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Synthesis and characterization of molecularly imprinted polymers for the selective extraction of oxazepam from complex environmental and biological samples
Fanny Varenne, Porkodi Kadhirvel, Pauline Bosman, Loïc Renault, Audrey Combès, Valérie Pichon
Anal. Bioanal. Chem - - doi: 10.1007/s00216-021-03268-w. - 2021
Oxazepam, one of the most frequently prescribed anxiolytic drugs, is not completely removed from wastewater with conventional treatment processes. It can thus be found at trace levels in environmental water, with human urine constituting the major source of contamination. This study focused on the development and characterization of molecularly imprinted polymers (MIPs) for the selective solid-phase extraction of oxazepam at trace levels from environmental water and human urine samples. Two MIPs were synthesized, and their selectivity in pure organic and aqueous media were assayed. After optimizing the extraction procedure adapted to a large sample volume to reach a high enrichment factor, the most promising MIP was applied to the selective extraction of oxazepam from environmental water. Extraction recoveries of 83 ± 12, 92 ± 4 and 89 ± 10% were obtained using the MIP for tap, mineral and river water, respectively, while a recovery close to 40% was obtained on the corresponding non-imprinted polymer (NIP). Thanks to the high enrichment factors, a limit of quantification (LOQ) of 4.5 ng L-1 was obtained for river water. A selective extraction procedure was also developed for urine samples and gave rise to extraction recoveries close to 95% for the MIP and only 23% for the NIP. Using the MIP, a LOQ of 357 ng L-1 was obtained for oxazepam in urine. The use of the MIP also helped to limit the matrix effects encountered for the quantification of oxazepam in environmental samples and in human urine samples after extraction on an Oasis HLB sorbent.

Identification and semi-relative quantification of intact glycoforms of human chorionic gonadotropin alpha and beta subunits by nano liquid chromatography-Orbitrap mass spectrometry
AmiraAl Matari, Anastasia Goumenou, Audrey Combèsa, Thierry Fournier, Valérie Pichon, Nathalie Delaunay
J. Chromatography A - 1640 461945 - doi.org/10.1016/j.chroma.2021.461945 - 2021
The human chorionic gonadotropin (hCG) protein belongs to a family of glycoprotein hormones called gonadotropins. It is a heterodimer made of two non-covalently linked subunits. The α-subunit structure, hCGα, has 2 N-glycosylation sites, while the beta subunit, hCGβ, has 2 N- and 4 O-glycosylation sites. This leads to numerous glycoforms. A method based on the analysis of hCG glycoforms at the intact level by nano-reversed phase liquid chromatography coupled to high resolution mass spectrometry (nanoLC-HRMS) with an Orbitrap analyzer was previously developed using a recombinant hCG-based drug, Ovitrelle®, as standard. It allowed the detection of about 30 hCGα glycoforms, but didn't allow the detection of hCGβ glycoforms. This method was thus here significantly modified (addition of a pre-concentration step of the sample to increase the sample volume from 70 nl to 1 µl, optimization of the gradient slope and the nature and content of the acidic additive in the mobile phase). It led to an improvement of the separation of hCGα and hCGβ glycoforms, which allowed for the first time the detection of 33 hCGβ glycoforms at intact level. In addition, a higher number of hCGα glycoforms (42 in total, i.e. a 40% increase) was detected. The figures of merit of this new method were next assessed. The relative standard deviations (RSDs) of the retention time ranged between 0.02 and 0.95% (n = 3), with an average value of 0.36% for the alpha glycoforms and between 0.01 and 1.08% (n = 3) with an average value of 0.23% for the beta glycoforms. The RSDs of the relative peak area measured on the extracted ion chromatogram of each glycoform were below 20% (n = 3), with an average value of 9.8%, thus allowing semi-relative quantification. Therefore, this method has a high potential for rapid quality control aiming for the detection and comparison of glycoforms present in glycoprotein-based pharmaceutical preparations.


Development of a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the analysis of tryptic digest of human hemoglobin exposed to sulfur mustard
Florine Hallez, Audrey Combès, Charlotte Desoubries, Anne Bossée, Valérie Pichon
J. Chromatography A - 1163 122518 - doi.org/10.1016/j.jchromb.2020.122518 - 2021
Sulfur mustard is a highly reactive chemical warfare agent that causes severe damages to the victims exposed by alkylating multiple biomolecules such as proteins. Resulting alkylated products can be used as biomarkers of exposure to this chemical agent. A liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) method was thus developed to detect alkylated peptides after the tryptic digestion of hemoglobin (50 mg.mL−1) incubated with sulfur mustard at different concentrations (0.25, 0.5, 1, 10 and 100 µg.mL−1). Five new alkylation sites were accurately identified on the protein (α-His72, α-His87, α-His89, β-His2 and β-Val98) and fifteen adducted peptides were detected, among which eight of them resulted from the alkylation of four peptides, each presenting two potential sites of adduction that could be discriminated by the method specificity. Similarly, it was possible to discriminate the three potential adduction sites of the peptide α-T9. Moreover, the method allowed the quantification of all the alkylated peptides with a satisfying repeatability, with RSD ranging from 0.5 to 9.3% for an exposure of hemoglobin to sulfur mustard at 100 µg.mL−1. The analysis of hemoglobin incubated with different concentrations of sulfur mustard levels led to a linear response for all the alkylated peptides with the studied concentrations (0.25, 0.5, 1, 10 and 100 µg.mL−1). A variation of the alkylation rate was also observed between the different peptides studied, with a preferential adduction of sulfur mustard on the histidine residues but also on the N-terminal valine residues of both globin chains and on the Val98 residue of globin β. Furthermore, the presented method proved to be sensitive, with a theoretical possibility to detect alkylated peptides resulting from in vitro incubation of hemoglobin in deionized water with sulfur mustard at 2.63 ng.mL−1. After further development, this method could potentially be used for the analysis of blood samples in vivo exposed to sulfur mustard.



COVID-19 and Dentistry in 72 Questions: An Overview of the Literature
Stéphane Derruau, Jérôme Bouchet, Ali Nassif, Alexandre Baudet, Kazutoyo Yasukawa, Sandrine Lorimier, Isabelle Prêcheur, Agnès Bloch-Zupan, Bernard Pellat, Hélène Chardin
J. Clin. Med. - 10 122518 - 4 - 2021
The outbreak of Coronavirus Disease 2019 (COVID-19), caused by Severe Acute Respiratory Syndrome Coronavirus 2 (SARS-CoV-2), has significantly affected the dental care sector. Dental professionals are at high risk of being infected, and therefore transmitting SARS-CoV-2, due to the nature of their profession, with close proximity to the patient’s oropharyngeal and nasal regions and the use of aerosol-generating procedures. The aim of this article is to provide an update on different issues regarding SARS-CoV-2 and COVID-19 that may be relevant for dentists. Members of the French National College of Oral Biology Lecturers (“Collège National des EnseignantS en Biologie Orale”; CNESBO-COVID19 Task Force) answered seventy-two questions related to various topics, including epidemiology, virology, immunology, diagnosis and testing, SARS-CoV-2 transmission and oral cavity, COVID-19 clinical presentation, current treatment options, vaccine strategies, as well as infection prevention and control in dental practice. The questions were selected based on their relevance for dental practitioners. Authors independently extracted and gathered scientific data related to COVID-19, SARS-CoV-2 and the specific topics using scientific databases. With this review, the dental practitioners will have a general overview of the COVID-19 pandemic and its impact on their practice. View Full-Text



Molecularly imprinted polymers in miniaturized extraction and separation devices
Thomas Bouvarel, Nathalie Delaunay, Valérie Pichon
First published - 44(8) 1727-1751 - doi.org/10.1002/jssc.202001223 - 2021
Molecularly imprinted polymers are highly selective and cost-effective materials, which have attracted significant interest in various areas such as sample pretreatment and chromatographic and electrophoretic separations. This review aims to present the state of the art concerning the miniaturization of these materials in order to meet the societal demand for reliable, fast, cheap, and solvent/sample saving analyses. The polymerization route specificities for the production of miniaturized molecularly imprinted polymers in capillaries or chip channels, such as open tubular, packed particles, magnetic nanoparticles, and in situ imprinted monoliths, are investigated. Their performances as selective supports in solid phase extraction and as stationary phases in electrochromatography and liquid chromatography, as well as their possible perspectives are discussed.




Reversible Supra-Folding of User-Programmed Functional DNA Nanostructures on Fuzzy Cationic Substrates
Koyomi Nakazawa, Farah El Fakih, Vincent Jallet, Caroline Rossi-Gendron, Marina Mariconti, Léa Chocron, Mafumi Hishida, Kazuya Saito, Mathieu Morel, Sergii Rudiuk, Damien Baigl
Angew Chem Int Ed Engl - - DOI: 10.1002/anie.202101909 - 2021
We report that user-defined DNA nanostructures, such as two-dimensional (2D) origamis and nanogrids, undergo a rapid higher-order folding transition, referred to as supra-folding, into three-dimensional (3D) compact structures (origamis) or well-defined μm-long ribbons (nanogrids), when they adsorb on a soft cationic substrate prepared by layer-by-layer deposition of polyelectrolytes. Once supra-folded, origamis can be switched back on the surface into their 2D original shape through addition of heparin, a highly charged anionic polyelectrolyte known as an efficient competitor of DNA-polyelectrolyte complexation. Orthogonal to DNA base-pairing principles, this reversible structural reconfiguration is also versatile; we show in particular that 1) it is compatible with various origami shapes, 2) it perfectly preserves fine structural details as well as site-specific functionality, and 3) it can be applied to dynamically address the spatial distribution of origami-tethered proteins.
Withdrawal and dip coating of an object from a yield-stress reservoir
Wilbert J. Smit, Christophe Kusina, Annie Colin, Jean-François Joanny
Physical Review Fluids - 6(6) - DOI:10.1103/PhysRevFluids.6.063302 - 2021
The dip-coating process consists of withdrawing immersed objects from a liquid reservoir. After withdrawal, a significant layer of liquid remains on the object. Various industrial processes (food and beverage industry, automotive industry) use this technique to coat or treat surfaces. Recent studies have shown that the thickness of deposit is determined by the flow inside the reservoir for yield-stress fluids. This is different from the behavior of simple liquids for which the coating thickness is solely determined by the flow inside the meniscus. In this work, we reexamine this question and propose a complete phase diagram linking the Newtonian case and the yield-stress fluid case. We provide asymptotic scaling laws for extreme cases. A good agreement with experiments is obtained.
A new pressure sensor array for normal stress measurement in complex fluids
Anaïs Gauthiera, Mickaël Pruvost, Olivier Gamache, and Annie Colin
Journal of Rheology - 65 583 - doi.org/10.1122/8.0000249 - 2021
A new pressure sensor array, positioned on the bottom plate of a standard torsional rheometer, is presented. It is built from a unique piezo-capacitive polymeric foam and consists of 25 capacitive pressure sensors (of surface 4.5×4.5mm2 each) built together in a 5×5 regular array. The sensor array is used to obtain a mapping of the normal stresses in complex fluids, which dramatically extends the capability of the rheometer. We demonstrate this with three examples. First, a pressure profile is reconstructed in a polymer solution, which enables the simultaneous measurement of the first and the second normal stress differences N1 and N2, with a precision of 2 Pa. In a second part, we show that negative pressures can also be measured. Finally, we focus on the normal stress fluctuations that extend both spatially and temporally in a shear-thickening suspension of cornstarch particles. We evidence the presence of a unique heterogeneity rotating very regularly. In addition to their low cost and high versatility, the sensors show here their potential to finely characterize the normal stresses in viscosimetric flows.
Aging of cornstarch particles suspended in aqueous solvents at room temperature
Christophe Kusina, Wilbert J. Smit, Jean-Baptiste Boitte, Odile Aubrun, and Annie Colin
Phys. Rev. - 103 052609 - doi.org/10.1103/PhysRevE.103.052609 - 2021
Starch suspensions are often used as model systems to demonstrate extreme shear-thickening effects. We study the aging of cornstarch particles in aqueous suspensions at room temperature by granulometry and rheological measurements. When starch is diluted in glycerol, no long-term changes are observed. The situation differs when water is used as solvent. For volume fractions up to 20 vol %, when the cornstarch suspensions in water are stored under continual agitation, we observe an increase in viscosity. When the cornstarch suspension is aged under quiescent conditions, no evolution of the particle size is observed. In the concentrated situation, the rheological properties vary independent of the storage condition. We show that the increase in viscosity is related to air trapped in the pore space and to the swelling of the granules and leakage of the amylopectin component of the starch into the surrounding water. The relative importance of the two processes depends upon the particle concentration and upon the energy brought to the system
Highly conductive colloidal carbon based suspension for flow-assisted electrochemical systems
Marco S. Alfonso, Hélène Parant, Jinkai Yuan, Wilfrid Neri, Eric Laurichesse, Katerina Kampioti, Annie Colin, PhilippePoulin
Iscience - 24(5) 102456 - doi.org/10.1016/j.isci.2021.102456 - 2021
Carbon suspension electrodes are promising for flow-assisted electrochemical energy storage systems. They serve as flowable electrodes in electrolyte solutions of flow batteries, or flow capacitors. They can also be used for other applications such as capacitive deionization of water. However, developments of such suspensions remain challenging. The suspensions should combine low viscosity and high electronic conductivity for optimized performances. In this work, we report a flowable aqueous carbon dispersion which exhibits a viscosity of only 2 Pa.s at a shear rate of 5 s−1 for a concentration of particles of 7 wt%. This suspension displays an electronic conductivity of 65 mS/cm, nearly two orders of magnitude greater than previously investigated related materials. The investigated suspensions are stabilized by sodium alginate and arabic gum in the presence of ammonium sulfate. Their use in flowable systems for the storage and discharge of electrical charges is demonstrated.

635 publications.