, Organic Chemistry, Diol, [CHIM.MATE]Chemical Sciences/Material chemistry, Toluene, Potassium carbonate, chemistry.chemical_compound, Monomer, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Polymer chemistry, Materials Chemistry, medicine, Benzene, medicine.drug
Abstract

1,3,5-Tris(4-fluorobenzoyl)benzene (TFBB) and 2,6,4′-trifluorobenzophenone (TFB) were polycondensed with isosorbide and isomanide. All polycondensations were performed in a mixture of dimethyl sulfoxide and toluene with potassium carbonate as promotor. Optimal concentration to avoid gelation was set at 0.06 mol L−1. The different cyclization tendencies on the basis of monomers conformations are discussed. In the TFB series, the feed ratio isosorbide/TFB was varied from 1.0:1.0 to 1.5:1.0. A majority of linear and hyperbranched species were identified as main reaction products by matrix-assisted laser desorption/ionization–time-of-flight mass spectrometry regardless of the diol with slight cyclization tendency for isomannide. When TFBB was polycondensed with isosorbide, the cyclization tendency was significantly improved. The products obtained at a feed ratio of 1.41/1.0 and 1.51/1.0 were rich in cyclic and multicyclic species. More interesting results were obtained from the polycondensation of TFBB and isomannide, giving rise majoritarily to cyclic, bicyclic, and multicyclic species. Differential scanning calorimetric measurements indicated high glass transition temperature (around 200°C).

Published
2014

24. Synthesis of biosourced polyether-amides from 1,4-3,6-dianhydrohexitols: Characterization by NMR and MALDI-ToF mass spectrometry

Author

Guy Raffin, Hans R. Kricheldorf, Salma Mghirbi, Marlène Desloir-Bonjour, Aurélie Fildier, Saber Chatti, Raouf Medimagh, Asma Saadaoui, Institut National de Recherche et d'Analyse Physico-Chimique (INRAP), TRACES - Technologie et Recherche en Analyse Chimique pour l'Environnement et la Santé, Institut des Sciences Analytiques (ISA), Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Institut fur Technische und Makromolekulare Chemie/Fachbereich Chemie TMC, Universität Hamburg (UHH), the Tunisian Ministry of Higher Education and Research, Ingénierie des Matériaux Polymères (IMP), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet [Saint-Étienne] (UJM)-Centre National de la Recherche Scientifique (CNRS), Laboratoire des Substances Naturelles (LR02INRAP10), Institut National de Recherche et d'Analyse Physico-chimique [Ariana, Tunisie] (INRAP), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), and Institut für Technische und Makromolekulare Chemie

Subjects
Polyether-amides, Isosorbide, Condensation polymer, General Chemical Engineering, 02 engineering and technology, 010402 general chemistry, MALDI-ToF mass spectrometry, 01 natural sciences, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, 4-3, medicine, [CHIM]Chemical Sciences, Organic chemistry, 6-Dianhydrohexitols, ComputingMilieux_MISCELLANEOUS, Polycondensation, Chemistry, General Chemistry, Nuclear magnetic resonance spectroscopy, 021001 nanoscience & nanotechnology, MALDI-TOF Mass Spectrometry, 0104 chemical sciences, Characterization (materials science), 0210 nano-technology, Biobased, medicine.drug
Abstract

International audience; New series of polyether-amides were prepared by polycondensation in solution of three diamines based on 1,4-3,6-dianhydrohexitols with two types of diacyl chlorides (sebacoyl and isophtaloyl). Unprecedented diamines based on isomannide and isoidide were elaborated. The corresponding polyether-amides (PeA) were obtained with high yields. They were characterized by different analytical techniques (NMR, MALDI-ToF MS, DSC). The combination of MALDI-ToF MS with NMR spectroscopy allowed us to confirm structure types. DSC measurements revealed an amorphous character for the isophtaloyl family with a high Tg value. The sebacoyl series proved to be semi-crystalline with a high Tm value. Isosorbide-based PeAs demonstrated interesting properties (Tg above 210 °C and Tm above 240 °C) and high viscosity (0.32).

Published
2013

25. Doping control using high and ultra-high resolution mass spectrometry based non-targeted metabolomics-A case study of salbutamol and budesonide abuse

Author

Cécile Cren-Olivé, Corinne Buisson, Aurélie Fildier, Marianna Lucio, Philippe Schmitt-Kopplin, Agnèta Kiss, TRACES - Technologie et Recherche en Analyse Chimique pour l'Environnement et la Santé, Institut des Sciences Analytiques (ISA), Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Helmholtz-Zentrum München (HZM), Département des Analyses, Agence Française de Lutte contre le Dopage (AFLD), Agence française de lutte contre le dopage-Agence française de lutte contre le dopage, Région Rhone-Alpes (Thèse A. Kiss), PHC Procope (METADOP), and METADOP

Subjects
Spectrometry, Mass, Electrospray Ionization, Metabolite, Electrospray ionization, lcsh:Medicine, Urine, Mass spectrometry, 01 natural sciences, Mass Spectrometry, 03 medical and health sciences, chemistry.chemical_compound, Metabolomics, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Partial least squares regression, Humans, ddc:630, Albuterol, Least-Squares Analysis, Budesonide, lcsh:Science, Chromatography, High Pressure Liquid, 030304 developmental biology, Doping in Sports, Principal Component Analysis, 0303 health sciences, Multidisciplinary, Chromatography, Fourier Analysis, OPLS, lcsh:R, 010401 analytical chemistry, Signal Processing, Computer-Assisted, Cyclotrons, Creatine, Healthy Volunteers, ddc, 3. Good health, 0104 chemical sciences, chemistry, Athletes, Xanthines, Principal component analysis, lcsh:Q, Ribonucleosides, Metabolic Networks and Pathways, Research Article
Abstract

International audience; We have detected differences in metabolite levels between doped athletes, clean athletes, and volunteers (non athletes). This outcome is obtained by comparing results of measurements from two analytical platforms: UHPLC-QTOF/MS and FT-ICR/MS. Twenty-seven urine samples tested positive for glucocorticoids or beta-2-agonists and twenty samples coming from volunteers and clean athletes were analyzed with the two different mass spectrometry approaches using both positive and negative electrospray ionization modes. Urine is a highly complex matrix containing thousands of metabolites having different chemical properties and a high dynamic range. We used multivariate analysis techniques to unravel this huge data set. Thus, the several groups we created were studied by Principal Components Analysis (PCA) and Partial Least Square regression (PLS-DA and OPLS) in the search of discriminating m/z values. The selected variables were annotated and placed on pathway by using MassTRIX.

Published
2013

26. A complementary LC-ESI-MS and MALDI-TOF approach for screening antibacterial proteomic signature of farmed European Sea bass mucus

Author

Sami Barrek, Aurélie Fildier, Sonia Fekih-Zaghbib, Balkiss Bouhaouala-Zahar, Food Technology laboratory, National Institute of Nutrition and Food Technology, Laboratoire des Venins et Biomolécules Thérapeutiques - Laboratory of Venoms and Therapeutic Biomolecules (LR11IPT08), Institut Pasteur de Tunis, Réseau International des Instituts Pasteur (RIIP)-Réseau International des Instituts Pasteur (RIIP), Institut des Sciences Analytiques (ISA), Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Institut Supérieur de Biotechnologie de Sidi Thabet (ISBST), Université de la Manouba [Tunisie] (UMA), Faculté de Médecine, Université de Tunis El Manar (UTM), and the National Institute of Chemistry Research, Sidi Thabet, Tunisia

Subjects
Fish Proteins, MALDI-TOF, Spectrometry, Mass, Electrospray Ionization, Tunisia, Proteome, Aquaculture, Microbial Sensitivity Tests, Aquatic Science, Biology, Chrysophsins, Gram-Positive Bacteria, medicine.disease_cause, Microbiology, 03 medical and health sciences, Minimum inhibitory concentration, Liquid chromatography–mass spectrometry, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Candida albicans, Gram-Negative Bacteria, medicine, Animals, Environmental Chemistry, Dicentrarchus labrax, 14. Life underwater, Sea bass, Escherichia coli, 030304 developmental biology, 0303 health sciences, Molecular mass, 04 agricultural and veterinary sciences, General Medicine, biology.organism_classification, Mucus, Immunity, Innate, Aeromonas, Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization, 040102 fisheries, 0401 agriculture, forestry, and fisheries, Bass, Dicentrarchus, Antimicrobial peptide, Antimicrobial Cationic Peptides, Chromatography, Liquid
Abstract

International audience; Antibacterial protection in the mucus is provided by antimicrobial compounds and till now few numbers of AMP and proteins were identified. Herein, mass spectral profiling of fresh mucus from farmed sea bass (Dicentrarchus labrax) using Matrix-assisted laser desorption/ionization-time-of-flight mass spectrometer (MALDI-TOF) and liquid chromatography mass spectrometry is investigated in order to survey the infective/healthy status of the mucus. We identify AMP peptides of 2891.7, 2919.45 and 2286.6 Da molecular weight respectively and characterize Chrysophsins in the mucus of Dicentrarchus labrax. These peptides display broad-spectrum bactericidal activity against Gram-negative (Minimum Inhibitory Concentrations namely MICs < 0.5 μM) and Gram-positive bacteria (MICs < 0.5 μM) including Escherichia coli and Bacillus subtilis. Furthermore, sensitivity to yeast Candida albicans is reported for the first time and shows interesting MICs of less than 2 μM. We also demonstrate that the fish pathogen Aeromonas salmonoicida is sensitive to Chrysophsins (MICs ranging between 5 and 14 μM). Our mucus molecular mass mapping developed approach allows for fast exploration of immune status. Our data provides evidence that Chrysophsins are secreted by immune cells and are released in mucus of non-challenged farmed European sea bass. These results suggest that Chrysophsins, secreted by gills of red sea bream, are an important widespread component of Teleostei defense against disease.

Published
2013

27. Synthesis of new poly(ether ketone)s derived from biobased diols

Author

Hans R. Kricheldorf, Aurélie Fildier, Saber Chatti, Hana Ben Abderrazak, Hatem Ben Romdhane, Institut National de Recherche et d'Analyse Physico-Chimique (INRAP), Laboratoire de Chimie Organique Structurale et Macromoléculaire (LR99ES14), Université de Tunis El Manar (UTM), TRACES - Technologie et Recherche en Analyse Chimique pour l'Environnement et la Santé, Institut des Sciences Analytiques (ISA), Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Institut für Technische und Makromolekulare Chemie, Universität Hamburg (UHH), and Higher Education Ministry of Tunisia (phD support) Collaboration INRAP/ISA

Subjects
Isosorbide, Ketone, Condensation polymer, Polymers and Plastics, Inherent viscosity, Ether, 02 engineering and technology, 010402 general chemistry, dianhydrohexitols, 01 natural sciences, poly(ether ketone)s, chemistry.chemical_compound, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Polymer chemistry, Materials Chemistry, medicine, Organic chemistry, Physical and Theoretical Chemistry, Benzene, chemistry.chemical_classification, Organic Chemistry, matrix-assisted laser desorption/ionization mass spectrometry (MALDI MS), 021001 nanoscience & nanotechnology, Condensed Matter Physics, 0104 chemical sciences, macrocycles, chemistry, Yield (chemistry), Mass spectrum, 0210 nano-technology, polycondensation, medicine.drug
Abstract

International audience; Thumbnail image of graphical abstract A new class of poly(ether ketone)s (PEKs) is prepared by polycondensation of various diols produced from biomass and various difluoro aromatics. After optimization of the reaction conditions, polycondensation of isosorbide and 4,4′-difluorodiphenylketone (2a) gives PEK1 with a high yield, moderate viscosity (0.31 dL g−1), and a glass-transition temperature (Tg) of 170 °C. The optimum conditions are applied to the synthesis of a series of PEKs (PEK 2-9) from difluoro agents and sugar diols. The polycondensation of isomannide (1b) with 1,4-di(p-fluorobenzoyl)benzene (2b) gives the best results with an inherent viscosity of 0.52 dL g−1 and the mass spectrum shows an abundance of cyclic structures. Similar conditions are used for the preparation of high-molar-mass copoly(ether ketone)s from a stoechiometric mixture of isosorbide/bisphenol-A.

Published
2013

28. Copolyesters of isosorbide, succinic acid, and isophthalic acid: biodegradable, high Tg engineering plastics

Author

Aurélie Fildier, Hans R. Kricheldorf, Saber Chatti, Steffen M. Weidner, Institut des Sciences Analytiques (ISA), Centre National de la Recherche Scientifique (CNRS)-Université de Lyon-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon, BAM Federal Institute for Materials Research and Testing, Federal Institute for Materials Research and Testing - Bundesanstalt für Materialforschung und -prüfung (BAM), Institut für Technische und Makromolekulare Chemie, Universität Hamburg (UHH), TRACES - Technologie et Recherche en Analyse Chimique pour l'Environnement et la Santé, Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Institut fur Technische und Makromolekulare Chemie/Fachbereich Chemie TMC, and Institute for Technical and Macromolecular Chemistry of the University of Hamburg

Subjects
Isosorbide, TEREPHTHALIC ACID, cyclization, Polymers and Plastics, isosorbide, DICARBOXYLIC-ACID, 4/3, polyesters, 010402 general chemistry, 01 natural sciences, Isophthalic acid, chemistry.chemical_compound, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Polymer chemistry, Materials Chemistry, medicine, succinic acid, Organic chemistry, Terephthalic acid, chemistry.chemical_classification, CYCLIC POLYMERS, 6-DIANHYDROHEXITOLS, Molar mass, 010405 organic chemistry, isophthalic acid, Organic Chemistry, ALIPHATIC POLYESTERS, CHAIN COMPETITION KINETICS, renewable resources, 0104 chemical sciences, cyclopolymerization, POLYMERIZATION, Dicarboxylic acid, chemistry, Succinic acid, Chlorobenzene, biodegradable, polycondensation, Stoichiometry, medicine.drug
Abstract

International audience; Isosorbide, succinyl chloride and isophthaloyl chloride are polycondensed under various reaction conditions. The heating in bulk with or without catalysts as well in an aromatic solvent without catalyst, and polycondensation with the addition of pyridine only yield low molar mass copolyesters. However, heating in chlorobenzene with addition of SnCl2 or ZnCl2 produces satisfactory molar masses. The number average molecular weights (Mn) of most copolyesters fall into the range of 700015,000 Da with polydispersities (PD) in the range of 39. The MALDI-TOF mass spectra almost exclusively displayed peaks of cyclics indicating that the chain growth was mainly limited by cyclization and not by side reactions, stoichiometric imbalance or incomplete conversion. The glass-transition temperatures increased with the content of isophthalic acid from 75 to 180 degrees C and the thermo-stabilities also followed this trend.

Published
2013

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