Article
Chemistry, Multidisciplinary
Achille Marchand, Rituraj Mishra, Aurelie Bernard, Jean-Nicolas Dumez
Summary: Online monitoring by flow NMR spectroscopy is a powerful tool for studying chemical reactions and processes, providing mechanistic understanding and driving optimizations. However, some useful methods for mixture analysis and reaction monitoring are not directly applicable in flow conditions. In this study, a fast and flow-compatible diffusion NMR experiment is described, allowing accurate diffusion data to be collected for samples flowing at up to 3 mL/min. This one-shot flow-compatible diffusion NMR opens up new possibilities for reaction monitoring applications.
CHEMISTRY-A EUROPEAN JOURNAL
(2022)
Article
Medicine, Research & Experimental
Manreet Kaur, Vanessa Yardley, Ke Wang, Jinit Masania, Adolfo Botana, Randolph R. J. Arroo, Mingzhong Li
Summary: The study aims to explore the formulation of ART cocrystals as oral dosage forms to enhance bioavailability, with results showing significant increase in solubility. PVP-VA was identified as the most effective crystallization inhibitor among a set of polymers, providing crucial information for formulation development. Experiments on the dissolution performance and bioavailability of ART cocrystals with excipients offered valuable insights into their effects.
MOLECULAR PHARMACEUTICS
(2021)
Article
Chemistry, Multidisciplinary
Andrey V. Shibaev, Alexander S. Ospennikov, Elizaveta K. Kuznetsova, Alexander I. Kuklin, Teimur M. Aliev, Valentin V. Novikov, Olga E. Philippova
Summary: This study investigates the effects of solubilizing hydrophobic and hydrophilic substances on the rheological properties and structure of wormlike surfactant micelles. The findings reveal that hydrophobic additives are completely solubilized inside the micelles, while only a small fraction of hydrophilic additives penetrate the micelles. Despite the differences in localization, both types of additives induce the breaking of micelles, resulting in a drop in viscosity.
Article
Biochemical Research Methods
Lori Manoukian, Jose A. Correa, Robin S. Stein, Dominic Frigon, Sidney Omelon
Summary: Inorganic polyphosphates (polyPs) are present in both eukaryotic and prokaryotic cells. This study optimized extraction methods for the identification and measurement of polyPs. The results showed that extraction processes reduced polyP migration and dispersion, leading to a potential overestimation of synthetic polyP chain length.
Article
Biochemistry & Molecular Biology
Matteo Zecchini, Robert A. Lucas, Cameron Robertson, Tomris Coban, Ravtej Thatti, Adam Le Gresley
Summary: This study investigated the UV-induced oligomerisation of squalene and its potential impact on the rheology of biological systems. The molecular weight range was determined using DOSY NMR and validated with ASAP TOF MS. Results showed that the wavelength and time of UV exposure influenced the formation of oligomers, and the cross oligomerisation of squalene with free fatty acids resulted in higher molecular weight distribution. However, rheological changes did not affect diffusion.
Article
Agriculture, Multidisciplinary
Wannes L. De Man, Ewoud Vaneeckhaute, Niels De Brier, Arno G. B. Wouters, Johan A. Martens, Eric Breynaert, Jan A. Delcour
Summary: The structural heterogeneity of water-extractable arabinoxylan (WE-AX) impacts wheat flour functionality, as revealed by H-1 diffusion-ordered (DOSY) nuclear magnetic resonance (NMR) spectroscopy. Different subpopulations within WE-AX fractions have varying diffusion rates, with high self-diffusivity subpopulations containing high levels of monosubstituted xylose and low self-diffusivity subpopulations rich in disubstituted xylose.
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
(2021)
Article
Biochemistry & Molecular Biology
Yu-Lin You, Fei-Fei Li, Ning Wang, Shu-Qi Wang
Summary: DOSY is a powerful tool for investigating mixtures, but similar diffusion coefficients of components can limit resolution. This study used matrix-assisted DOSY to explore diffusion resolution in complex mixtures and found that using SDS micelles as the matrix can improve resolution. Increasing SDS concentration can also enhance resolution of DOSY spectrum.
Article
Chemistry, Multidisciplinary
Saroj Kumar Kushvaha, Paula Kallenbach, Shahnaz S. Rohman, Madhusudan K. Pandey, Zohreh Hendi, Franziska Ruttger, Regine Herbst-Irmer, Dietmar Stalke, Pattiyil Parameswaran, Herbert W. Roesky
Summary: The synthesis and characterization of the first inorganic four-membered neutral 2 pi-aromatic compound is reported. The unique ring structure has been successfully synthesized through a simple reaction and reduction process. The compound has been fully characterized using various analytical techniques. Computational calculations have shown the nature of the ring structure. This compound represents the first neutral planar inorganic analogue of cyclobutenyl dication.
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY
(2023)
Article
Biochemical Research Methods
Benjamin Lorandel, Rituraj Mishra, Oksana Cazimajou, Achille Marchand, Jean-Nicolas Dumez
Summary: This study presents an improved method for SPEN DOSY experiments by accounting for the non-uniformity of the field gradient, resulting in increased accuracy.
JOURNAL OF MAGNETIC RESONANCE
(2023)
Article
Chemistry, Inorganic & Nuclear
Andrew J. Straiton, James D. Parish, Joshua J. Smith, John P. Lowe, Andrew L. Johnson
Summary: A series of zinc phosphate complexes supported by nitrogen donor-base ligands were synthesized and their molecular structures were determined in both solid and solution states. The complexes showed polymeric and bimetallic structures, with some undergoing monomer-dimer equilibrium in solution. 1H DOSY experiments were conducted to measure the diffusion coefficients of the complexes and approximate the thermodynamic parameters of the monomer-dimer equilibria. One complex maintained its monomeric structure in the solid state, while another existed as both bimetallic species and free ligand in solution.
INORGANIC CHEMISTRY
(2023)
Article
Chemistry, Analytical
Haolin Zhan, Mengyou Hao, Enping Lin, Zeyu Zheng, Chengda Huang, Shuhui Cai, Shuohui Cao, Yuqing Huang, Zhong Chen
Summary: In this study, a new technique is developed to simultaneously observe molecular self-diffusion behaviors and multiplet structures in complex mixture samples, providing an effective method for studying complex mixtures.
ANALYTICAL CHEMISTRY
(2023)
Article
Chemistry, Analytical
Maximilian Weiss, Zuzana Gajarska, Hans Lohninger, Martina Marchetti-Deschmann, Georg Ramer, Bernhard Lendl, Andreas Limbeck
Summary: The growing importance of fluoropolymers in high-tech applications and green technologies has led to an increased demand for their characterization. This study presents a novel approach for quantitative mapping of fluorine in fluoropolymer samples using laser-induced breakdown spectroscopy (LIBS). The approach is based on monitoring molecular emission bands arising from fluorine-containing molecules. The study evaluates two techniques - spray coating and sputter coating - for their effects on sensitivity and spatial resolution in elemental mapping.
ANALYTICA CHIMICA ACTA
(2022)
Article
Agriculture, Multidisciplinary
Donatella Ancora, Jerneja Milavec, Anton Gradisek, Mario Cifelli, Ana Sepe, Tomaz Apih, Bostjan Zalar, Valentina Domenici
Summary: The study focuses on the detection of adulterated extra-virgin olive oil using H-1 NMR relaxation and diffusion measurements, comparing samples from Italy with various vegetable oils. Results indicate significant differences in diffusion coefficients between olive oils and vegetable oils, with linseed oil and macadamia oil being the easiest and most difficult frauds to detect, respectively.
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
(2021)
Article
Chemistry, Analytical
Taylor F. Nelson, Collin P. Ward
Summary: This study develops a diffusion-ordered spectroscopy (DOSY) method for determining the molecular weight (MW) of polymers, specifically focusing on consumer plastics. The DOSY method demonstrates high-throughput, accurate, and precise measures of polymer MW, as well as the ability to track the evolution of polymer MW during environmental degradation processes. The study also compares DOSY with gel permeation chromatography (GPC) and discusses future developments and potential applications of DOSY.
ANALYTICAL CHEMISTRY
(2023)
Article
Chemistry, Multidisciplinary
Corentin Jacquemmoz, Rituraj Mishra, Ludmilla Guduff, Carine van Heijenoort, Jean-Nicolas Dumez
Summary: Diffusion-ordered NMR spectroscopy (DOSY NMR) is a widely used method for the analysis of mixtures, allowing for the separation of spectra and analysis of interactions. Spatially-encoded (SPEN) DOSY enables the collection of a complete data set in less than 1 second, but there is a lack of thorough characterization of its features and practical use. Understanding the unusual principles and implementation of SPEN DOSY experiments is crucial for optimal utilization of the method in systems that evolve in time.
MAGNETIC RESONANCE IN CHEMISTRY
(2022)
Article
Chemistry, Analytical
Jonathan R. J. Yong, Eriks Kupce, Tim D. W. Claridge
Summary: NMR supersequences allow for faster experiments by tailoring the detection of NMR responses. The online tool GENESIS generates pulse programs for NOAH supersequences compatible with Bruker spectrometers. It provides customized supersequences, related scripts, and detailed instructions, while also facilitating the dissemination of new developments in NOAH sequences.
ANALYTICAL CHEMISTRY
(2022)
Article
Chemistry, Physical
Jihyun Kim, Mihajlo Novakovic, Sundaresan Jayanthi, Adonis Lupulescu, Eriks Kupce, J. Tassilo Gruenorcid, Klara Mertinkus, Andreas Oxenfarth, Harald Schwalbe, Lucio Frydman
Summary: Hadamard encoded saturation transfer can improve the efficiency and sensitivity of NOE-based NMR correlations in proteins, glycans, and RNAs. However, it fails in correlating labile protons within a pool. This study proposes an extended Hadamard scheme that allows for artifact-free correlations within the labile pool and between labile and non-labile protons, while still benefiting from Hadamard encoding and solvent repolarizations. The extended Hadamard scheme demonstrates clean, artifact-free, sensitivity-enhancing performance on RNA fragments derived from the SARS-CoV-2 genome.
Article
Polymer Science
Jin Hamaura, Ryo Honma, Hisao Hori, Abdelatif Manseri, Bruno Ameduri
Summary: Mineralization of PVDF, VDF-co-HFP and ETFE in superheated water with an alkaline reagent was studied for fluorine element recycling. The polymers underwent defluorination to form fluoride ions at 250 degrees Celsius in an Ar atmosphere. The presence of O2 instead of Ar resulted in different products. Consecutive runs did not reduce the yield of fluoride ions. PVDF, VDF-co-HFP, and ETFE copolymers completely mineralized to form fluoride ions with yields of 95%, 100%, and 98%, respectively. Adding Ca(OH)2 to the reaction solutions produced artificial fluorspar.
EUROPEAN POLYMER JOURNAL
(2023)
Article
Chemistry, Inorganic & Nuclear
Bruno Ameduri
Summary: Per- or polyfluoroalkyl substances (PFASs) can be divided into two families: low molar-mass PFASs, which are toxic and restricted, and polymeric ones. Fluoropolymers (FPs) are niche specialty bio-inert and safe polymers with outstanding properties, making them valuable and irreplaceable materials in many high tech applications. Despite the pressure faced by all PFASs, the concerns regarding industrial production of FPs have been addressed, highlighting their separation from conventional PFASs.
JOURNAL OF FLUORINE CHEMISTRY
(2023)
Article
Biochemistry & Molecular Biology
Lolwa Haydar, Wassim El Malti, Vincent Ladmiral, Ali Alaaeddine, Bruno Ameduri
Summary: New fluorinated polyhydroxyurethanes (FPHUs) were synthesized through the polyaddition reaction of a fluorinated bis(cyclocarbonate) (bis-CC) with a diamine. The fluorinated bis-CC was synthesized using a fluorinated diepoxide and LiBr catalyst. The reaction conditions were optimized and the FPHUs were characterized by various spectroscopic techniques and compared to their hydrogenated counterparts.
Article
Biochemistry & Molecular Biology
Frederic Boschet, Georgi Kostov, Hristina Raynova, Bruno Ameduri
Summary: The copolymerization and terpolymerization of 1,1,3,3,3-pentafluoropropene (PFP) with various fluorinated and hydrogenated comonomers were studied. The addition of vinylidene fluoride (VDF) improved the yields of terpolymers, while copolymers with non-homopolymerizable monomers showed low yields. The resulting polymers were amorphous fluoroelastomers or fluorothermoplastics with good thermal stability.
Article
Polymer Science
Jamila Taibi, Sophie Rouif, Bruno Ameduri, Rodolphe Sonnier, Belkacem Otazaghine
Summary: This study focuses on the one-step radiografting of flax fabrics with phosphonated and fluorinated polymer chains using (meth)acrylic monomers. The pre-irradiation procedure at 20 and 100 kGy allows the flax fabrics to have flame retardancy and hydro- and oleophobicity properties. The successful grafting of flax fibers is confirmed by FTIR spectroscopy, while the morphology, regioselectivity of grafting, and distribution of elements are assessed by SEM-EDX.
Review
Chemistry, Multidisciplinary
Zexi Zhang, Kaixuan Chen, Bruno Ameduri, Mao Chen
Summary: Fluorinated polymeric nanoparticles (FPNPs) combine the properties of fluorocarbon and polymeric nanoparticles. Well-defined FPNPs with complex structures, compositions, morphologies, and functionalities can be obtained through reversible-deactivation radical polymerizations (RDRPs). These FPNPs have promising applications in magnetic resonance imaging, biomedical delivery, energy storage, etc.
Article
Polymer Science
Jeet Sharma, Cedric Totee, Vaibhav Kulshrestha, Bruno Ameduri
Summary: This study provides new insights into the dehydrofluorination of poly(vinylidene fluoride) in alcoholic sodium hydroxide through the use of infrared, Raman and nuclear magnetic resonance spectroscopies. The reactivity of different phases and site selectivity is examined, and the formation of the -(CH=CF)- double bond is confirmed by 1H -19F heteronuclear correlation spectroscopy.
EUROPEAN POLYMER JOURNAL
(2023)
Article
Materials Science, Biomaterials
Ryohei Koguchi, Katja Jankova, Yukiko Tanaka, Aki Yamamoto, Daiki Murakami, Qizhi Yang, Bruno Ameduri, Masaru Tanaka
Summary: Hydrophilic materials can be made water insoluble by copolymerizing hydrophilic monomers with hydrophobic ones. By adding small amounts of fluorine to the copolymers, the hydrophilicity can be improved and excellent bio-inert properties can be achieved.
BIOMATERIALS ADVANCES
(2023)
Article
Polymer Science
Fatima Ezzahra Bouharras, Salima Atlas, Simone Capaccioli, Massimiliano Labardi, Abdelghani Hajlane, Bruno Ameduri, Mustapha Raihane
Summary: Core-double-shell-structured nanocomposite films consisting of PVDF-g-BT incorporated into a P(VDF-co-HFP) copolymer matrix were prepared for energy storage applications. The addition of PVDF-g-BT improved the thermal stability and crystallinity of the films. The films exhibited three dielectric processes, and mechanical analysis confirmed the uniform distribution and strong interaction of PVDF-g-BT with the copolymer matrix. The suggested system shows promise for high-energy-density storage devices such as supercapacitors.
Review
Chemistry, Multidisciplinary
Bruno Ameduri, Hisao Hori
Summary: This article presents the latest technology in the recycling, reuse, thermal decomposition, and life cycle assessment of fluoropolymers. Fluoropolymers have exceptional properties and are widely used in high-tech industries. The reuse of fluoropolymers is still underdeveloped, leading to increased interest in their recycling. Recent studies have also focused on vitrimers, and efforts have been made to avoid the release of harmful substances during thermal degradation.
CHEMICAL SOCIETY REVIEWS
(2023)
Article
Chemistry, Multidisciplinary
Ali Alaaeddine, Vincent Ladmiral, Wassim El Malti, Lolwa Haydar, Sylvain Caillol, Bruno Ameduri
Summary: Efficient methods for the cycloaddition of CX2 with fluorinated epoxides to produce cyclic carbonates or cyclic xanthates were developed. By optimizing the reaction conditions, high yields of the desired products were obtained. The reaction was proven to be reproducible with different substrates and two new fluorinated five-membered bis-CCs and bis-XAs were synthesized with high yields.
COMPTES RENDUS CHIMIE
(2023)
Article
Polymer Science
Fatima Ezzahra Bouharras, Massimiliano Labardi, Elpidio Tombari, Simone Capaccioli, Mustapha Raihane, Bruno Ameduri
Summary: The dielectric properties of PVDF-g-BT core-shell structured nanocomposites obtained by RAFT polymerization were investigated. The dielectric constant increased with the addition of BT, exhibiting a larger increase than predicted by usual modeling methods for composite materials, due to the effect of the interfacial core-shell structure. PVDF's known dielectric relaxations were observed in both the neat polymer and its nanocomposites, unaffected by the presence of nanoparticles. A relaxation process due to interfacial polarization was found at higher temperatures, attributed to the high crystallinity of the materials produced by RAFT.
Review
Biochemistry & Molecular Biology
Bruno Ameduri
Summary: This review discusses the differences between fluoropolymers (FPs) and low-molar-mass per- and polyfluoroalkyl substances (PFASs), highlighting the safety, durability, and diverse applications of FPs in various aspects of daily life. It also provides information on the recycling and risk assessment of FPs.