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1. Microbubbles decorated with dendronized magnetic nanoparticles for biomedical imaging: effective stabilization via fluorous interactions

Author

Da Shi, Justine Wallyn, Dinh-Vu Nguyen, Francis Perton, Delphine Felder-Flesch, Sylvie Bégin-Colin, Mounir Maaloum, and Marie Pierre Krafft

Subjects
diagnostic imaging, fluorinated dendrons, fluorocarbon, iron oxide nanoparticles, magnetic nanoparticles, microbubbles, Technology, Chemical technology, TP1-1185, Science, Physics, QC1-999
Abstract

Dendrons fitted with three oligo(ethylene glycol) (OEG) chains, one of which contains a fluorinated or hydrogenated end group and bears a bisphosphonate polar head (CnX2n+1OEG8Den, X = F or H; n = 2 or 4), were synthesized and grafted on the surface of iron oxide nanoparticles (IONPs) for microbubble-mediated imaging and therapeutic purposes. The size and stability of the dendronized IONPs (IONP@CnX2n+1OEG8Den) in aqueous dispersions were monitored by dynamic light scattering. The investigation of the spontaneous adsorption of IONP@CnX2n+1OEG8Den at the interface between air or air saturated with perfluorohexane and an aqueous phase establishes that exposure to the fluorocarbon gas markedly increases the rate of adsorption of the dendronized IONPs to the gas/water interface and decreases the equilibrium interfacial tension. This suggests that fluorous interactions are at play between the supernatant fluorocarbon gas and the fluorinated end groups of the dendrons. Furthermore, small perfluorohexane-stabilized microbubbles (MBs) with a dipalmitoylphosphatidylcholine (DPPC) shell that incorporates IONP@CnX2n+1OEG8Den (DPPC/Fe molar ratio 28:1) were prepared and subsequently characterized using both optical microscopy and an acoustical method of size determination. The dendrons fitted with fluorinated end groups lead to smaller and more stable MBs than those fitted with hydrogenated groups. The most effective result is already obtained with C2F5, for which MBs of ≈1.0 μm in radius reach a half-life of ≈6.0 h. An atomic force microscopy investigation of spin-coated mixed films of DPPC/IONP@C2X5OEG8Den combinations (molar ratio 28:1) shows that the IONPs grafted with the fluorinated dendrons are located within the phospholipid film, while those grafted with the hydrocarbon dendrons are located at the surface of the phospholipid film.

Published
2019
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2. Unravelling the Thermal Decomposition Parameters for The Synthesis of Anisotropic Iron Oxide Nanoparticles

Author

Geoffrey Cotin, Céline Kiefer, Francis Perton, Dris Ihiawakrim, Cristina Blanco-Andujar, Simona Moldovan, Christophe Lefevre, Ovidiu Ersen, Benoit Pichon, Damien Mertz, and Sylvie Bégin-Colin

Subjects
iron oxide nanoparticles, synthesis, shape control, thermal decomposition, precursor, Chemistry, QD1-999
Abstract

Iron oxide nanoparticles are widely used as a contrast agent in magnetic resonance imaging (MRI), and may be used as therapeutic agent for magnetic hyperthermia if they display in particular high magnetic anisotropy. Considering the effect of nanoparticles shape on anisotropy, a reproducible shape control of nanoparticles is a current synthesis challenge. By investigating reaction parameters, such as the iron precursor structure, its water content, but also the amount of the surfactant (sodium oleate) reported to control the shape, iron oxide nanoparticles with different shape and composition were obtained, in particular, iron oxide nanoplates. The effect of the surfactant coming from precursor was taking into account by using in house iron stearates bearing either two or three stearate chains and the negative effect of water on shape was confirmed by considering these precursors after their dehydration. Iron stearates with three chains in presence of a ratio sodium oleate/oleic acid 1:1 led mainly to nanocubes presenting a core-shell Fe1−xO@Fe3−xO4 composition. Nanocubes with straight faces were only obtained with dehydrated precursors. Meanwhile, iron stearates with two chains led preferentially to the formation of nanoplates with a ratio sodium oleate/oleic acid 4:1. The rarely reported flat shape of the plates was confirmed with 3D transmission electronic microscopy (TEM) tomography. The investigation of the synthesis mechanisms confirmed the major role of chelating ligand and of the heating rate to drive the cubic shape of nanoparticles and showed that the nanoplate formation would depend mainly on the nucleation step and possibly on the presence of a given ratio of oleic acid and chelating ligand (oleate and/or stearate).

Published
2018
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3. One Pot Synthesis of Dithiolane Dendron Functionalized Gold Nanoparticles

Author

Barbara Freis, Francis Perton, Sylvie Begin-Colin, Damien Mertz, Marlène Palluel, Céline Kiefer, Institut de Physique et Chimie des Matériaux de Strasbourg (IPCMS), and Université Louis Pasteur - Strasbourg I-Centre National de la Recherche Scientifique (CNRS)

Subjects
Chemistry, One-pot synthesis, [CHIM.MATE]Chemical Sciences/Material chemistry, [CHIM.THER]Chemical Sciences/Medicinal Chemistry, 02 engineering and technology, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, Combinatorial chemistry, 0104 chemical sciences, Dithiolane, Inorganic Chemistry, chemistry.chemical_compound, Colloidal gold, Dendrimer, 0210 nano-technology, ComputingMilieux_MISCELLANEOUS
Abstract

International audience

Published
2021

5. Small iron oxide nanoparticles as MRI

Author

Maximilian O, Besenhard, Luca, Panariello, Céline, Kiefer, Alec P, LaGrow, Liudmyla, Storozhuk, Francis, Perton, Sylvie, Begin, Damien, Mertz, Nguyen Thi Kim, Thanh, and Asterios, Gavriilidis

Abstract

Small iron oxide nanoparticles (IONPs) were synthesised in water via co-precipitation by quenching particle growth after the desired magnetic iron oxide phase formed. This was achieved in a millifluidic multistage flow reactor by precisely timed addition of an acidic solution. IONPs (≤5 nm), a suitable size for positive T1 magnetic resonance imaging (MRI) contrast agents, were obtained and stabilised continuously. This novel flow chemistry approach facilitates a reproducible and scalable production, which is a crucial paradigm shift to utilise IONPs as contrast agents and replace currently used Gd complexes. Acid addition had to be timed carefully, as the inverse spinel structure formed within seconds after initiating the co-precipitation. Late quenching allowed IONPs to grow larger than 5 nm, whereas premature acid addition yielded undesired oxide phases. Use of a flow reactor was not only essential for scalability, but also to synthesise monodisperse and non-agglomerated small IONPs as (i) co-precipitation and acid addition occurred at homogenous environment due to accurate temperature control and rapid mixing and (ii) quenching of particle growth was possible at the optimum time, i.e., a few seconds after initiating co-precipitation. In addition to the timing of growth quenching, the effect of temperature and dextran present during co-precipitation on the final particle size was investigated. This approach differs from small IONP syntheses in batch utilising either growth inhibitors (which likely leads to impurities) or high temperature methods in organic solvents. Furthermore, this continuous synthesis enables the low-cost (£10 per g) and large-scale production of highly stable small IONPs without the use of toxic reagents. The flow-synthesised small IONPs showed high T1 contrast enhancement, with transversal relaxivity (r2) reduced to 20.5 mM-1 s-1 and longitudinal relaxivity (r1) higher than 10 mM-1 s-1, which is among the highest values reported for water-based IONP synthesis.

Published
2021

6. Iron Stearate Structures: An Original Tool for Nanoparticles Design

Author

Jean-Marc Strub, Nathalie Parizel, Benoît Heinrich, Damien Mertz, Céline Kiefer, Benoit P. Pichon, Sarah Cianférani, Sylvie Begin-Colin, Geoffrey Cotin, Francis Perton, Jean-Marc Greneche, Institut de Physique et Chimie des Matériaux de Strasbourg (IPCMS), 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)-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), Département Sciences Analytiques et Interactions Ioniques et Biomoléculaires (DSA-IPHC), Institut Pluridisciplinaire Hubert Curien (IPHC), Institut National de Physique Nucléaire et de Physique des Particules du CNRS (IN2P3)-Université de Strasbourg (UNISTRA)-Centre National de la Recherche Scientifique (CNRS)-Institut National de Physique Nucléaire et de Physique des Particules du CNRS (IN2P3)-Université de Strasbourg (UNISTRA)-Centre National de la Recherche Scientifique (CNRS), Institut des Molécules et Matériaux du Mans (IMMM), Le Mans Université (UM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie de Strasbourg, Université de Strasbourg (UNISTRA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), RENARD (TGE Réseau National de RPE interdisciplinaire - 3443 ), Aix Marseille Université (AMU)-Université de Strasbourg (UNISTRA)-Ecole Nationale Supérieure de Chimie de Paris - Chimie ParisTech-PSL (ENSCP), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Institut de Chimie du CNRS (INC)-Université de Lille-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS)-Université de Paris (UP)-Laboratoire de Chimie et de Biochimie Pharmacologiques et Toxicologiques (LCBPT - UMR 8601), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Paris (UP)-Centre National de la Recherche Scientifique (CNRS)-Université de Paris (UP)-Université Grenoble Alpes (UGA), Université de Strasbourg (UNISTRA)-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)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Réseau nanophotonique et optique, 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)-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 Physique Nucléaire et de Physique des Particules du CNRS (IN2P3)-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 Physique Nucléaire et de Physique des Particules du CNRS (IN2P3)-Centre National de la Recherche Scientifique (CNRS), Université de Strasbourg (UNISTRA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Institut de Chimie du CNRS (INC)-Université de Lille-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS)-Université Paris Cité (UPCité)-Laboratoire de Chimie et de Biochimie Pharmacologiques et Toxicologiques (LCBPT - UMR 8601), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Paris Cité (UPCité)-Centre National de la Recherche Scientifique (CNRS)-Université Paris Cité (UPCité)-Université Grenoble Alpes (UGA), Université de Strasbourg (UNISTRA)-Institut National de Physique Nucléaire et de Physique des Particules du CNRS (IN2P3)-Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA)-Institut National de Physique Nucléaire et de Physique des Particules du CNRS (IN2P3)-Centre National de la Recherche Scientifique (CNRS), and Gaillard, Brigitte

Subjects
[CHIM.INOR] Chemical Sciences/Inorganic chemistry, 02 engineering and technology, [CHIM.INOR]Chemical Sciences/Inorganic chemistry, 010402 general chemistry, 01 natural sciences, Chloride, Catalysis, Inorganic Chemistry, chemistry.chemical_compound, Stearate, Polymer chemistry, medicine, Lamellar structure, Carboxylate, Physical and Theoretical Chemistry, iron stearate synthesis mechanisms, Thermal decomposition, nucleation mechanism, iron oxide nanoparticles, 021001 nanoscience & nanotechnology, 0104 chemical sciences, iron stearate, chemistry, Chimie/Chimie inorganique, iron stearate composition and structure, Stearic acid, 0210 nano-technology, Iron oxide nanoparticles, medicine.drug
Abstract

International audience; Iron carboxylates are widely used as iron precursors in the thermal decomposition process or considered as in situ formed intermediate precursors. Their molecular and three-dimensional (3D)-structural nature has been shown to affect the shape, size, and composition of the resulting iron oxide nanoparticles (NPs). Among carboxylate precursors, stearates are particularly attractive because of their higher stability to aging and hydration and they are used as additives in many applications. Despite the huge interest of iron stearates, very few studies aimed up to now at deciphering their full metal-ligand structures and the mechanisms allowing us to achieve in a controlled manner the bottom-up NP formation. In this work, we have thus investigated the molecular structure and composition of two iron stearate precursors, synthesized by introducing either two (FeSt2) or three (FeSt3) stearate (St) chains. Interestingly, both iron stearates consist of lamellar structures with planes of iron polynuclear complexes (polycations) separated with stearate chains in all-trans conformation. The iron content in polycations was found very different between both iron stearates. Their detailed characterizations indicate that FeSt2 is mainly composed of [Fe3-(μ3-O)St6·xH2O]Cl, with no (or few) free stearate, whereas FeSt3 is a mixture of mainly [Fe7(μ3-O(H))6(μ2-OH)xSt12–2x]St with some [Fe3(μ3-O)St6·xH2O]St and free stearic acid. The formation of bigger polynuclear complexes with FeSt3 was related to higher hydrolysis and condensation rates within the iron(III) chloride solution compared to the iron(II) chloride solution. These data suggested a nucleation mechanism based on the condensation of polycation radicals generated by the catalytic departure of two stearate chains from an iron polycation-based molecule.

Published
2021

7. Small iron oxide nanoparticles as MRI T1 contrast agent: scalable inexpensive water-based synthesis using a flow reactor

Author

Luca Panariello, Nguyen T. K. Thanh, Francis Perton, Asterios Gavriilidis, Sylvie Begin, Céline Kiefer, Maximilian O. Besenhard, Damien Mertz, Alec P. LaGrow, Liudmyla Storozhuk, Institut de Physique et Chimie des Matériaux de Strasbourg (IPCMS), and Université Louis Pasteur - Strasbourg I-Centre National de la Recherche Scientifique (CNRS)

Subjects
Quenching (fluorescence), Materials science, Dispersity, Oxide, Iron oxide, [CHIM.MATE]Chemical Sciences/Material chemistry, [CHIM.THER]Chemical Sciences/Medicinal Chemistry, 02 engineering and technology, Flow chemistry, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, 0104 chemical sciences, chemistry.chemical_compound, chemistry, Chemical engineering, Reagent, General Materials Science, Particle size, 0210 nano-technology, Iron oxide nanoparticles
Abstract

Small iron oxide nanoparticles (IONPs) were synthesised in water via co-precipitation by quenching particle growth after the desired magnetic iron oxide phase formed. This was achieved in a millifluidic multistage flow reactor by precisely timed addition of an acidic solution. IONPs (≤5 nm), a suitable size for positive T1 magnetic resonance imaging (MRI) contrast agents, were obtained and stabilised continuously. This novel flow chemistry approach facilitates a reproducible and scalable production, which is a crucial paradigm shift to utilise IONPs as contrast agents and replace currently used Gd complexes. Acid addition had to be timed carefully, as the inverse spinel structure formed within seconds after initiating the co-precipitation. Late quenching allowed IONPs to grow larger than 5 nm, whereas premature acid addition yielded undesired oxide phases. Use of a flow reactor was not only essential for scalability, but also to synthesise monodisperse and non-agglomerated small IONPs as (i) co-precipitation and acid addition occurred at homogenous environment due to accurate temperature control and rapid mixing and (ii) quenching of particle growth was possible at the optimum time, i.e., a few seconds after initiating co-precipitation. In addition to the timing of growth quenching, the effect of temperature and dextran present during co-precipitation on the final particle size was investigated. This approach differs from small IONP syntheses in batch utilising either growth inhibitors (which likely leads to impurities) or high temperature methods in organic solvents. Furthermore, this continuous synthesis enables the low-cost (

Published
2021

8. Harnessing Composition of Iron Oxide Nanoparticle: Impact of Solvent-Mediated Ligand–Ligand Interaction and Competition between Oxidation and Growth Kinetics

Author

Valentin Begin, Damien Mertz, Corinne Petit, Christophe Lefevre, Geoffrey Cotin, Jean-Marc Greneche, Sylvie Begin-Colin, Francis Perton, Sécou Sall, Céline Kiefer, Benoit P. Pichon, Institut de Physique et Chimie des Matériaux de Strasbourg (IPCMS), 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)-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), Institut des Molécules et Matériaux du Mans (IMMM), and Le Mans Université (UM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Chemistry, Growth kinetics, Ligand, General Chemical Engineering, media_common.quotation_subject, Iron oxide, Nanoparticle, 02 engineering and technology, General Chemistry, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, Competition (biology), 0104 chemical sciences, Solvent, chemistry.chemical_compound, Chemical engineering, Materials Chemistry, [CHIM]Chemical Sciences, Composition (visual arts), 0210 nano-technology, Stoichiometry, media_common
Abstract

International audience; The composition of metal oxide nanoparticles is of great importance for their applications because defects and/or deviation from stoechiometry strongly affect their physical properties. We report here on the crucial role of synthesis parameters such as solvent, ligand and iron precursors on the composition of spinel iron oxide nanoparticles synthesized by the thermal decomposition method. At first, the investigation of the thermal decomposition of iron stearates bearing either two or three stearate chains by thermogravimetric analysis, IR spectroscopy and Mössbauer spectrometry as a function of temperature and syntheses with only oleic acid and iron stearate confirmed that the composition of the first nuclei is wüstite Fe 1-x O. The synthesis of nanoparticles with high sizes requires the use of very high boiling point solvents to ensure an effective growth step. We observed that, when the grain growth and oxidation kinetics are similar, nanoparticles with a spinel composition and quite no defects are produced. An oxidation rate slower than the nuclei growth rate favours the formation of core-shell Fe 1-x O@Fe 3-x O 4 NPs. The oxidation kinetics is shown to be influenced by surfactant and solvent natures. Indeed, surfactants such as oleic acid form a dense monolayer at the nuclei surface which oxidation kinetics will depend on this monolayer permeability. Temperature, solvents with high surfactant affinity, deprotonated surfactants or decomposition products of solvents affect the monolayer stability and thus the nanoparticle composition. The solvents' nature and solvent mediated ligand-ligand interactions are thus evidenced to be important parameters to control the formation of defectsfree and stoechiometric oxide nanoparticles.

Published
2020

9. A Confinement‐Driven Nucleation Mechanism of Metal Oxide Nanoparticles Obtained via Thermal Decomposition in Organic Media

Author

Geoffrey Cotin, Benoît Heinrich, Francis Perton, Céline Kiefer, Gregory Francius, Damien Mertz, Barbara Freis, Benoit Pichon, Jean‐Marc Strub, Sarah Cianférani, Nathalie Ortiz Peña, Dris Ihiawakrim, David Portehault, Ovidiu Ersen, Amir Khammari, Matthieu Picher, Florian Banhart, Clement Sanchez, and Sylvie Begin‐Colin

Subjects
Biomaterials, Iron, Stearates, Aucun, Metal Nanoparticles, Oxides, General Materials Science, General Chemistry, Ferric Compounds, Culture Media, Biotechnology
Abstract

Thermal decomposition is a very efficient synthesis strategy to obtain nanosized metal oxides with controlled structures and properties. For the iron oxide nanoparticle synthesis, it allows an easy tuning of the nanoparticle's size, shape, and composition, which is often explained by the LaMer theory involving a clear separation between nucleation and growth steps. Here, the events before the nucleation of iron oxide nanocrystals are investigated by combining different complementary in situ characterization techniques. These characterizations are carried out not only on powdered iron stearate precursors but also on a preheated liquid reaction mixture. They reveal a new nucleation mechanism for the thermal decomposition method: instead of a homogeneous nucleation, the nucleation occurs within vesicle-like-nanoreactors confining the reactants. The different steps are: 1) the melting and coalescence of iron stearate particles, leading to "droplet-shaped nanostructures" acting as nanoreactors; 2) the formation of a hitherto unobserved iron stearate crystalline phase within the nucleation temperature range, simultaneously with stearate chains loss and Fe(III) to Fe(II) reduction; 3) the formation of iron oxide nuclei inside the nanoreactors, which are then ejected from them. This mechanism paves the way toward a better mastering of the metal oxide nanoparticles synthesis and the control of their properties.

Published
2022

10. Mastering bioactive coatings of metal oxide nanoparticles and surfaces through phosphonate dendrons

Author

Philippe Lavalle, Da Shi, Emilie Voirin, Miriam Filippi, Geoffrey Cotin, Sylvie Begin-Colin, Marie Pierre Krafft, Delphine Felder-Flesch, Dinh-Vu Nguyen, Francis Perton, Arnaud Scherberich, Laura Power, Ludivine Hugoni, 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), 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)-Université de Strasbourg (UNISTRA)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Langmuir, Chemistry, Nanoparticle, 02 engineering and technology, General Chemistry, Quartz crystal microbalance, [CHIM.MATE]Chemical Sciences/Material chemistry, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, Phosphonate, Catalysis, 0104 chemical sciences, Biofouling, Metal, chemistry.chemical_compound, Chemical engineering, visual_art, Monolayer, Materials Chemistry, visual_art.visual_art_medium, 0210 nano-technology, Iron oxide nanoparticles
Abstract

International audience; We reported herein an efficient method for constructing dendritic bisphosphonic acid tweezers of generations 1 and 2, which have been proven as versatile surface coatings for metal oxides implant or nanoparticles. These procedures delineated a practical and general route to a library of functional dendrons. Several of these dendritic architectures were successfully tested as biocompatible coverings for iron oxide nanoparticles through in vitro assays, but also as antifouling surface coatings for silica through Quartz Crystal Microbalance studies or as stabilizing structure for magnetic nanoparticles-microbubbles conjugates thanks to preliminary Langmuir monolayers studies.

Published
2020

11. Metronidazole-functionalized iron oxide nanoparticles for molecular detection of hypoxic tissues

Author

Sylvie Begin-Colin, Arnaud Scherberich, Francis Perton, Laura Power, Delphine Felder-Flesch, Dinh-Vu Nguyen, Miriam Filippi, and Francesca Garello

Subjects
Erythrocytes, Cell Survival, Cell Culture Techniques, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Ferric Compounds, Hemolysis, Fluorescence, chemistry.chemical_compound, 3D cell culture, Mice, Tissue engineering, Dendrimer, Metronidazole, Human Umbilical Vein Endothelial Cells, Animals, Humans, General Materials Science, Viability assay, Magnetite Nanoparticles, Cell Proliferation, Anthracenes, Microscopy, Cell growth, Chemistry, 021001 nanoscience & nanotechnology, Cell Hypoxia, Microscopy, Fluorescence, RAW 264.7 Cells, 0104 chemical sciences, Cell culture, Biophysics, Stem cell, 0210 nano-technology, Iron oxide nanoparticles
Abstract

Being crucial under several pathological conditions, tumors, and tissue engineering, the MRI tracing of hypoxia within cells and tissues would be improved by the use of nanosystems allowing for direct recognition of low oxygenation and further treatment-oriented development. In the present study, we functionalized dendron-coated iron oxide nanoparticles (dendronized IONPs) with a bioreductive compound, a metronidazole-based ligand, to specifically detect the hypoxic tissues. Spherical IONPs with an average size of 10 nm were obtained and then decorated with the new metronidazole-conjugated dendron. The resulting nanoparticles (metro-NPs) displayed negligible effects on cell viability, proliferation, and metabolism, in both monolayer and 3D cell culture models, and a good colloidal stability in bio-mimicking media, as shown by DLS. Overtime quantitative monitoring of the IONP cell content revealed an enhanced intracellular retention of metro-NPs under anoxic conditions, confirmed by the in vitro MRI of cell pellets where a stronger negative contrast generation was observed in hypoxic primary stem cells and tumor cells after labeling with metro-NPs. Overall, these results suggest desirable properties in terms of interactions with the biological environment and capability of selective accumulation into the hypoxic tissue, and indicate that metro-NPs have considerable potential for the development of new nano-platforms especially in the field of anoxia-related diseases and tissue engineered models.

Published
2019

12. Microbubbles Decorated with Dendronized Magnetic Nanoparticles for Biomedical Imaging. Effective Stabilization via Fluorous Interactions

Author

Francis Perton, Marie Pierre Krafft, Dinh-Vu Nguyen, Mounir Maaloum, Sylvie Begin-Colin, Justine Wallyn, Da Shi, Delphine Felder-Flesch, Conception et application de molécules bioactives (CAMB), Université de Strasbourg (UNISTRA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut de Physique et Chimie des Matériaux de Strasbourg (IPCMS), 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)-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), 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), 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)-Université de Strasbourg (UNISTRA)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)

Subjects
magnetic nanoparticles, diagnostic imaging, General Physics and Astronomy, 02 engineering and technology, lcsh:Chemical technology, lcsh:Technology, 01 natural sciences, Full Research Paper, microbubbles, chemistry.chemical_compound, Adsorption, Dynamic light scattering, Nanotechnology, lcsh:TP1-1185, General Materials Science, Fluorocarbon, Electrical and Electronic Engineering, lcsh:Science, Perfluorohexane, lcsh:T, 010405 organic chemistry, fluorinated dendrons, iron oxide nanoparticles, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, lcsh:QC1-999, 0104 chemical sciences, Nanoscience, End-group, chemistry, Chemical engineering, Dipalmitoylphosphatidylcholine, Magnetic nanoparticles, lcsh:Q, fluorocarbon, 0210 nano-technology, Ethylene glycol, lcsh:Physics
Abstract

Dendrons fitted with three oligoethylene glycol (OEG) chains, one of which carrying a fluorinated or hydrogenated end group, and bearing a bisphosphonate polar head (C n X2 n +1OEG8Den, X = F or H; n= 2 or 4) were synthesized and grafted on the surface of iron oxide nanoparticles (IONPs) for microbubble-mediated imaging and therapeutic purposes. The size and stability of the dendronized IONPs (IONP@C n X2 n +1OEG8Den) in aqueous dispersions were monitored by dynamic light scattering. Investigation of the spontaneous adsorption of IONP@C n X2 n +1OEG8Den at the interface between air - or air saturated with perfluorohexane - and an aqueous phase establishes that exposure to the fluorocarbon gas markedly increases the rate of adsorption of the dendronized IONPs to the gas/water interface and decreases the equilibrium interfacial tension. This suggests that fluorous interactions are at play between the supernatant fluorocarbon gas and the fluorinated end groups of the dendrons. Furthermore, small, stable perfluorohexane-stabilized microbubbles (MBs) with a dipalmitoylphosphatidylcholine (DPPC) shell that incorporates IONP@C n X2 n +1OEG8Den (DPPC/Fe molar ratio 28:1) were prepared and characterized using both optical microscopy and an acoustical method of size determination. The dendrons fitted with fluorinated end groups lead to smaller and more stable MBs than those fitted with hydrogenated groups. The most effective result is already obtained with C2F5, for which MBs, ~1.0mm in radius, reach a half-life of ~6.0 h. An atomic force microscopy investigation of spin-coated mixed films of DPPC/IONP@C2X5OEG8Den combinations (molar ratio 28:1) shows that the IONPs grafted with the fluorinated dendrons are located within the phospholipid film, while those grafted with the hydrocarbon dendrons are completely absent from the phospholipid film.

Published
2019

13. Wrapped stellate silica nanocomposites as biocompatible luminescent nanoplatforms assessed in vivo

Author

Ksenia Parkhomenko, Damien Mertz, Francis Perton, Sylvie Begin-Colin, Jacky G. Goetz, Sébastien Harlepp, Gautier Follain, Institut de Physique et Chimie des Matériaux de Strasbourg (IPCMS), 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)-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), Immuno-Rhumatologie Moléculaire, Université de Strasbourg (UNISTRA)-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), 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)-Centre National de la Recherche Scientifique (CNRS)-Matériaux et nanosciences d'Alsace, 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)-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)-Réseau nanophotonique et optique, 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), Immunorhumathologie moléculaire, Institut National de la Santé et de la Recherche Médicale (INSERM), 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)-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)-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)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Réseau nanophotonique et optique, 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)-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), and Mertz, Damien

Subjects
Materials science, Biocompatibility, Cell Survival, Phosphines, Surface Properties, [CHIM.THER] Chemical Sciences/Medicinal Chemistry, Nanoparticle, Biocompatible Materials, Nanotechnology, 02 engineering and technology, [CHIM.THER]Chemical Sciences/Medicinal Chemistry, Sulfides, engineering.material, 010402 general chemistry, Indium, 01 natural sciences, Nanocomposites, Biomaterials, Mice, Colloid and Surface Chemistry, Coating, Polysaccharides, In vivo, Cell Line, Tumor, Quantum Dots, Animals, Particle Size, Zebrafish, ComputingMilieux_MISCELLANEOUS, Fluorescent Dyes, [CHIM.MATE] Chemical Sciences/Material chemistry, Nanocomposite, technology, industry, and agriculture, [CHIM.MATE]Chemical Sciences/Material chemistry, Mesoporous silica, Silicon Dioxide, 021001 nanoscience & nanotechnology, Amides, Fluorescence, 0104 chemical sciences, Surfaces, Coatings and Films, Electronic, Optical and Magnetic Materials, Spectrometry, Fluorescence, Zinc Compounds, Drug delivery, engineering, 0210 nano-technology, Porosity
Abstract

The engineering of luminescent nanoplatforms for biomedical applications displaying ability for scaling-up, good colloidal stability in aqueous solutions, biocompatibility, and providing an easy detection in vivo by fluorescence methods while offering high potential of functionalities, is currently a challenge. The original strategy proposed here involves the use of large pore (ca. 15 nm) mesoporous silica (MS) nanoparticles (NPs) having a stellate morphology (denoted STMS) on which fluorescent InP/ZnS quantum dots (QDs) are covalently grafted with a high yield (≥90%). These nanoplatforms are after that further coated to avoid a potential QDs release. To protect the QDs from potential release or dissolution, two wrapping methods are developed: (i) a further coating with a silica shell having small pores (≤2 nm) or (ii) a tight polysaccharide shell deposited on the surface of these STMS@QDs particles via an original isobutyramide (IBAM)-mediated method. Both wrapping approaches yield to novel luminescent nanoplatforms displaying a highly controlled structure, a high size monodispersity (ca. 200 and 100 nm respectively) and colloidal stability in aqueous solutions. Among both methods, the IBAM-polysaccharide coating approach is shown the most suitable to ensure QDs protection and to avoid metal cation release over three months. Furthermore, these original STMS@QDs@polysaccharide luminescent nanoplatforms are shown biocompatible in vitro with murine cancer cells and in vivo after injections within zebrafish (ZF) translucent embryos where no sign of toxicity is observed during their development over several days. As assessed by in vivo confocal microscopy imaging, these nanoplatforms are shown to rapidly extravasate from blood circulation to settle in neighboring tissues, ensuring a remanent fluorescent labelling of ZF tissues in vivo. Such fluorescent and hybrid STMS composites are envisioned as novel luminescent nanoplatforms for in vivo fluorescence tracking applications and offer a versatile degree of additional functionalities (drug delivery, incorporation of magnetic/plasmonic core).

Published
2019

14. Fluorescent and magnetic stellate mesoporous silica for bimodal imaging and magnetic hyperthermia

Author

Cristina Blanco-Andujar, Mariana Tasso, Guillermo Arturo Muñoz Medina, Florent Meyer, Marcela Beatriz Fernández van Raap, Dominique Begin, Francis Perton, Damien Mertz, Mathilde Ménard, Sylvie Begin-Colin, Enrique Leo Portiansky, Institut de Physique et Chimie des Matériaux de Strasbourg (IPCMS), 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)-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), Instituto de Investigaciones Fisicoquímicas Teóricas y Aplicadas [La Plata] (INIFTA), Facultad de Ciencias Exactas [La Plata], Universidad Nacional de la Plata [Argentine] (UNLP)-Universidad Nacional de la Plata [Argentine] (UNLP), Universidad Nacional de la Plata [Argentine] (UNLP), Biomatériaux et Bioingénierie (BB), Université de Strasbourg (UNISTRA)-Institut National de la Santé et de la Recherche Médicale (INSERM)-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), Institut de chimie et procédés pour l'énergie, l'environnement et la santé (ICPEES), 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)-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)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Réseau nanophotonique et optique, 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)-Centre National de la Recherche Scientifique (CNRS), Université de Strasbourg (UNISTRA)-Institut National de la Santé et de la Recherche Médicale (INSERM)-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)-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), and Mertz, Damien

Subjects
[CHIM.INOR] Chemical Sciences/Inorganic chemistry, Materials science, Biocompatibility, [SDV.IB.IMA]Life Sciences [q-bio]/Bioengineering/Imaging, [CHIM.THER] Chemical Sciences/Medicinal Chemistry, Nanotechnology, Large pore mesoporous silica and albumin coatings, 02 engineering and technology, [CHIM.THER]Chemical Sciences/Medicinal Chemistry, Fluorescent and magnetic silica, engineering.material, [CHIM.INOR]Chemical Sciences/Inorganic chemistry, 010402 general chemistry, 01 natural sciences, Coating, General Materials Science, Magnetic hyperthermia, [CHIM.MATE] Chemical Sciences/Material chemistry, Nanocomposite, Física, [CHIM.MATE]Chemical Sciences/Material chemistry, Química, Mesoporous silica, 021001 nanoscience & nanotechnology, Fluorescence, 0104 chemical sciences, 3. Good health, [SDV.IB.IMA] Life Sciences [q-bio]/Bioengineering/Imaging, 13. Climate action, Quantum dot, Specific and non-specific cell/nanoparticle interactions, Bimodal imaging probes, engineering, Nanomedicine, 0210 nano-technology
Abstract

There is currently a crucial need of innovative multifunctional nanoparticles combining, in one formulation, imaging and therapy capacities allowing thus an accurate diagnosis and a therapy monitored by imaging. Multimodal imaging will ensure to speed up diagnosis, and to increase its sensitivity, reliability and specificity for a better management of the disease. Combined with a therapeutic action, it will also enable to treat the disease in a specific personalized manner in feedback mode. The mastered design of such bioprobes as well as the demonstration of their efficiency are still challenges to face in nanomedicine. In this work, novel fluorescent and magnetic core–shell nanocomposites have been designed to ensure, in one nanoformulation, bimodal fluorescence and MRI imaging coupled with therapy by magnetic hyperthermia. They consist in the coating of a magnetic iron oxide (IO) core (ca. 18 nm diameter to ensure magnetic hyperthermia) by an original large pore stellate mesoporous silica (STMS) shell to produce uniform and mono-core magnetic core–shell nanocomposites denoted IO@STMS NPs. To confer fluorescence properties, CdSe/ZnS quantum dots (QDs) NPs were grafted inside the large pores of the IO@STMS nanocomposites. To provide biocompatibility and opsonization-resistance, a tightly-bound human serum albumin (HSA) coating is added around the nanocomposite using an original IBAM-based strategy. Cellular toxicity and non-specific cell–nanomaterial interactions allowed to determine a concentration range for safe application of these NPs. Cellular endosomes containing spontaneously-uptaken NPs displayed strong and photostable QD fluorescence signals while magnetic relaxivity measurements confirm their suitability as contrast agent for MRI. HeLa cell-uptaken NPs exposed to a magnetic field of 100 kHz and 357 Gauss (or 28.5 kA m−1) display an outstanding 65% cell death at a very low iron concentration (1.25 μg Fe mL−1), challenging current magnetic hyperthermia nanosystems. Furthermore, at the particularly demanding conditions of clinical use with low frequency and amplitude field (100 kHz, 117 Gauss or 9.3 kA m−1), magnetic hyperthermia combined with the delivery of a chemotherapeutic drug, doxorubicin, allowed 46% cell death, which neither the drug nor the NPs alone yielded, evidencing thus the synergistic effect of this combined treatment., Facultad de Ciencias Veterinarias, Instituto de Investigaciones Fisicoquímicas Teóricas y Aplicadas, Instituto de Física La Plata

Published
2019

15. Contributors

Author

Laura Asín, Sylvie Bégin-Colin, Lilianne Beola, Cristina Blanco-Andujar, Whitney N. Boehm, Ana C. Bohórquez, Carlos D.S. Brites, David Cabrera, Luis D. Carlos, Geoffrey Cotin, Thomas K. Darlington, Jesús M. de la Fuente, Rohan Dhavalikar, Luc Dupré, Neil Farrow, Raluca M. Fratila, Betty C. Galarreta, Eneko Garaio, Laura Gonzalez-Moragas, Valeria Grazú, Lucía Gutiérrez, Yulán Hernández, Javier Idiago-López, Balachandran Jeyadevan, Ryoichi Kitaura, Anna Laromaine, Shinya Maenosono, Hiroaki Mamiya, Damien Mertz, Angel Millán, Priyank Mohan, Eduardo Moreno-Antolín, Maria Moros, Steven J. Oldenburg, Daniel Ortega, Marta Pérez-Hernández, Francis Perton, Benoit Pichon, Rafael Piñol, Fernando Plazaola, Carlos Rinaldi, Irene Rubia-Rodríguez, Karolina Sauerova, Nuno J. Silva, Mari Takahashi, Neil Telling, Francisco J. Terán, Angela Tino, and Claudia Tortiglione

Published
2019

16. Design of Anisotropic Iron-Oxide-Based Nanoparticles for Magnetic Hyperthermia

Author

Benoit P. Pichon, Geoffrey Cotin, Sylvie Begin-Colin, Cristina Blanco-Andujar, Damien Mertz, Francis Perton, Institut de Physique et Chimie des Matériaux de Strasbourg (IPCMS), 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)-Réseau nanophotonique et optique, and 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)

Subjects
Heating power, Materials science, Anisotropy energy, Thermal ablation, Iron oxide, Nanoparticle, Nanotechnology, 02 engineering and technology, [CHIM.MATE]Chemical Sciences/Material chemistry, [CHIM.THER]Chemical Sciences/Medicinal Chemistry, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, 0104 chemical sciences, 3. Good health, chemistry.chemical_compound, Magnetic hyperthermia, chemistry, Surface modification, 0210 nano-technology, Anisotropy, ComputingMilieux_MISCELLANEOUS
Abstract

In the field of the synthesis and functionalization of iron-oxide nanoparticles (IONPs) for biomedical applications, most researches aimed at first at optimizing IONPs to be used as contrast agent for MRI. Then functionalized iron-oxide NPs have been also shown promising for therapy by magnetic hyperthermia (MH). The use of MH as a stand-alone or an adjacent therapy for cancer is closer to be a reality in every hospital to the positive results achieved by the clinical trials carried out by Magforce (Germany). Nonetheless, one of MH limitations is the low-power heating of usual magnetic NPs, requiring a local injection of large quantities of NPs. There is thus currently a challenge for optimizing the heating power of magnetic NPs. The amount of heat generated by magnetic NPs strongly depends on the NPs magnetic properties, which have to display high saturation magnetization and in particular high anisotropy energy, which depends strongly on their size, composition, and shape. The particle size distribution is also important as size distribution or energy barriers can cause overheating and undesired magnetic thermal ablation. Current developments for the synthesis of NPs optimized for MH rely on quality by design. Indeed first studies have shown that spherical IONPs with a mean size around 20 nm are suitable for clinical MH and progress in the NPs synthesis allowed synthesizing NPs with different shapes and core-shell structures which improved the NPs magnetic properties. Some intrinsic parameters of the NPs have thus been underlined as boosters for MH. Yet, the synthesis development/strategy remains empirical. In this chapter, we briefly list the features that can help increasing the heating values of NPs and we present an overview of the ways to control those NPs characteristics with the thermal decomposition synthesis method.

Published
2019

17. Magnetite- and Iodine-Containing Nanoemulsion as a Dual Modal Contrast Agent for X-ray/Magnetic Resonance Imaging

Author

Christophe A. Serra, Thierry F. Vandamme, Laurent Lemaire, Sylvie Begin-Colin, Francis Perton, Florence Franconi, Halina Anton, Nicolas Anton, Nadia Messaddeq, Hélène Libouban, Manuela Chiper, Justine Wallyn, Damien Mertz, Conception et application de molécules bioactives (CAMB), Université de Strasbourg (UNISTRA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut de Physique et Chimie des Matériaux de Strasbourg (IPCMS), 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)-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), Institut de chimie et procédés pour l'énergie, l'environnement et la santé (ICPEES), 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), Plate-forme de Recherche en Imagerie et Spectroscopie Multi-modales (PRISM [SFR ICAT - UA]), SFR UA 4208 Interactions Cellulaires et Applications Thérapeutiques (ICAT), Université d'Angers (UA)-Université d'Angers (UA), Micro et Nanomédecines Translationnelles (MINT), Université d'Angers (UA)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Biotechnologie et signalisation cellulaire (BSC), Université de Strasbourg (UNISTRA)-Centre National de la Recherche Scientifique (CNRS)-Institut de recherche de l'Ecole de biotechnologie de Strasbourg (IREBS), Groupe d'Études Remodelage Osseux et bioMatériaux (GEROM), Université d'Angers (UA), Institut de génétique et biologie moléculaire et cellulaire (IGBMC), Université Louis Pasteur - Strasbourg I-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Bioimagerie et Pathologies (LBP), and Université de Strasbourg (UNISTRA)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, Biocompatibility, [SDV.IB.IMA]Life Sciences [q-bio]/Bioengineering/Imaging, Contrast Media, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, chemistry.chemical_compound, Mice, [SDV.SP.MED]Life Sciences [q-bio]/Pharmaceutical sciences/Medication, In vivo, medicine, Animals, Humans, General Materials Science, Patient compliance, Magnetite Nanoparticles, ComputingMilieux_MISCELLANEOUS, Magnetite, medicine.diagnostic_test, X-ray, Magnetic resonance imaging, 021001 nanoscience & nanotechnology, Magnetic Resonance Imaging, 0104 chemical sciences, chemistry, Emulsions, Nanocarriers, 0210 nano-technology, Tomography, X-Ray Computed, Preclinical imaging, Biomedical engineering, HeLa Cells, Iodine
Abstract

Noninvasive diagnostic by imaging combined with a contrast agent (CA) is by now the most used technique to get insight into human bodies. X-ray and magnetic resonance imaging (MRI) are widely used technologies providing complementary results. Nowadays, it seems clear that bimodal CAs could be an emerging approach to increase the patient compliance, accessing different imaging modalities with a single CA injection. Owing to versatile designs, targeting properties, and high payload capacity, nanocarriers are considered as a viable solution to reach this goal. In this study, we investigated efficient superparamagnetic iron oxide nanoparticle (SPION)-loaded iodinated nano-emulsions (NEs) as dual modal injectable CAs for X-ray imaging and MRI. The strength of this new CA lies not only in its dual modal contrasting properties and biocompatibility, but also in the simplicity of the nanoparticulate assembling: iodinated oily core was synthesized by the triiodo-benzene group grafting on vitamin E (41.7% of iodine) via esterification, and SPIONs were produced by thermal decomposition during 2, 4, and 6 h to generate SPIONs with different morphologies and magnetic properties. SPIONs with most anisotropic shape and characterized by the highest r2/ r1 ratio once encapsulated into iodinated NE were used for animal experimentation. The in vivo investigation showed an excellent contrast modification because of the presence of the selected NEs, for both imaging techniques explored, that is, MRI and X-ray imaging. This work provides the description and in vivo application of a simple and efficient nanoparticulate system capable of enhancing contrast for both preclinical imaging modalities, MRI, and computed tomography.

Published
2018

18. Unravelling the Thermal Decomposition Parameters for The Synthesis of Anisotropic Iron Oxide Nanoparticles

Author

Christophe Lefevre, Simona Moldovan, Céline Kiefer, Sylvie Begin-Colin, Cristina Blanco-Andujar, Dris Ihiawakrim, Ovidiu Ersen, Benoit P. Pichon, Damien Mertz, Geoffrey Cotin, Francis Perton, Moldovan, Simona, Institut de Physique et Chimie des Matériaux de Strasbourg (IPCMS), Université de Strasbourg (UNISTRA)-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)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Réseau nanophotonique et optique, 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)-Centre National de la Recherche Scientifique (CNRS), Groupe de physique des matériaux (GPM), Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche sur les Matériaux Avancés (IRMA), Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), 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)-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), Centre National de la Recherche Scientifique (CNRS)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), and Normandie Université (NU)

Subjects
Materials science, synthesis, General Chemical Engineering, precursor, Iron oxide, Nucleation, Nanoparticle, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Article, lcsh:Chemistry, 03 medical and health sciences, chemistry.chemical_compound, Stearate, [CHIM] Chemical Sciences, [CHIM]Chemical Sciences, General Materials Science, shape control, thermal decomposition, 030304 developmental biology, 0303 health sciences, nanotechnology, 030302 biochemistry & molecular biology, Thermal decomposition, iron oxide nanoparticles, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Oleic acid, Magnetic hyperthermia, chemistry, Chemical engineering, lcsh:QD1-999, 0210 nano-technology, Iron oxide nanoparticles
Abstract

Iron oxide nanoparticles are widely used as a contrast agent in magnetic resonance imaging (MRI), and may be used as therapeutic agent for magnetic hyperthermia if they display in particular high magnetic anisotropy. Considering the effect of nanoparticles shape on anisotropy, a reproducible shape control of nanoparticles is a current synthesis challenge. By investigating reaction parameters, such as the iron precursor structure, its water content, but also the amount of the surfactant (sodium oleate) reported to control the shape, iron oxide nanoparticles with different shape and composition were obtained, in particular, iron oxide nanoplates. The effect of the surfactant coming from precursor was taking into account by using in house iron stearates bearing either two or three stearate chains and the negative effect of water on shape was confirmed by considering these precursors after their dehydration. Iron stearates with three chains in presence of a ratio sodium oleate/oleic acid 1:1 led mainly to nanocubes presenting a core-shell Fe1&minus, xO@Fe3&minus, xO4 composition. Nanocubes with straight faces were only obtained with dehydrated precursors. Meanwhile, iron stearates with two chains led preferentially to the formation of nanoplates with a ratio sodium oleate/oleic acid 4:1. The rarely reported flat shape of the plates was confirmed with 3D transmission electronic microscopy (TEM) tomography. The investigation of the synthesis mechanisms confirmed the major role of chelating ligand and of the heating rate to drive the cubic shape of nanoparticles and showed that the nanoplate formation would depend mainly on the nucleation step and possibly on the presence of a given ratio of oleic acid and chelating ligand (oleate and/or stearate).

Published
2018

19. Unveiling the role of surface, size, shape and defects of iron oxide nanoparticles for theranostic applications

Author

Delphine Felder-Flesch, Francisco J. Teran, Sophie Laurent, Gianluigi A. Botton, Céline Henoumont, Céline Kiefer, Florent Meyer, Jean-Marc Greneche, Wilfried Reichardt, Ovidiu Ersen, Jesús M. de la Fuente, Michael Chatzidakis, Geoffrey Cotin, Daniel Ortega, Dinh-Vu Ngyen, Damien Mertz, Simo Spassov, Sylvie Begin-Colin, Laura Asín, Denise Schaffner, Francis Perton, Cristina Blanco-Andujar, Région Alsace, Université de Strasbourg, Interreg POCTEFA, National Fund for Scientific Research (Belgium), Fonds de la Recherche Scientifique (Fédération Wallonie-Bruxelles), European Commission, Ministerio de Economía y Competitividad (España), Agencia Estatal de Investigación (España), Comunidad de Madrid, Diputación General de Aragón, Ministerio de Ciencia, Innovación y Universidades (España), Institut de Physique et Chimie des Matériaux de Strasbourg (IPCMS), Université Louis Pasteur - Strasbourg I-Centre National de la Recherche Scientifique (CNRS), 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)-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), Biomatériaux et Bioingénierie (BB), 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)-Institut National de la Santé et de la Recherche Médicale (INSERM)

Subjects
Biodistribution, [SDV.BIO]Life Sciences [q-bio]/Biotechnology, Materials science, Contrast Media, Nanotechnology, 02 engineering and technology, [CHIM.THER]Chemical Sciences/Medicinal Chemistry, engineering.material, 010402 general chemistry, 01 natural sciences, Ferric Compounds, Theranostic Nanomedicine, chemistry.chemical_compound, Magnetics, Coating, Dendrimer, General Materials Science, Tumor growth, Tissue Distribution, Precision Medicine, Magnetite Nanoparticles, Relaxation (NMR), [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Magnetic Resonance Imaging, 3. Good health, 0104 chemical sciences, Magnetic field, Magnetic hyperthermia, chemistry, engineering, Magnetic Iron Oxide Nanoparticles, 0210 nano-technology, Iron oxide nanoparticles
Abstract

Iron oxide nanoparticles (IONPs) are well-known contrast agents for MRI for a wide range of sizes and shapes. Their use as theranostic agents requires a better understanding of their magnetic hyperthermia properties and also the design of a biocompatible coating ensuring their stealth and a good biodistribution to allow targeting of specific diseases. Here, biocompatible IONPs of two different shapes (spherical and octopod) were designed and tested in vitro and in vivo to evaluate their abilities as high-end theranostic agents. IONPs featured a dendron coating that was shown to provide anti-fouling properties and a small hydrodynamic size favoring an in vivo circulation of the dendronized IONPs. While dendronized nanospheres of about 22 nm size revealed good combined theranostic properties (r2 = 303 mM s−1, SAR = 395 W gFe−1), octopods with a mean size of 18 nm displayed unprecedented characteristics to simultaneously act as MRI contrast agents and magnetic hyperthermia agents (r2 = 405 mM s−1, SAR = 950 W gFe−1). The extensive structural and magnetic characterization of the two dendronized IONPs reveals clear shape, surface and defect effects explaining their high performance. The octopods seem to induce unusual surface effects evidenced by different characterization techniques while the nanospheres show high internal defects favoring Néel relaxation for magnetic hyperthermia. The study of octopods with different sizes showed that Néel relaxation dominates at sizes below 20 nm while the Brownian one occurs at higher sizes. In vitro experiments demonstrated that the magnetic heating capability of octopods occurs especially at low frequencies. The coupling of a small amount of glucose on dendronized octopods succeeded in internalizing them and showing an effect of MH on tumor growth. All measurements evidenced a particular signature of octopods, which is attributed to higher anisotropy, surface effects and/or magnetic field inhomogeneity induced by tips. This approach aiming at an analysis of the structure–property relationships is important to design efficient theranostic nanoparticles., The Region Alsace, France, and the Labex Chimie des Systemes Complexes, University of Strasbourg, France are gratefully acknowledged for the doctoral fellowship to Geoffrey Cotin. This research project was also co-funded by Labex CSC, Alsace contre le cancer, INCA (project PRTK14, THERAMAG 2014-225) and the INTERREG project NANOTRANSMED. The “NANOTRANSMED” project is co-funded by the European Regional Development Fund (ERDF) and by the Swiss Confederation and the Swiss cantons of Aargau, Basel-Landschaft and Basel-Stadt, in the framework of the INTERREG V Upper Rhine program (“Transcending borders with every project”). The authors thank Morgane Rabineau for epifluorescence imaging and Nadia Messaddeq for TEM imaging of cells. The authors thank the Center for Microscopy and Molecular Imaging (CMMI, supported by the European Regional Development Fund and the Walloon Region). This work was supported by the Fond National de la Recherche Scientifique (FNRS), UIAP VII, ARC Programs of the French Community of Belgium and the Walloon region (Gadolymph and Holocancer programs). All the authors acknowledge the COST action TD1402 “RADIOMAG”. D. Ortega and F. J. Teran acknowledge support from the ‘Severo Ochoa’ Programme for Centres of Excellence in R&D (MINECO, Grant SEV-2016-0686), the Spanish Ministry of Economy and Competitiveness for the NANOLICO project (MAT2017-85617-R), the Spanish Ministry of Science through the NaNoCAR grant PID2020-117544RB-I00, the Ramón y Cajal grant RYC2018-025253-I and Research Networks grant RED2018-102626-T, the HEATOOLS project (BIO2017-84246-C2-1-R), the Comunidad de Madrid for grant NANOMAGCOST (P2018/NMT-4321), DGA for public funding from Fondo Social (grupos DGA), and the European Commission for the funding received through the H2020 “NoCanTher” project (GA No. 685795).

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20. Evaluating the Critical Roles of Precursor Nature and Water Content When Tailoring Magnetic Nanoparticles for Specific Applications

Author

Geoffrey Cotin, Francis Perton, Burak Özdamar, Mauro Boero, Assil Bouzid, Guido Ori, Damien Mertz, Dominique Begin, Sylvie Begin-Colin, Carlo Massobrio, Céline Kiefer, Benoit P. Pichon, Institut de Physique et Chimie des Matériaux de Strasbourg (IPCMS), 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)-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 Louis Pasteur - Strasbourg I-Centre National de la Recherche Scientifique (CNRS), Institut de chimie et procédés pour l'énergie, l'environnement et la santé (ICPEES), 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
iron oxide, Materials science, molecular-dynamics, Iron oxide, 1st principles, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, [SPI.MAT]Engineering Sciences [physics]/Materials, chemistry.chemical_compound, iron precursor, On demand, [CHIM]Chemical Sciences, General Materials Science, high values, hydration rate, synthesis mechanism, Water content, hot-injection, ComputingMilieux_MISCELLANEOUS, thermal decomposition, shape control, Range (particle radiation), Thermal decomposition, modeling, semiconductor, 021001 nanoscience & nanotechnology, 0104 chemical sciences, [CHIM.THEO]Chemical Sciences/Theoretical and/or physical chemistry, chemistry, Chemical engineering, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], Magnetic nanoparticles, 1st-principles, iron-oxide nanoparticles, 0210 nano-technology, Iron oxide nanoparticles, nanocrystal synthesis, energy
Abstract

Because of the broad range of application of iron oxide nanoparticles (NPs), the control of their size and shape on demand remains a great challenge, as these parameters are of upmost importance to provide NPs with magnetic properties tailored to the targeted application. One promising synthesis process to tune their size and shape is the thermal decomposition one, for which a lot of parameters were investigated. But two crucial issues were scarcely addressed: the precursors nature and water content. Two in house iron stearates with two or three stearate chains were synthesized, dehydrated, and then tested in standard synthesis conditions of spherical and cubic NPs. Investigations combined with modeling showed that the precursors nature and hydration rate strongly affect the thermal decomposition kinetics and yields, which, in turn, influence the NP size. The cubic shape depends on the decomposition kinetics but also crucially on the water content. A microscopic insight was provided by first-principles simulation showing an iron reduction along the reaction pathway and a participation of water molecules to the building unit formation.

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