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1. Screening and Evaluation of Dermo-Cosmetic Activities of the Invasive Plant Species Polygonum cuspidatum

Author

Vanille Quinty, Cyril Colas, Rouba Nasreddine, Reine Nehmé, Christine Piot, Micheline Draye, Emilie Destandau, David Da Silva, and Gregory Chatel

Subjects
Polygonaceae, Polygonum cuspidatum, invasive plant species, superoxide dismutase, hyaluronidase, elastase, Botany, QK1-989
Abstract

Polygonum cuspidatum (P. cuspidatum) is among the world’s most problematic invasive plant species with negative ecological, socio-economic and security consequences. Management operations in areas invaded systematically generate a large quantity of plant waste, most often without outlets. Using this plant material could constitute a new alternative treatment for sustainable management. P. cuspidatum is well known to have numerous biological properties, containing notably stilbenes, quinones, flavonoids and phenolic acids. The present work proposes a reliable strategy using powerful techniques for the screening and the evaluation of the dermo-cosmetic potential of its aerial parts (AP) and root parts (RP). To the best of our knowledge, only antioxidant and anti-tyrosinase activities were previously evaluated on P. cuspidatum among the targets studied (superoxide dismutase, hyaluronidase, elastase, collagenase and tyrosinase). The results revealed strong antioxidant and anti-collagenase activities, moderate anti-hyaluronidase activity, while weak anti-elastase and anti-tyrosinase activities were observed for ethanolic extracts. Different standards selected and screened on the same targets made it possible to correlate the observed residual activities of produced extracts of P. cuspidatum from Savoie Mont Blanc and their chemical compositions. A structure-activity study was thus conducted on main molecular families, widely represented in the genus Polygonum.

Published
2022
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2. An Assessment of Indoor Air Quality in the Arrivals Hall of Beirut–Rafic Hariri International Airport: Monitoring of VOCs and NO2

Author

Tharwat Mokalled, Jocelyne Adjizian Gérard, Maher Abboud, Céline Liaud, Rouba Nasreddine, and Stéphane Le Calvé

Subjects
indoor air pollution, Volatile Organic Compounds (VOCs), heavy alkanes, nitrogen dioxide (NO2), airport, Beirut, Meteorology. Climatology, QC851-999
Abstract

In Beirut–Rafic Hariri International Airport (RHIA), airport employees stay at least 12 h inside the airport’s buildings and suffer from respiratory symptoms. Additionally, direct openings exist between the apron and the arrivals hall providing a pathway for contaminated air to enter the buildings. Hence, we study the impact of Beirut–RHIA’s activities on the indoor air of the arrivals hall (impact on employees and passengers) during June, November, and October 2014. Due to their impacts on air quality and human health, assessing of the concentrations of nitrogen dioxide (NO2) and Volatile Organic Compounds (VOCs) was the target of our study by using gas chromatographic techniques (GC-MS and GC-FID) for VOCs and calorimetric methods for NO2 concentrations. NO2 levels indicated a probable hazard to the health of passengers and employees, while measured VOC levels did not present any risks except for acrolein. This is the first study to assess the speciation of a large number of VOCs (46 VOCs) for airport indoor air while revealing a very interesting correlation between aircraft number and the concentrations of VOC groups (namely heavy alkanes, aldehydes and ketones, and monoaromatics). Moreover, this is the first study in Lebanon to assess the speciation of a large number of VOCs in indoor air.

Published
2021
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3. Water-Based Extraction of Bioactive Principles from Blackcurrant Leaves and Chrysanthellum americanum: A Comparative Study

Author

Phu Cao-Ngoc, Laurent Leclercq, Jean-Christophe Rossi, Jasmine Hertzog, Anne-Sylvie Tixier, Farid Chemat, Rouba Nasreddine, Ghassan Al Hamoui Dit Banni, Reine Nehmé, Philippe Schmitt-Kopplin, and Hervé Cottet

Subjects
blackcurrant, hawthorn, Chrysanthellum americanum, water-based extraction, polyphenol, flavonoid, Chemical technology, TP1-1185
Abstract

The water-based extraction of bioactive components from flavonoid-rich medicinal plants is a key step that should be better investigated. This is especially true when dealing with easy-to-use home-made conditions of extractions, which are known to be a bottleneck in the course for a better control and optimization of the daily uptake of active components from medicinal plants. In this work, the water-based extraction of Blackcurrant (Ribes nigrum) leaves (BC) and Chrysanthellum americanum (CA), known to have complementary pharmacological properties, was studied and compared with a previous work performed on the extraction of Hawthorn (Crataegus, HAW). Various extraction modes in water (infusion, percolation, maceration, ultrasounds, microwaves) were compared for the extraction of bioactive principles contained in BC and CA in terms of extraction yield, of amount of flavonoids, phenolic compounds, and proanthocyanidin oligomers, and of UHPLC profiles of the extracted compounds. The qualitative and quantitative aspects of the extraction, in addition to the kinetic of extraction, were studied. The optimized easy-to-use-at-home extraction protocol developed for HAW was found very efficient to easily extract bioactive components from BC and CA plants. UHPLC-ESI-MS and high-resolution Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) were also implemented to get more qualitative information on the specific and common chemical compositions of the three plants (including HAW). Their antihyaluronidase, antioxidant, and antihypertensive activities were also determined and compared, demonstrating similar activities as the reference compound for some of these plants.

Published
2020
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5. Reproducibility and accuracy of microscale thermophoresis in the NanoTemper Monolith: a multi laboratory benchmark study

Author

Caroline Mas, Grzegorz Piszczek, Marjetka Podobnik, Kathryn Perez, Timothy Sharpe, Stephen H. McLaughlin, Roland Montserret, Stefan H. Knauer, Bruno Baron, Christopher M. Johnson, Quyen Nguyen, Mark A. Williams, Katja Pirc, Arthur Sedivy, Celeste Abreu, Tina Daviter, David Ortega-Alarcon, Daumantas Matulis, Rouba Nasreddine, Carlo Carolis, Thomas A. Jowitt, Stephan Uebel, David Staunton, Andrew P. Leech, Maria Garcia-Alai, June Southall, Alexander Fish, Jitka Holková, Alexander K. Buell, Michael Weyand, Jasmina Rokov-Plavec, Blanca López-Méndez, Sylvie Berger, Josef Houser, Natalia Rodrigo, Wojciech Bal, Chad A. Brautigam, Josef Hamacek, Reine Nehmé, Olga Abian, Christian Guenther, Ondrej Vanek, Susanne Schaefer, Sharon M. Kelly, Malgorzata Adamczyk, Di Wu, Pedro Tavares, University of Copenhagen = Københavns Universitet (KU), Biophysique Moléculaire (plateforme) - Molecular Biophysics (platform), Institut Pasteur [Paris]-Centre National de la Recherche Scientifique (CNRS), University of Texas Southwestern Medical Center [Dallas], University of Manchester [Manchester], Universität Bayreuth, Max Planck Institute of Biochemistry (MPIB), Max-Planck-Gesellschaft, University of London [London], Vienna Biocenter Core Facilities, Partenaires INRAE, University of Zaragoza - Universidad de Zaragoza [Zaragoza], Charles University [Prague] (CU), Warsaw University of Technology [Warsaw], Institute of Biochemistry and Biophysics, Polish Academy of Sciences (PAN), Institut de Recherches SERVIER (IRS), Technical University of Denmark [Lyngby] (DTU), Centre for Genomic Regulation [Barcelona] (CRG), Universitat Pompeu Fabra [Barcelona] (UPF)-Centro Nacional de Analisis Genomico [Barcelona] (CNAG), The institute of cancer research [London], Netherlands Cancer Institute (NKI), Antoni van Leeuwenhoek Hospital, EMBL Hamburg, Centre de biophysique moléculaire (CBM), Université d'Orléans (UO)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), Central European Institute of Technology [Brno] (CEITEC MU), Brno University of Technology [Brno] (BUT), MRC Laboratory of Molecular Biology [Cambridge, UK] (LMB), University of Cambridge [UK] (CAM)-Medical Research Council, University of Glasgow, University of York [York, UK], Integrated Structural Biology Grenoble (ISBG - UMS 3518 ), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-European Molecular Biology Laboratory [Grenoble] (EMBL)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA), Vilnius University [Vilnius], Institut de biologie et chimie des protéines [Lyon] (IBCP), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie Organique et Analytique (ICOA), Université d'Orléans (UO)-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Institut National de la Santé et de la Recherche Médicale (INSERM), EMBL Heidelberg, National Institute of Chemistry, National Heart, Lung, and Blood Institute [Bethesda] (NHLBI), University of Zagreb, University of Bayreuth, University of Basel (Unibas), University of Oxford [Oxford], Faculdade de Ciências e Tecnologia [Faro] (FCT), Universidade do Algarve (UAlg), This research was funded by Fondo de Investigaciones Sanitarias from Instituto de Salud Carlos III and European Union (ERDF/ESF, 'Investing in your future' PI18/00349 and Diputación General de Aragón Digestive Pathology Group B25_17R to O.A. Spanish Ministry of Science, Innovation and Universities, FPI Predoctoral Research Contract BES-2017-080739 to D.O.A. This research was funded by project no 2015/17/B/NZ2/01160 (granted to MA), we also acknowledge financial support, from the Faculty of Chemistry at Warsaw University of Technology. As part of the Federal FTI strategy, this work was generously supported by the City of Vienna and the Austrian Ministry for Education, Science and Research., Frapart, Isabelle, University of Copenhagen = Københavns Universitet (UCPH), Institut Pasteur [Paris] (IP)-Centre National de la Recherche Scientifique (CNRS), Max-Planck-Institut für Biochemie = Max Planck Institute of Biochemistry (MPIB), Danmarks Tekniske Universitet = Technical University of Denmark (DTU), Université d'Orléans (UO)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Integrated Structural Biology Grenoble (ISBG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université d'Orléans (UO)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), and University of Oxford

Subjects
0301 basic medicine, 030103 biophysics, Materials science, Thermophoresis, Interaction, Biophysics, [SDV.BBM.BP] Life Sciences [q-bio]/Biochemistry, Molecular Biology/Biophysics, Calorimetry, Benchmark, 03 medical and health sciences, Biomolècules, MST, TRIC, KD, [PHYS.PHYS.PHYS-INS-DET]Physics [physics]/Physics [physics]/Instrumentation and Detectors [physics.ins-det], Surface plasmon resonance, Monolith, Reliability (statistics), Reproducibility, geography, geography.geographical_feature_category, K D, Microscale thermophoresis, Intensity change, Temperature, Reproducibility of Results, Correction, General Medicine, Biofísica, [SDV.BBM.BP]Life Sciences [q-bio]/Biochemistry, Molecular Biology/Biophysics, Benchmarking, 030104 developmental biology, [PHYS.PHYS.PHYS-INS-DET] Physics [physics]/Physics [physics]/Instrumentation and Detectors [physics.ins-det], Benchmark (computing), Original Article, Biological system, Laboratories
Abstract

Microscale thermophoresis (MST), and the closely related Temperature Related Intensity Change (TRIC), are synonyms for a recently developed measurement technique in the field of biophysics to quantify biomolecular interactions, using the (capillary-based) NanoTemper Monolith and (multiwell plate-based) Dianthus instruments. Although this technique has been extensively used within the scientific community due to its low sample consumption, ease of use, and ubiquitous applicability, MST/TRIC has not enjoyed the unambiguous acceptance from biophysicists afforded to other biophysical techniques like isothermal titration calorimetry (ITC) or surface plasmon resonance (SPR). This might be attributed to several facts, e.g., that various (not fully understood) effects are contributing to the signal, that the technique is licensed to only a single instrument developer, NanoTemper Technology, and that its reliability and reproducibility have never been tested independently and systematically. Thus, a working group of ARBRE-MOBIEU has set up a benchmark study on MST/TRIC to assess this technique as a method to characterize biomolecular interactions. Here we present the results of this study involving 32 scientific groups within Europe and two groups from the US, carrying out experiments on 40 Monolith instruments, employing a standard operation procedure and centrally prepared samples. A protein-small molecule interaction, a newly developed protein-protein interaction system and a pure dye were used as test systems. We characterized the instrument properties and evaluated instrument performance, reproducibility, the effect of different analysis tools, the influence of the experimenter during data analysis, and thus the overall reliability of this method. All authors acknowledge the COST Action project ARBRE-MOBIEU CA15126 under the auspices of whose Working Group 4 this study was carried out. ARBRE-MOBIEU COST Action CA15126 funded meetings in the Center for Protein Research, University of Copenhagen (ECOST-MEETING-CA15126-280618-098884) to organize this study and in the Vienna Biocenter Core Facilities GmbH (ECOST-MEETING-CA15126-121119-111544) to discuss the results of the benchmark. Ondřej Vaněk acknowledges support from the Ministry of Education, Youth and Sports of the Czech Republic (LTC17065 in frame of the COST Action CA15126). Jitka Holková and Josef Houser acknowledge CF Biomolecular Interactions and Crystallization of CIISB, Instruct-CZ Centre, supported by MEYS CR (LM2018127). Jasmina Rokov-Plavec acknowledges support from the Croatian Science Foundation (IP-2016-06-6272). Alexander K. Buell thanks the Novo Nordisk Foundation (grant number NNFSA170028392) for funding. Li Peng Lundgren acknowledges for preliminary MST/TRIC experiments (STMS 37745 in the frame of the COST Action CA15126) and the COST Action (CA15126) for a STMS (STMS 44783) for the data analysis. The Novo Nordisk Foundation Center for Protein Research is supported financially by the Novo Nordisk Foundation (Grant agreement NNF14CC0001). Katja Pirc and Marjetka Podobnik acknowledge the grant by the Slovenian Research Agency P1-0391 (Title: Molecular Interactions). This research was funded by Fondo de Investigaciones Sanitarias from Instituto de Salud Carlos III and European Union (ERDF/ESF, “Investing in your future” PI18/00349 and Diputación General de Aragón Digestive Pathology Group B25_17R to O.A. Spanish Ministry of Science, Innovation and Universities, FPI Predoctoral Research Contract BES-2017-080739 to D.O.A. This research was funded by project no 2015/17/B/NZ2/01160 (granted to MA)

Published
2021
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6. An assessment of indoor air quality in the maintenance room at Beirut-Rafic Hariri International Airport

Author

Rouba Nasreddine, Tharwat Mokalled, Céline Liaud, Maher Abboud, Stéphane Le Calvé, Jocelyne Adjizian Gerard, Université Saint-Joseph de Beyrouth (USJ), Laboratoire des Matériaux, Surfaces et Procédés pour la Catalyse (LMSPC), Institut de chimie et procédés pour l'énergie, l'environnement et la santé (ICPEES), Université de Strasbourg (UNISTRA)-Matériaux et nanosciences d'Alsace (FMNGE), Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA)-Matériaux et nanosciences d'Alsace (FMNGE), and Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)

Subjects
[SDU.OCEAN]Sciences of the Universe [physics]/Ocean, Atmosphere, Atmospheric Science, Ozone, 010504 meteorology & atmospheric sciences, Indoor air, Environmental engineering, 010501 environmental sciences, 01 natural sciences, Pollution, International airport, World health, chemistry.chemical_compound, Indoor air quality, chemistry, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, 13. Climate action, [SDE]Environmental Sciences, [CHIM]Chemical Sciences, Environmental science, Nitrogen dioxide, Contaminated air, Waste Management and Disposal, ComputingMilieux_MISCELLANEOUS, 0105 earth and related environmental sciences
Abstract

In Beirut-Rafic Hariri International Airport (RHIA)-Lebanon, direct openings exist between the apron and the arrivals hall providing a pathway for contaminated air to enter the buildings. Also, airport employees spend no less than 12 h inside the airport's buildings and experience respiratory symptoms. Therefore, the influence of Beirut-RHIA's activities on the indoor air quality of the maintenance room in the control tower (impact on employees) was the focus of this study. This is the first study to assess the speciation of 46 Volatile organic compounds (VOCs) in indoor air of an airport workplace. Measurements, conducted during June and October 2014, has focused, in particular, on nitrogen dioxide (NO2) and Volatile organic compounds (VOCs), key ozone and PM precursors emitted from aircraft exhaust. Gas chromatographic techniques (GC-FID) were used to assess the concentrations of 46 VOCs, whereas colorimetric methods were adopted to determine NO2 concentrations. In general, the concentrations of measured VOCs did not present any risks except for acrolein, and NO2 concentrations inside the maintenance room were significantly below the World Health Organization (WHO) annual threshold limit (40 μg m−3). An interesting correlation was observed between aircraft number and the concentration of light aldehydes/ketones measured in the maintenance room. This is the first study dedicated to assess the speciation of a large number of VOCs in a work place environment in Lebanon.

Published
2019
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7. Investigation of lipase-ligand interactions in porcine pancreatic extracts by microscale thermophoresis

Author

Axel Marchal, Syntia Fayad, Cyril Colas, Rouba Nasreddine, Ghassan Al Hamoui Dit Banni, Reine Nehmé, Institut de Chimie Organique et Analytique (ICOA), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université d'Orléans (UO)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut de chimie et procédés pour l'énergie, l'environnement et la santé (ICPEES), Université de Strasbourg (UNISTRA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Matériaux et Nanosciences Grand-Est (MNGE), Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS), Unité de Recherche Oenologie [Villenave d'Ornon] (OENO), Université de Bordeaux (UB)-Institut des Sciences de la Vigne et du Vin (ISVV)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Université d'Orléans (UO)-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Institut National de la Santé et de la Recherche Médicale (INSERM), Université de Strasbourg (UNISTRA)-Matériaux et nanosciences d'Alsace (FMNGE), Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), and Unité de Recherche Oenologie [Villenave d'Ornon]

Subjects
Swine, Pancreatic Extracts, 02 engineering and technology, Ligands, 01 natural sciences, Biochemistry, Analytical Chemistry, Small Molecule Libraries, Hydrolysis, Capillary electrophoresis, Animals, Lipase, Ammonium sulfate precipitation, Chromatography, biology, Chemistry, Microscale thermophoresis, 010401 analytical chemistry, 021001 nanoscience & nanotechnology, Ligand (biochemistry), 0104 chemical sciences, Dissociation constant, [SDE]Environmental Sciences, biology.protein, 0210 nano-technology, Protein Binding
Abstract

International audience; The evaluation of binding affinities between large biomolecules and small ligands is challenging and requires highly sensitive techniques. Microscale thermophoresis (MST) is an emerging biophysical technique used to overcome this limitation. This work describes the first MST binding method to evaluate binding affinities of small ligands to lipases from crude porcine pancreatic extracts. The conditions of the MST assay were thoroughly optimized to successfully evaluate the dissociation constant (Kd) between pancreatic lipases (PL) and triterpenoid compounds purified from oakwood. More precisely, the fluorescent labeling of PL (PL*) using RED-NHS dye was achieved via a buffer exchange procedure. The MST buffer was composed of 20 mM NaH2PO4 + 77 mM NaCl (pH 6.6) with 0.05% Triton-X added to efficiently prevent protein aggregation and adsorption, even when using only standard, uncoated MST capillaries. Storage at −20 °C ensured stability of PL* and its fluorescent signal. MST results showed that crude pancreatic extracts were suitable as a source of PL for the evaluation of binding affinities of small ligands. Quercotriterpenoside-I (QTT-I) demonstrated high PL* binding affinity (31 nM) followed by 3-O-galloylbarrinic acid (3-GBA) (500 nM) and bartogenic acid (BA) (1327 nM). To enrich the 50 kDa lipase responsible for the majority of hydrolysis activity in the crude pancreatic extracts, ammonium sulfate precipitation was attempted and its efficiency confirmed using capillary electrophoresis (CE)-based activity assays and HRMS. Moreover, to accurately explain enzyme modulation mechanism, it is imperative to complement binding assays with catalytic activity ones.

Published
2021
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8. Correction to: Reproducibility and accuracy of microscale thermophoresis in the NanoTemper Monolith: a multi laboratory benchmark study

Author

Di Wu, Reine Nehmé, David Ortega-Alarcon, Michael Weyand, June Southall, David Staunton, Carlo Carolis, Blanca López-Méndez, Christian Guenther, Quyen Nguyen, Maria Garcia-Alai, Alexander Fish, Josef Hamacek, Pedro Tavares, Thomas A. Jowitt, Caroline Mas, Stephan Uebel, Jitka Holková, Wojciech Bal, Bruno Baron, Katja Pirc, Olga Abian, Sylvie Berger, Roland Montserret, Sharon M. Kelly, Rouba Nasreddine, Marjetka Podobnik, Ondrej Vanek, Chad A. Brautigam, Timothy Sharpe, Natalia Rodrigo, Alexander K. Buell, Josef Houser, Mark A. Williams, Arthur Sedivy, Celeste Abreu, Kathryn Perez, Stephen H. McLaughlin, Andrew P. Leech, Malgorzata Adamczyk, Grzegorz Piszczek, Stefan H. Knauer, Jasmina Rokov-Plavec, Daumantas Matulis, Susanne Schaefer, Christopher M. Johnson, and Tina Daviter

Subjects
geography, Reproducibility, geography.geographical_feature_category, Materials science, Microscale thermophoresis, Nuclear engineering, Biophysics, Benchmark (computing), General Medicine, Monolith
Published
2021
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9. Screening for pancreatic lipase natural modulators by capillary electrophoresis hyphenated to spectrophotometric and conductometric dual detection

Author

Reine Nehmé, Rouba Nasreddine, Axel Marchal, Syntia Fayad, Jean-Christophe Rossi, Hervé Cottet, Ghassan Al Hamoui Dit Banni, Laurent Leclercq, Phu Cao-Ngoc, Leclercq, Laurent, Institut de Chimie Organique et Analytique (ICOA), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université d'Orléans (UO)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Unité de Recherche Œnologie [Villenave d'Ornon] (OENO), Université de Bordeaux (UB)-Institut des Sciences de la Vigne et du Vin (ISVV)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut des Biomolécules Max Mousseron [Pôle Chimie Balard] (IBMM), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Montpellier (UM)-Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM), Université de Montpellier (UM), Université d'Orléans (UO)-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Institut National de la Santé et de la Recherche Médicale (INSERM), Institut de chimie et procédés pour l'énergie, l'environnement et la santé (ICPEES), Université de Strasbourg (UNISTRA)-Matériaux et nanosciences d'Alsace (FMNGE), Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Unité de Recherche Oenologie [Villenave d'Ornon], Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM), Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Institut de Chimie du CNRS (INC)-Université de Montpellier (UM)-Centre National de la Recherche Scientifique (CNRS), ANR-11-LABX-0029,SYNORG,Synthèse Organique : des molécules au vivant(2011), Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Université de Montpellier (UM)-Centre National de la Recherche Scientifique (CNRS), Université d'Orléans (UO)-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut National de la Santé et de la Recherche Médicale (INSERM), Université de Strasbourg (UNISTRA)-Centre National de la Recherche Scientifique (CNRS)-Matériaux et nanosciences d'Alsace, and Centre National de la Recherche Scientifique (CNRS)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Université de Strasbourg (UNISTRA)-Centre National de la Recherche Scientifique (CNRS)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Université de Strasbourg (UNISTRA)

Subjects
Tris, [CHIM.ANAL] Chemical Sciences/Analytical chemistry, Capillary electrophoresis lipase assay, UPLC/MS molecular characterization of water plant extracts, [CHIM.THER] Chemical Sciences/Medicinal Chemistry, education, TDLFP based on-line enzymatic assay, 02 engineering and technology, [CHIM.THER]Chemical Sciences/Medicinal Chemistry, 01 natural sciences, Biochemistry, Analytical Chemistry, Enzyme catalysis, Hydrolysis, chemistry.chemical_compound, Capillary electrophoresis, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Contactless conductivity detector, Electrochemistry, Environmental Chemistry, [CHIM]Chemical Sciences, Lipase, Spectroscopy, health care economics and organizations, Chromatography, biology, Chemistry, 010401 analytical chemistry, Natural inhibitor screening, Electrophoresis, Capillary, Substrate (chemistry), 021001 nanoscience & nanotechnology, 0104 chemical sciences, MOPS, Kinetics, [CHIM.POLY]Chemical Sciences/Polymers, Spectrophotometry, Dipalmitoylphosphatidylcholine, [SDE]Environmental Sciences, biology.protein, 0210 nano-technology
Abstract

International audience; The search for novel pancreatic lipase (PL) inhibitors has gained increasing attention in recent years. For the first time, a dual detection capillary electrophoresis (CE)-based homogeneous lipase assay was developed employing both the offline and online reaction modes. The hydrolysis of 4-nitrophenyl butyrate (4-NPB) catalyzed by PL into 4-nitrophenol and butyrate was monitored by spectrophotometric and conductimetric detection, respectively. The assays presented several advantages such as economy in consumption (few tens of nanoliters for online assays to few tens of microliters for offline assays), no modification of lipase, rapidity (

Published
2021
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10. Capillary electrophoresis-mass spectrometry at trial by metabo-ring

Author

Marianne Fillet, Cyril Colas, N. Thuy Tran, Erika P. Portero, Meera Shanmuganathan, Jan Nouta, Marton Szigeti, Christopher Lößner, Elena Tobolkina, Herbert Lindner, Peter Nemes, Jens Meixner, Iseult Lynch, J.A. Thorn, Marie-Jia Gou, Nicolas Drouin, Sabrina Ferré, Christian Neusüß, Guinevere S. M. Lageveen-Kammeijer, Zachary Kroezen, Rouba Nasreddine, Ghassan Al Hamoui Dit Banni, Santiago Codesido, Myriam Taverna, András Guttman, Klaus Faserl, Marlien van Mever, Ángeles López Gonzálvez, Wei Zhang, Rawi Ramautar, Claudia Bich-Muracciole, Antony Lechner, Manuel Nelke, Serge Rudaz, Reine Nehmé, Laurent Nyssen, Víctor González-Ruiz, Andrew J. Chetwynd, Stefan Lämmerer, Anne-Catherine Servais, Sylvie Liu, Coral Barbas, Thomas Hankemeier, Catherine Perrin, Yannis François, Philip Britz-McKibbin, Chimie de la matière complexe (CMC), and Université de Strasbourg (UNISTRA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Biomarker identification, Computational chemistry, Metabolite, Interfaces, 010402 general chemistry, Mass spectrometry, 01 natural sciences, Capillary electrophoresis–mass spectrometry, Article, Analytical Chemistry, chemistry.chemical_compound, Electrolytes, Capillary electrophoresis, Metabolomics, Tandem Mass Spectrometry, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Cations, Genetics, Humans, Organic Chemicals, Reproducibility, ddc:615, Chromatography, Chemistry, 010401 analytical chemistry, Electrophoresis, Capillary, Reproducibility of Results, 0104 chemical sciences, Electrophoresis, Metabolism, Metabolome, Databases, Chemical
Abstract

Capillary zone electrophoresis-mass spectrometry (CE-MS) is a mature analytical tool for the efficient profiling of (highly) polar and ionizable compounds. However, the use of CE-MS in comparison to other separation techniques remains underrepresented in metabolomics, as this analytical approach is still perceived as technically challenging and less reproducible, notably for migration time. The latter is key for a reliable comparison of metabolic profiles and for unknown biomarker identification that is complementary to high resolution MS/MS. In this work, we present the results of a Metabo-ring trial involving 16 CE-MS platforms among 13 different laboratories spanning two continents. The goal was to assess the reproducibility and identification capability of CE-MS by employing effective electrophoretic mobility (mu(eff)) as the key parameter in comparison to the relative migration time (RMT) approach. For this purpose, a representative cationic metabolite mixture in water, pretreated human plasma, and urine samples spiked with the same metabolite mixture were used and distributed for analysis by all laboratories. The mu(eff) was determined for all metabolites spiked into each sample. The background electrolyte (BGE) was prepared and employed by each participating lab following the same protocol. All other parameters (capillary, interface, injection volume, voltage ramp, temperature, capillary conditioning, and rinsing procedure, etc.) were left to the discretion of the contributing laboratories. The results revealed that the reproducibility of the mu(eff) for 20 out of the 21 model compounds was below 3.1% vs 10.9% for RMT, regardless of the huge heterogeneity in experimental conditions and platforms across the 13 laboratories. Overall, this Metabo-ring trial demonstrated that CE-MS is a viable and reproducible approach for metabolomics.

Published
2020
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11. Water-Based Extraction of Bioactive Principles from Blackcurrant Leaves and Chrysanthellum americanum: A Comparative Study

Author

Rouba Nasreddine, Reine Nehmé, Ghassan Al Hamoui Dit Banni, Anne-Sylvie Fabiano Tixier, Laurent Leclercq, Phu Cao-Ngoc, Philippe Schmitt-Kopplin, Jasmine Hertzog, Hervé Cottet, Jean-Christophe Rossi, Farid Chemat, Institut des Biomolécules Max Mousseron [Pôle Chimie Balard] (IBMM), Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Institut de Chimie du CNRS (INC)-Université de Montpellier (UM)-Centre National de la Recherche Scientifique (CNRS), Research Unit Analytical BioGeoChemistry (BGC), Helmholtz Zentrum München = German Research Center for Environmental Health, Sécurité et Qualité des Produits d'Origine Végétale (SQPOV), Avignon Université (AU)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut de Chimie Organique et Analytique (ICOA), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université d'Orléans (UO)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Leclercq, Laurent, Helmholtz-Zentrum München (HZM), and Université d'Orléans (UO)-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Institut National de la Santé et de la Recherche Médicale (INSERM)

Subjects
Chrysanthellum americanum, Health (social science), Flavonoid, enzymatic activity, Plant Science, Ribes, lcsh:Chemical technology, 01 natural sciences, Health Professions (miscellaneous), Microbiology, Crataegus, granulometry, [CHIM] Chemical Sciences, [SDV.BBM] Life Sciences [q-bio]/Biochemistry, Molecular Biology, Maceration (wine), ddc:630, Chrysanthellum, [CHIM]Chemical Sciences, lcsh:TP1-1185, flavonoid, [SDV.BBM]Life Sciences [q-bio]/Biochemistry, Molecular Biology, water-based extraction, Medicinal plants, infusion, chemistry.chemical_classification, Chromatography, biology, 010405 organic chemistry, Chemistry, 010401 analytical chemistry, biology.organism_classification, hawthorn, ddc, 0104 chemical sciences, [SDE.BE] Environmental Sciences/Biodiversity and Ecology, polyphenol, Proanthocyanidin, Blackcurrant, Hawthorn, Chrysanthellum Americanum, Water-based Extraction, Polyphenol, Procyanidin, Granulometry, Infusion, Enzymatic Activity, procyanidin, [SDE.BE]Environmental Sciences/Biodiversity and Ecology, blackcurrant, Food Science
Abstract

The water-based extraction of bioactive components from flavonoid-rich medicinal plants is a key step that should be better investigated. This is especially true when dealing with easy-to-use home-made conditions of extractions, which are known to be a bottleneck in the course for a better control and optimization of the daily uptake of active components from medicinal plants. In this work, the water-based extraction of Blackcurrant (Ribes nigrum) leaves (BC) and Chrysanthellum americanum (CA), known to have complementary pharmacological properties, was studied and compared with a previous work performed on the extraction of Hawthorn (Crataegus, HAW). Various extraction modes in water (infusion, percolation, maceration, ultrasounds, microwaves) were compared for the extraction of bioactive principles contained in BC and CA in terms of extraction yield, of amount of flavonoids, phenolic compounds, and proanthocyanidin oligomers, and of UHPLC profiles of the extracted compounds. The qualitative and quantitative aspects of the extraction, in addition to the kinetic of extraction, were studied. The optimized easy-to-use-at-home extraction protocol developed for HAW was found very efficient to easily extract bioactive components from BC and CA plants. UHPLC-ESI-MS and high-resolution Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) were also implemented to get more qualitative information on the specific and common chemical compositions of the three plants (including HAW). Their antihyaluronidase, antioxidant, and antihypertensive activities were also determined and compared, demonstrating similar activities as the reference compound for some of these plants.

Published
2020
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12. Kinetic theory of hyaluronan cleavage by bovine testicular hyaluronidase in standard and crowded environments

Author

Francesco Piazza, Rouba Nasreddine, Lucija Orlic, Chrystel Lopin-Bon, Josef Hamacek, Reine Nehmé, Institut de Chimie Organique et Analytique (ICOA), Université d'Orléans (UO)-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Institut National de la Santé et de la Recherche Médicale (INSERM), Institut de chimie et procédés pour l'énergie, l'environnement et la santé (ICPEES), Université de Strasbourg (UNISTRA)-Matériaux et nanosciences d'Alsace (FMNGE), Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Centre de biophysique moléculaire (CBM), Université d'Orléans (UO)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université d'Orléans (UO)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université de Strasbourg (UNISTRA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Matériaux et Nanosciences Grand-Est (MNGE), Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS), Université d'Orléans (UO)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), and CCSD, Accord Elsevier

Subjects
0301 basic medicine, Male, Reaction mechanism, [SDV]Life Sciences [q-bio], Biophysics, FOS: Physical sciences, Hyaluronoglucosaminidase, Condensed Matter - Soft Condensed Matter, Cleavage (embryo), 01 natural sciences, Biochemistry, Polyethylene Glycols, 03 medical and health sciences, Hydrolysis, Capillary electrophoresis, PEG ratio, Testis, Animals, Fragmentation (cell biology), Hyaluronic Acid, Molecular Biology, ComputingMilieux_MISCELLANEOUS, Enzyme Assays, chemistry.chemical_classification, 010401 analytical chemistry, 0104 chemical sciences, [SDV] Life Sciences [q-bio], Kinetics, 030104 developmental biology, Enzyme, chemistry, Soft Condensed Matter (cond-mat.soft), Cattle, Dimerization, Recombination
Abstract

In this paper, we introduce a comprehensive kinetic model describing the enzymatic cleavage of hyaluronan (HA) by bovine testicular hyaluronidase (BTH). Our theory focuses specifically on the late stage of the hydrolysis, where the concentrations of a limited number of oligomers may be determined experimentally with accuracy as functions of time. The present model was applied to fit different experimental sets of kinetic data collected by capillary electrophoresis at two HA concentrations and three concentrations of PEG crowder (0, 10, 17% w/w). Our theory seems to apply universally, irrespective of HA concentration and crowding conditions, reproducing to an excellent extent the time evolution of the individual molar fractions of oligomers. Remarkably, we found that the reaction mechanism in the late degradation stage essentially reduces to the cleavage or transfer of active dimers. While the recombination of dimers is the fastest reaction, the rate-limiting step turns out to be invariably the hydrolysis of hexamers. Crowding, HA itself or other inert, volume-excluding agents, clearly boosts recombination events and concomitantly slows down all fragmentation pathways. Overall, our results bring a novel and comprehensive quantitative insight into the complex reaction mechanism underlying enzymatic HA degradation. Importantly, rationalizing the effect of crowding not only brings the intricate conditions of in-vivo settings a little closer, but also emerges as a powerful tool to help pinpointing relevant kinetic pathways in complex systems.

Published
2020
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13. Polyethylene glycol crowding effect on hyaluronidase activity monitored by capillary electrophoresis

Author

Rouba Nasreddine, Josef Hamacek, Reine Nehmé, Lucija Orlic, Ghassan Al Hamoui Dit Banni, Francesco Piazza, Axel Marchal, Syntia Fayad, Chrystel Lopin-Bon, Institut de Chimie Organique et Analytique (ICOA), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université d'Orléans (UO)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Centre de biophysique moléculaire (CBM), Université d'Orléans (UO)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Center for Advanced Studies and Research in Information and Communication Technologies & Society (ICT&S Center), University of Salzburg, ANR-11-LABX-0029,SYNORG,Synthèse Organique : des molécules au vivant(2011), Université d'Orléans (UO)-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Institut National de la Santé et de la Recherche Médicale (INSERM), Université d'Orléans (UO)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), Frapart, Isabelle, and Synthèse Organique : des molécules au vivant - - SYNORG2011 - ANR-11-LABX-0029 - LABX - VALID

Subjects
Male, [SDV]Life Sciences [q-bio], Hyaluronoglucosaminidase, 02 engineering and technology, Polyethylene glycol, Polysaccharide, 01 natural sciences, Biochemistry, Polyethylene Glycols, Analytical Chemistry, Capillary electrophoresis, chemistry.chemical_compound, Hydrolysis, Hyaluronidase, Testis, PEG ratio, Hyaluronic acid, medicine, Hyaluronidase activity, Animals, Hyaluronic Acid, [SDV.BBM.BC]Life Sciences [q-bio]/Biochemistry, Molecular Biology/Biochemistry [q-bio.BM], [SDV.BBM.BC] Life Sciences [q-bio]/Biochemistry, Molecular Biology/Biochemistry [q-bio.BM], Enzyme Assays, chemistry.chemical_classification, Chromatography, Inhibitors, 010401 analytical chemistry, Electrophoresis, Capillary, 021001 nanoscience & nanotechnology, 0104 chemical sciences, [SDV] Life Sciences [q-bio], Kinetics, Enzyme, Crowding, chemistry, Cattle, 0210 nano-technology, medicine.drug
Abstract

International audience; To mimic the activity of hyaluronidase in natural environment, the hydrolysis of hyaluronic acid (HA) by hyaluronidase was investigated for the first time in the presence of crowding agents using capillary electrophoresis (CE) as a simple and reliable technique for conducting enzymatic assay. Polyethylene glycol (PEG) 6000 was selected as a model crowder and the hyaluronic acid degradation catalyzed by bovine testes hyaluronidase (BTH) was carried out at different PEG concentrations (0%, 10%, and 17%). After optimization of the CE analytical method and enzymatic assay, the degradation products were monitored at different HA concentrations. At 10% of PEG and 0.3 mg mL−1 of HA, the activity of the enzyme was significantly reduced showing inconvenient interactions of PEG with the hyaluronidase blocking the release of hydrolysis products. A similar reduction of hyaluronidase activity was observed at 1 mg mL−1 of HA due to the presumable formation of the BTH-substrate complex. The experimental curves obtained by CE also evidence that the overall kinetics are governed by the hydrolysis of hexasaccharide intermediates. Finally, the effect of PEG on hyaluronidase activity was evaluated in the presence of natural or synthetic inhibitors. Our results show a significant difference of the inhibitors’ affinity toward hyaluronidase in the presence of PEG. Surprisingly, the presence of the crowding agent results in a loss of the inhibition effect of small polycyclic inhibitors, while larger charged inhibitors were less affected. In this work, CE analyses confirm the importance of mimicking the cellular environment for the discovery and development of reliable inhibitors.

Published
2020
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14. Microscale thermophoresis for studying protein-small molecule affinity: Application to hyaluronidase

Author

Reine Nehmé and Rouba Nasreddine

Subjects
chemistry.chemical_classification, Chromatography, Chemistry, Microscale thermophoresis, Substrate (chemistry), Small molecule, Fluorescence, Analytical Chemistry, Dissociation constant, Enzyme, Pulmonary surfactant, Hyaluronidase, medicine, Spectroscopy, medicine.drug
Abstract

Studying the binding affinity between large biomolecules (i.e. enzyme) and small molecules (molecular weight less than 1000 Da) is an extremely challenging task when using conventional techniques because of the difficulty associated with the detection of the minuscule variations caused by the binding. Microscale thermophoresis (MST) is a sensitive novel emerging biophysical tool allowing a rapid and accurate determination of the dissociation constant (Kd) of enzyme - small molecule system. For the first time, a systematic MST study was carried out to evaluate Kd between hyaluronidase (Hyal), a model enzyme, and two small flavonoid compounds known as potent Hyal's inhibitors, epigallocatechin gallate (EGCG) and apigenin-7-glucoside. In the optimized conditions, hyaluronidase fluorescent labelling (Hyal*) was achieved by direct labelling with RED-NHS NT647 dye using a phosphate ammonia buffer (20 mM NaH2PO4 + 50 mM NH3) + 77 mM NaCl at pH 6.6. This latter ensured a high labelling efficiency while preventing Hyal* precipitation (pI of hyaluronidase is equal to 8.6). Pre-capillary CE/UV enzymatic assays of Hyal* demonstrated the preservation of its enzymatic activity even though the tested concentration was very low (50-fold times lower than control enzymatic assay). Fluorescence signal intensity and shape as well as MST traces have shown that phosphate ammonia buffer required the addition of surfactant, Tween-20 at 0.05%, to efficiently improve the protein solubility and limited aggregate formation using standard uncoated capillaries. MST results revealed the absence of affinity between Hyal* and the tested flavonoids regardless of the incubation time and the tested inhibitory concentration range unless the hyaluronidase substrate, hyaluronic acid (HA) is added to the preparation. Kd values were estimated to be 163 µM for Hyal*/HA/EGCG and 157 µM for Hyal*/HA/apigenin-7-glucoside. The repeatability of the assays was excellent as confirmed by the very low standard deviation on Kd values.

Published
2021
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15. VOC tracers from aircraft activities at Beirut Rafic Hariri International Airport

Author

Jocelyne Adjizian Gerard, Rouba Nasreddine, Claire Trocquet, Tharwat Mokalled, Vincent Person, Maher Abboud, Stéphane Le Calvé, Université Saint-Joseph de Beyrouth (USJ), In’Air Solutions [Strasbourg, France], Institut de chimie et procédés pour l'énergie, l'environnement et la santé (ICPEES), Université de Strasbourg (UNISTRA)-Matériaux et nanosciences d'Alsace (FMNGE), and Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Engine power, [SDU.OCEAN]Sciences of the Universe [physics]/Ocean, Atmosphere, Atmospheric Science, Kerosene, Future studies, 010504 meteorology & atmospheric sciences, Environmental engineering, 010501 environmental sciences, 01 natural sciences, Pollution, International airport, Ambient air, 13. Climate action, Auxiliary power unit, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, [SDE]Environmental Sciences, Environmental science, [CHIM]Chemical Sciences, Takeoff, Waste Management and Disposal, Air quality index, ComputingMilieux_MISCELLANEOUS, 0105 earth and related environmental sciences
Abstract

This is the first study to assess the speciation of 48 VOCs from around 100 commercial aircraft under real operation, as close as possible to aircraft engines during the various modes of the landing/takeoff (LTO) cycles to identify special aircraft fingerprints and markers. Also, Jet A-1 kerosene vapor, gasoline exhaust, and the ambient airport concentrations were assessed. Air samples were taken at Beirut Rafic Hariri International Airport inside adsorbent tubes using a portable automatic remote sampler and analyzed using gas chromatographic techniques (GC-MS and GC-FID). Results showed that heavy alkanes (C8-C14, mainly n-nonane and n-decane), which contributed to about 51–64% of the total mass of heavy VOCs emitted by aircraft, and heavy aldehydes (nonanal and decanal) – although to a lesser amount – can be considered as potential tracers for aircraft emissions due to both their exclusive presence in aircraft-related emissions and their absence from gasoline exhaust emissions. On the other hand, the total concentration of heavy alkanes in the airport's ambient air was 47% of the total mass of heavy VOCs measured. No aircraft tracer was identified among the light VOCs (≤C7); however, results showed that emissions of light VOCs decrease as the engine power increases. Also, auxiliary power unit (APU) emissions were identified to be of the same order of magnitude as main engine emissions. This study opens the door for future studies aiming at evaluating the impact of airport activities on air quality and human health within or away from the airport vicinity.

Published
2019
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16. Development of a novel portable miniaturized GC for near real-time low level detection of BTEX

Author

Vincent Person, Rouba Nasreddine, Stéphane Le Calvé, Christophe A. Serra, Institut Charles Sadron (ICS), Université de Strasbourg (UNISTRA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Réseau nanophotonique et optique, Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Matériaux et nanosciences d'Alsace (FMNGE), Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS), Animal et gestion intégrée des risques (UPR AGIRs), and Centre de Coopération Internationale en Recherche Agronomique pour le Développement (Cirad)

Subjects
Analytical chemistry, PID controller, 02 engineering and technology, BTEX, 01 natural sciences, Ethylbenzene, chemistry.chemical_compound, Materials Chemistry, [SPI.GPROC]Engineering Sciences [physics]/Chemical and Process Engineering, Electrical and Electronic Engineering, Benzene, Instrumentation, Detection limit, Chromatography, Chemistry, 010401 analytical chemistry, Detector, Metals and Alloys, Repeatability, 021001 nanoscience & nanotechnology, Condensed Matter Physics, 0104 chemical sciences, 3. Good health, Surfaces, Coatings and Films, Electronic, Optical and Magnetic Materials, Volumetric flow rate, 0210 nano-technology
Abstract

This paper reports on the development and optimization of a miniaturized GC/PID system dedicated to BTEX monitoring in near-real time conditions at ppb level. The system consists of a 6-ports valve, a capillary column and a mini-photoionization detector (PID), its final weight is around 4 kg. The system operates at very low flow rate (lower than 4 mL min−1) irrespective of the carrier gas used. The device is controlled through homemade software which provides instrument control and real-time chromatograms collection. The system's performance was studied and optimized with two different carrier gases, namely hydrogen and nitrogen. The optimal experimental conditions of BTEX separation was determined according to the calculated H.E.T.P. and the total analysis time for a single run which was set to a maximum of 10 min. Using the optimal conditions, the detection limit, stability and repeatability of the analytical system were assessed. A detection limit of 1 ppb was found for benzene and toluene with both carrier gases and less than 3 ppb for other compounds of the family. A slight advantage in terms of separation was found with hydrogen especially for ethylbenzene and xylenes using the defined experimental conditions.

Published
2016
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17. Portable novel micro-device for BTEX real-time monitoring: Assessment during a field campaign in a low consumption energy junior high school classroom

Author

Vincent Person, Rouba Nasreddine, Christophe A. Serra, Coralie Schoemaecker, Stéphane Le Calvé, Institut Charles Sadron (ICS), Université de Strasbourg (UNISTRA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Réseau nanophotonique et optique, Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Matériaux et nanosciences d'Alsace (FMNGE), Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS), Animal et gestion intégrée des risques (UPR AGIRs), and Centre de Coopération Internationale en Recherche Agronomique pour le Développement (Cirad)

Subjects
Atmospheric Science, Engineering, Spectrum analyzer, Continuous operation, business.industry, School classroom, 010401 analytical chemistry, Environmental engineering, Time resolution, Natural ventilation, 02 engineering and technology, BTEX, 021001 nanoscience & nanotechnology, 01 natural sciences, 0104 chemical sciences, law.invention, law, Ventilation (architecture), [SPI.GPROC]Engineering Sciences [physics]/Chemical and Process Engineering, 0210 nano-technology, business, Field campaign, General Environmental Science
Abstract

A novel micro-device was deployed during an indoor field campaign to validate and demonstrate its ability to highlight rapid changes of atmospheric BTEX concentrations. The field campaign was carried out in a junior high school recently built respecting the thermal regulation of 2005 and equipped with a modern ventilation. BTEX concentrations were continuously measured using the novel micro-device and a commercial analyzer for two weeks during the winter holidays, both operating with a time resolution of 10 min. Toluene appeared to be the major VOC inside the investigated classroom. Its concentration varied between 1 and 18 ppb and was strongly correlated with the room ventilation status. This latter was partially programmed to mimic the school period. In order to compare the efficiency of the ventilation with natural ventilation, the windows were opened for 1 h when the ventilation was OFF. In all tested conditions, the toluene concentrations measured with our new micro-device were in very good agreement with those provided by the commercial BTEX analyzer. In addition, punctual short calibrations were performed during the campaign for both instruments (after 4 days and 9 days). Results showed that our micro-GC was more stable (gap less than 15% after 9 days) while the commercial analyzer required regular calibrations because of the loose of 60% of its sensitivity after 9 days of continuous operation. Therefore, our micro-device, of about 3 kg and fully controlled by homemade software, appears to be suitable to monitor BTEX concentrations higher than 1 ppb in near real time.

Published
2016
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18. BTEX near real-time monitoring in two primary schools in La Rochelle, France

Author

Stéphanette Englaro, Irene Lara-lbeas, Béatrice Cormerais, Rouba Nasreddine, Christina Andrikopoulou, Vincent Person, Stéphane Le Calvé, Claire Trocquet, In’Air Solutions [Strasbourg, France], Institut de chimie et procédés pour l'énergie, l'environnement et la santé (ICPEES), Université de Strasbourg (UNISTRA)-Matériaux et nanosciences d'Alsace (FMNGE), Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Le Calvé, Stéphane, Université de Strasbourg (UNISTRA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Matériaux et Nanosciences Grand-Est (MNGE), and Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Atmospheric Science, Portable device, 010504 meteorology & atmospheric sciences, Health, Toxicology and Mutagenesis, Real-time computing, real-time, BTEX, 010501 environmental sciences, Management, Monitoring, Policy and Law, 01 natural sciences, Ethylbenzene, [PHYS.PHYS.PHYS-AO-PH] Physics [physics]/Physics [physics]/Atmospheric and Oceanic Physics [physics.ao-ph], law.invention, chemistry.chemical_compound, law, toluene, Benzene, Field campaign, 0105 earth and related environmental sciences, [PHYS.PHYS.PHYS-AO-PH]Physics [physics]/Physics [physics]/Atmospheric and Oceanic Physics [physics.ao-ph], 4. Education, Time resolution, Pollution, [SDE.BE] Environmental Sciences/Biodiversity and Ecology, Real time, chemistry, [CHIM.OTHE] Chemical Sciences/Other, CO2 levels, Ventilation (architecture), indoor air schools, Environmental science, Toluene Indoor air schools, [SDE.BE]Environmental Sciences/Biodiversity and Ecology, [CHIM.OTHE]Chemical Sciences/Other
Abstract

International audience; The present field campaign was conducted in two French primary schools for 5 weeks, where the experimental conditions were modified every week. During the first week, the classrooms were empty and not occupied, whereas the furniture was added the second week. For the three last weeks, the classrooms were normally occupied by students and various scenarios of ventilation were applied. BTEX concentrations were monitored by using novel portable pre-industrial prototypes with low gas and energy consumption, which worked continuously and operated in near real time with a time resolution of 10 min. The BTEX concentrations were compared to CO2 measurements since the latter is commonly considered as a confinement indicator. In both schools, BTEX were not detected during the absence of students indicating that neither building materials nor furniture emit such compounds. Once the schools occupied by students, BTEX have been detected from time to time, and their concentrations ranged as follows: 0–12 ppb (benzene); 0–29 ppb (toluene), 0–4 ppb (ethylbenzene), 0–11 ppb (m/p-xylenes), and 0–10 ppb (o-xylene) excluding huge values due to paint emissions in one of the schools. Toluene was found to be strongly correlated to high levels of CO2, showing that it was emitted by internal students activities scheduled at the end of mornings. On the contrary, benzene peak was not correlated to high values of CO2, suggesting that it comes from external sources.

Published
2018
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19. Experimental performances study of a transportable GC-PID and two thermo-desorption based methods coupled to FID and MS detection to assess BTEX exposure at sub-ppb level in air

Author

Ngoc Tinh Nguyen, C. Liaud, S. Le Calvé, Rouba Nasreddine, In’Air Solutions [Strasbourg, France], Institut d'Électronique et des Technologies du numéRique (IETR), Nantes Université (NU)-Université de Rennes 1 (UR1), Université de Rennes (UNIV-RENNES)-Université de Rennes (UNIV-RENNES)-Institut National des Sciences Appliquées - Rennes (INSA Rennes), Institut National des Sciences Appliquées (INSA)-Université de Rennes (UNIV-RENNES)-Institut National des Sciences Appliquées (INSA)-CentraleSupélec-Centre National de la Recherche Scientifique (CNRS), Centre de géochimie de la surface (CGS), Institut national des sciences de l'Univers (INSU - CNRS)-Université Louis Pasteur - Strasbourg I-Centre National de la Recherche Scientifique (CNRS), Université de Nantes (UN)-Université de Rennes (UR)-Institut National des Sciences Appliquées - Rennes (INSA Rennes), Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-CentraleSupélec-Centre National de la Recherche Scientifique (CNRS), and Université de Nantes (UN)-Université de Rennes 1 (UR1)

Subjects
Chromatography, Gas, 010504 meteorology & atmospheric sciences, GC-PID, Analytical chemistry, BTEX, Xylenes, 010501 environmental sciences, Mass spectrometry, Analytical method, 01 natural sciences, Analytical Chemistry, law.invention, chemistry.chemical_compound, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Limit of Detection, law, Benzene Derivatives, Flame ionization detector, Benzene, 0105 earth and related environmental sciences, [SDU.OCEAN]Sciences of the Universe [physics]/Ocean, Atmosphere, Detection limit, Air Pollutants, Chromatography, [SDE.IE]Environmental Sciences/Environmental Engineering, Chemistry, Repeatability, 13. Climate action, Calibration, Thermo-desorption Highlights, Adsorption, Gas chromatography, GC-MS, Gas chromatography–mass spectrometry, GC-FID, Environmental Monitoring, Toluene
Abstract

BTEX compounds are of particular interest, above all benzene because it is a carcinogenic compound for which guideline value in European indoor environments is set to be 1.6 ppb. Therefore, the detection of such relatively low value requires the use of particularly sensitive analytical techniques. Several existing chromatographic techniques, such as fast and transportable Gas Chromatograph with Photoionization Detection (GC-PID) or sedentary chromatographic-based techniques equipped with a thermo-desorption device (ATD) and coupled to either Flame Ionization Detection (FID) or Mass Spectrometry (MS), can quantify benzene and its derivatives at such low levels. These instruments involve different injection modes, i.e. on-line gaseous sampling or thermo-desorption of adsorbent tubes spiked with liquid or gas samples. In this study, the performances of 3 various analytical techniques mentioned above were compared in terms of sensitivity, linearity, accuracy and repeatability for the 6 BTEX. They were also discussed related to their analyses time consumption or transportability. The considered analytical techniques are ATD–GC–FID, ATD–GC–MS where both full scan and SIM modes were tested and a transportable GC-PID. For benzene with on-line injection, Limits of Detection (LOD) were significantly below the European guideline with values of 0.085, 0.022, 0.007 and 0.058 ppb for ATD–GC–FID, ATD–GC–MS in a full scan mode, ATD–GC–MS in an SIM mode and transportable GC-PID, respectively. LOD obtained with adsorbent tubes spiked with liquid standards were approximately in the same order of magnitude.

Published
2014
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