References of "Detrembleur, Christophe"
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See detailLinear amphiphilic diblock copolymers of lactide and 2-dimethylaminoethyl methacrylate using bifunctional-initiator and one-pot approaches
Kryuchkov, Maksym A.; Detrembleur, Christophe ULg; Bazuin, Géraldine

in Polymer (2014), 55(10), 2316-2324

Linear amphiphilic diblock copolymers of polylactide (PLA) and poly(2-dimethylaminoethyl methacrylate) (PDMAEMA) were synthesized by atom transfer radical polymerization (ATRP) of DMAEMA followed by ring ... [more ▼]

Linear amphiphilic diblock copolymers of polylactide (PLA) and poly(2-dimethylaminoethyl methacrylate) (PDMAEMA) were synthesized by atom transfer radical polymerization (ATRP) of DMAEMA followed by ring-opening polymerization (ROP) of LLA using the bifunctional initiator, 2′-hydroxyethyl 2-bromoisobutyrate. NMR showed that the resulting PLA block was racemic and a quaternization/precipitation technique showed that there were significant amounts of racemic PLA homopolymer. In addition, simultaneous ATRP of DMAEMA and ROP of l-lactide by tin octoate were conducted at varied temperatures, indicating 90 °C as a suitable compromise temperature; this one-pot process also led to racemization and P(L)LA homopolymer. The racemization was attributed to reversible deprotonation of LLA by the N(CH3)2 moiety of (P)DMAEMA and the PLA homopolymer impurity was related to in situ formation of lactoyl lactate (LA–LA) due to nucleophilic ring opening of lactide by the amino moieties of (P)DMAEMA. The methods presented can be useful for the preparation of PDMAEMA–b–PLA/PLA composites in a two-step process or in a single step, one-pot process. [less ▲]

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See detailSupercritical CO2 and polycarbonate based nanocomposites: A critical issue for foaming
Monnereau, Laure; Urbanczyk, Laetitia; Thomassin, Jean-Michel ULg et al

in Polymer (2014), 55(10), 2422-2431

Supercritical carbon dioxide readily induced foaming of various polymers. In that context, supercritical CO2 was applied to carbon nanotubes based polycarbonate nanocomposites to ensure their foaming ... [more ▼]

Supercritical carbon dioxide readily induced foaming of various polymers. In that context, supercritical CO2 was applied to carbon nanotubes based polycarbonate nanocomposites to ensure their foaming. Surprisingly, efficient foaming only occurs when low pressure is applied while at high pressure, no expansion of the samples was observed. This is related to the ability of supercritical carbon dioxide to induce crystallization of amorphous polycarbonate. Moreover, this behaviour is amplified by the presence of carbon nanotubes that act as nucleating agents for crystals birth. The thermal behaviour of the composites was analysed by DSC and DMA and was related to the foaming observations. The uniformity of the cellular structure was analysed by scanning electron microscopy (SEM). By saturating the polycarbonate nanocomposites reinforced with 1 wt% of MWNTs at 100 bar and 100 °C during 16 h, microcellular foams were generated, with a density of 0.62, a cell size ranging from 0.6 to 4 μm, and a cellular density of 4.1 × 1011 cells cm−3. The high ability of these polymeric foams to absorb electromagnetic radiation was demonstrated at low MWNT content as the result of the high affinity of the polycarbonate matrix for MWNTs, and therefore to the good MWNTs dispersion. [less ▲]

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See detailPoly(methyl methacrylate)/graphene oxide nanocomposites by a precipitation polymerization process and their dielectric and rheological characterization
Thomassin, Jean-Michel ULg; Trifkovic, Milana; Alkarmo, Walid et al

in Macromolecules (2014), 47(6), 2149-2155

We report a method for achieving controlled dispersion of graphene oxide (GO) in poly(methyl methacrylate) (PMMA) via the precipitation polymerization process in a water/ methanol mixture. GO acts as a ... [more ▼]

We report a method for achieving controlled dispersion of graphene oxide (GO) in poly(methyl methacrylate) (PMMA) via the precipitation polymerization process in a water/ methanol mixture. GO acts as a surfactant and adsorbs on the interface between polymerized PMMA particles and solvent mixture. Scanning electron and transmission electron microscopy confirmed that the precipitate consists of polymer particles (<1 μm) surrounded by the GO sheets. Compression molding of the precipitate yields a polymer nanocomposite with the GO organized into a regularly spaced 3D network which percolates at 0.2 wt % GO. Simple thermal reduction of the GO sheets dispersed in PMMA at relatively low temperature (210 °C) achieved electrical conductivity higher than 10−2 S/m at 0.4 wt % of GO. Parallel dielectric and rheological characterization demonstrated that the thermal reduction is a quite fast process without significant degradation of the polymer. The study should open up new opportunities in the design of GO-based polymer nanocomposites. [less ▲]

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See detail(Co)Polymerization of vinyl levulinate by cobalt-mediated radical polymerization and functionalization by ketoxime click chemistry
Allaoua, Imène; Eleuterio, Beatriz; Obadia, Mona M. et al

in Polymer Chemistry (2014), 5(8), 2973-2979

Vinyl levulinate is synthesized from levulinic acid by palladium-catalyzed vinyl exchange and is characterized by NMR and ESI-HRMS techniques. Homopolymerization of vinyl levulinate and random ... [more ▼]

Vinyl levulinate is synthesized from levulinic acid by palladium-catalyzed vinyl exchange and is characterized by NMR and ESI-HRMS techniques. Homopolymerization of vinyl levulinate and random copolymerization with vinyl acetate by cobalt-mediated radical polymerization affords well-defined ketone functionalized poly(vinyl ester)s. The impact of temperature, solvent and theoretical degree of polymerization on monomer conversion and control of the polymerization is studied by 1H NMR and size exclusion chromatography techniques. The ketoxime conjugation of O-benzylhydroxylamine with the pendant ketone functionality of poly(vinyl levulinate-co-vinyl acetate) is demonstrated. [less ▲]

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See detailGreen and bio-inspired processes for the functionalization of surfaces
Detrembleur, Christophe ULg

Conference (2014, March 18)

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See detailPrecision design of ethylene- and polar-monomer-based copolymers by organometallic-mediated radical polymerization
Kermagoret, Anthony ULg; Debuigne, Antoine ULg; Jérôme, Christine ULg et al

in Nature Chemistry (2014), 6(3), 179-187

The copolymerization of ethylene with polar monomers is a major challenge when it comes to the manufacture of materials with potential for a wide range of commercial applications. In the chemical industry ... [more ▼]

The copolymerization of ethylene with polar monomers is a major challenge when it comes to the manufacture of materials with potential for a wide range of commercial applications. In the chemical industry, free-radical polymerization is used to make a large proportion of such copolymers, but the forcing conditions result in a lack of fine control over the architecture of the products. Herein we introduce a synthetic tool, effective under mild experimental conditions, for the precision design of unprecedented ethylene- and polar-monomer-based copolymers. We demonstrate how an organocobalt species can control the growth of the copolymer chains, their composition and the monomer distribution throughout the chain. By fine tuning the ethylene pressure during polymerization and by exploiting a unique reactive mode of the end of the organometallic chain, novel block-like copolymer structures can be prepared. This highly versatile synthetic platform provides access to a diverse range of polymer materials. [less ▲]

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See detailGlucose-, pH- and thermo-responsive nanogels crosslinked by functional superparamagnetic maghemite nanoparticles as innovative drug delivery systems
Liu, Ji ULg; Detrembleur, Christophe ULg; Debuigne, Antoine ULg et al

in Journal of Materials Chemistry B (2014), 2(8), 1009-1023

Reversibly crosslinked (RCL) nanogels made of thermo-responsive poly(vinyl alcohol)-b-poly(Nvinylcaprolactam) copolymers were combined with maghemite nanoparticles and developed as new drug delivery ... [more ▼]

Reversibly crosslinked (RCL) nanogels made of thermo-responsive poly(vinyl alcohol)-b-poly(Nvinylcaprolactam) copolymers were combined with maghemite nanoparticles and developed as new drug delivery systems (DDS). The crosslinking was formed via boronate/diol bonding from the surfacefunctionalized superparamagnetic maghemite nanoparticles, endowing the DDS with thermo-, pH- and glucose-responsiveness. The capability to load a hydrophobic drug model Nile red (NR) within the RCL nanogels was evaluated, and stimuli-triggered drug release behaviours under different conditions were tested. Zero premature release behaviour was detected at physiological pH in the absence of glucose, whereas triggered release was observed upon exposure to acidic pH (5.0) and/or in the presence of glucose. In light of the superparamagnetic properties of the maghemite nanoparticles and RCL nanogels, magnetically-induced heating, MR imaging performance, as well as remotely magnetically-triggered drug release under alternating magnetic field (AMF), were investigated. Cytotoxicity against fibroblast-like L929 and human melanoma MEL-5 cell lines was assessed via the MTS assay. In vitro stimuli-triggered release of tamoxifen, a chemotherapeutic drug, was also studied within MEL-5 cell cultures under different conditions. These innovative RCL nanogels, integrating different stimuli-responsive components, hydrophobic chemotherapeutic moieties and also diagnostic agents together via reversible crosslinking, are promising new theranostic platforms. [less ▲]

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See detailGold nanorods coated with a thermo-responsive poly(ethylene glycol)-b-poly(N-vinylcaprolactam) corona as drug delivery systems for remotely near infrared-triggered release
Liu, Ji ULg; Detrembleur, Christophe ULg; De Pauw-Gillet, Marie-Claire ULg et al

in Polymer Chemistry (2014), 5(3), 799-813

Poly(ethylene glycol)-b-poly(N-vinylcaprolactam) (PEG-b-PNVCL) copolymers are prepared from a PEG macro-chain transfer agent in DMF at 65 °C via reversible addition-fragmentation chain transfer (RAFT ... [more ▼]

Poly(ethylene glycol)-b-poly(N-vinylcaprolactam) (PEG-b-PNVCL) copolymers are prepared from a PEG macro-chain transfer agent in DMF at 65 °C via reversible addition-fragmentation chain transfer (RAFT) polymerization. The well-defined PEG114-b-PNVCL237 copolymer with a cloud point temperature of 39 °C is used for the formation of a thermo-responsive polymer corona on the surface of gold nanorods (GNRs) via a “grafting-to” approach. Thermo-responsiveness and thermo-dependent optical properties of the as-obtained GNR@PEG-b-PNVCL nanoparticles are studied with dynamic light scattering and UV/vis spectroscopy techniques. Near infrared (NIR)-induced heating of GNR@PEG-b-PNVCL is also explored in aqueous suspension under NIR laser irradiation (802 nm, up to 250 mW). The potential of these GNR@PEG-b-PNVCL nanoparticles to be used as smart drug delivery systems (DDS) is then studied. A hydrophilic drug model, Rhodamine ® B, is used to assess the guest loading capacity, and triggered release behaviours are then evaluated under conventional external heating or internal heating induced by remote NIR irradiation. Cytotoxicity evaluation of the GNR@PEG-b-PNVCL against the fibroblast-like L929 cell line is carried out via the MTS assay in order to confirm the improved biocompatibility of the GNRs after polymer coating. These thermo-responsive GNR@PEG-b-PNVCL nanoparticles are promising DDS that combine the chemotherapeutic and phototherapeutic functions. [less ▲]

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See detailPrecision synthesis of poly(ionic liquid)-based block copolymers by cobalt-mediated radical polymerization and preliminary study of their self-assembling properties
Coupillaud, Paul; Fèvre, Maréva; Wirotius, Anne-Laure et al

in Macromolecular Rapid Communications (2014), 35(4), 422-430

A poly(ionic liquid)-based block copolymer (PIL BCP), namely, poly(vinyl acetate)-b-poly(N-vinyl-3-butylimidazolium bromide), PVAc-b-PVBuImBr, is synthesized by sequential cobalt-mediated radical ... [more ▼]

A poly(ionic liquid)-based block copolymer (PIL BCP), namely, poly(vinyl acetate)-b-poly(N-vinyl-3-butylimidazolium bromide), PVAc-b-PVBuImBr, is synthesized by sequential cobalt-mediated radical polymerization (CMRP). A PVAc precursor is first prepared at 30 °C in bulk by CMRP of VAc, using bis(acetylacetonato)cobalt(II), Co(acac)2, and a radical source (V-70). Growth of PVBuImBr from PVAc-Co(acac)2 is accomplished by CMRP in DMF/MeOH (2:1, v/v). This PIL BCP self-assembles in the sub-micron size range into aggregated core–shell micelles in THF, whereas polymeric vesicles are observed in water, as evidenced by dynamic light scattering (DLS) and transmission electron microscopy (TEM). Thin-solid sample cut from raw materials analyzed by TEM shows an ordered lamellar organization by temperature-dependent synchrotron small-angle X-ray scattering (SAXS). Anion exchange can be accomplished to achieve the corresponding PIL BCP with bis(trifluorosulfonyl)imide (Tf2N−) anions, which also gives rise to an ordered lamellar phase in bulk samples. A complete suppression of SAXS second-order reflection suggests that this compound has a symmetric volume fraction (f ≈ 0.5). SAXS characterization of both di- and triblock PIL BCP analogues previously reported also shows a lamellar phase of very similar behavior, with only an increase of the period by about 8% at 60 °C. [less ▲]

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See detailHeat-triggered drug release systems based on mesoporous silica nanoparticles filled with a maghemite core and phase-change molecules as gatekeepers
Liu, Ji ULg; Detrembleur, Christophe ULg; De Pauw-Gillet, Marie-Claire ULg et al

in Journal of Materials Chemistry B (2014), 2(1), 59-70

Core–shell nanoparticlesmade of a maghemite core and a mesoporous silica shell were developed as drug delivery systems (DDS). Doxorubicin® (DOX, DNA intercalating drug) was loaded within the mesoporous ... [more ▼]

Core–shell nanoparticlesmade of a maghemite core and a mesoporous silica shell were developed as drug delivery systems (DDS). Doxorubicin® (DOX, DNA intercalating drug) was loaded within the mesoporous cavities, while phase-change molecules (PCMs), e.g. 1-tetradecanol (TD) with a melting temperature (Tm) of 39 °C, were introduced as gatekeepers to regulate the release behaviours. An overall loading amount of ca. 20 wt% (TD/DOX ca. 50/50 wt/wt) was confirmed. Heat-triggered release of DOX evidenced a “zero premature release” (<3% of the entire payload in 96 h release) under physiological conditions (37°C), and however, a sustainable release (ca. 40% of the entire payload in 96 h) above Tm of TD (40 °C). It also demonstrated the possibility to deliver drug payloads in small portions (pulsatile release mode) via multiple heating on/off cycles, due to the reversible phase change of the PCMs. In vitro heattriggered release of DOX within cell culture of the MEL-5 melanoma cell line was also tested. It was found that DOX molecules were trapped efficiently within the mesopores even after internalization within the cytoplasm of MEL-5 cells at 37 °C, with the potential toxicity of DOX strongly quenched (>95% viability after 72 h incubation). However, continuous cell apoptosis was detected at cell culture temperature above Tm of TD, due to the heat-triggered release of DOX (<50% viability after 72 h incubation at 40 °C). Moreover, due to the presence of a maghemite core within the DDS, T2-weighted magnetic resonance imaging performance was also confirmed. These as-designed core–shell nanoparticles are envisaged to become promising DDS for “on-demand” heat-triggered release. [less ▲]

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See detailReversibly crosslinked thermo- and redox-responsive nanogels for controlled drug release
Liu, Ji ULg; Detrembleur, Christophe ULg; Hurtgen, Marie ULg et al

in Polymer Chemistry (2014), 5(1), 77-88

Reversibly crosslinked poly(vinyl alcohol)-b-poly(N-vinylcaprolactam) PVOH-b-PNVCL nanogels were prepared by using a redox-responsive crosslinking agent, 3,30-dithiodipropionic acid (DPA), to crosslink ... [more ▼]

Reversibly crosslinked poly(vinyl alcohol)-b-poly(N-vinylcaprolactam) PVOH-b-PNVCL nanogels were prepared by using a redox-responsive crosslinking agent, 3,30-dithiodipropionic acid (DPA), to crosslink the PVOH corona, above the lower critical solution temperature (LCST) of the PNVCL block. The stability of the as-prepared nanogels against heating and diluting with water was studied by dynamic light scattering (DLS) to follow the evolution of the hydrodynamic diameter and size distribution. Stability under reductive conditions was also studied by DLS and transmission electron microscopy (TEM) after exposure to dithiothreitol (DTT) buffer solutions at different pH. The reversibility of the crosslinking was evaluated by treating the de-crosslinked nanogels with hydrogen peroxide (H2O2) above the LCST. As a hydrophobic drug model, Nile red (NR) was loaded into the nanogels, and triggered release behaviours were studied after exposure to the same DTT buffer solutions. Moreover, two PVOH-b-PNVCL copolymers with different compositions and LCST were used to evaluate the effect of the LCST on the release behaviours of the nanogels. The cytotoxicity of the nanogels against a mouse fibroblast-like L929 cell line was assessed via the MTS assay, and preliminary studies on cellular uptake of the nanogels within human melanoma MEL-5 cells were also carried out by fluorescence microscopy and fluorescence-activated cell sorting. [less ▲]

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See detailExpanding the scope of controlled radical polymerization via cobalt–tellurium radical exchange reaction
Kermagoret, Anthony ULg; Nakamura, Yasuyuki; Bourguignon, Maxime et al

in ACS Macro Letters (2014), 3(1), 114-118

Cobalt-mediated radical polymerization (CMRP) and tellurium-mediated radical polymerization (TERP) were combined for the first time, offering new perspectives in the precision design of macromolecular ... [more ▼]

Cobalt-mediated radical polymerization (CMRP) and tellurium-mediated radical polymerization (TERP) were combined for the first time, offering new perspectives in the precision design of macromolecular structures. In particular, the present work highlights the benefits of this strategy for the synthesis of novel poly(vinyl acetate)-based block copolymers. A range of well-defined poly(vinyl acetate)s (PVAc) were first produced via CMRP using the bis(acetylacetonato)cobalt(II) complex (Co(acac)2) as a regulating agent. Substitution of a methyltellanyl moiety for Co(acac)2 at the ω-chain end of the precursor was then achieved upon treatment with dimethylditelluride. In contrast to the PVAc prepared by TERP, the ones produced by sequential CMRP and Co/Te exchange reaction almost exclusively consist of regular head-to-tail-TeMe chain-end species that can be activated by TERP. Ultimately, a series of monomers problematic in Co(acac)2-mediated radical polymerization including N-isopropylacrylamide (NIPAM), 2-(dimethylamino)ethyl acrylate (ADAME), n-butyl acrylate (BA), isoprene (IP), and vinylimidazole (NVIm) were polymerized by TERP from the PVAc–TeMe macroinitiators leading to novel diblock copolymers that cannot be made by each technique used separately. [less ▲]

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See detailGold nanorods with phase-changing polymer corona for remotely near-infrared-triggered drug release
Liu, Ji ULg; Detrembleur, Christophe ULg; Grignard, Bruno ULg et al

in Chemistry : An Asian Journal (2014), 9(1), 275-288

Herein, we report a new drug-delivery system (DDS) that is comprised of a near-infrared (NIR)- light-sensitive gold-nanorod (GNR) core and a phase-changing poly(e-caprolactone)- b-poly(ethylene glycol ... [more ▼]

Herein, we report a new drug-delivery system (DDS) that is comprised of a near-infrared (NIR)- light-sensitive gold-nanorod (GNR) core and a phase-changing poly(e-caprolactone)- b-poly(ethylene glycol) polymer corona (GNR@PCL-b-PEG). The underlying mechanism of the drugloading and triggered-release behaviors involves the entrapment of drug payloads among the PCL crystallites and a heat-induced phase change, respectively. A low premature release of the pre-loaded doxorubicin was observed in PBS buffer (pH 7.4) at 37 °C (<10% of the entire payload after 48 h). However, release could be activated within 30 min by conventional heating at 50 °C, above the Tm of the crystalline PCL domain (43.5 °C), with about 60% release over the subsequent 42 h at 37 °C. The NIR-induced heating of an aqueous suspension of GNR@PCL-b- PEG under NIR irradiation (802 nm) was investigated in terms of the irradiation period, power, and concentrationdependent heating behavior, as well as the NIR-induced shape-transformation of the GNR cores. Remotely NIR-triggered release was also explored upon NIR irradiation for 30 min and about 70% release was achieved in the following 42 h at 37°C, with a mild warming (<4 °C) of the surroundings. The cytotoxicity of GNR@PCL-b-PEG against the mouse fibroblastic-like L929 cell-line was assessed by MTS assay and good compatibility was confirmed with a cell viability of over 90% after incubation for 72 h. The cellular uptake of GNR@PCL-b-PEG by melanoma MEL-5 cells was also confirmed, with an averaged uptake of 1250 ( ± 110) particles cell-1 after incubation for 12 h (50 mg mL-1). This GNR@PCL-b-PEG DDS is aimed at addressing the different requirements for therapeutic treatments and is envisaged to provide new insights into DDS targeting for remotely triggered release by NIR activation. [less ▲]

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See detailNitroaldol condensation catalyzed by topologically modulable cooperative acid–base chitosan–TiO2 hybrid materials
Aqil, Abdelhafid ULg; El Kadib, Abdelkrim; Aqil, Mohamed ULg et al

in RSC Advances (2014), 4(63), 33360-33363

Chitosan–TiO2 shaped as macroporous aerogels, lamellar cryogels or electrospun films act synergistically as acid–base bifunctional catalysts. Depending on the topology of the material, a marked difference ... [more ▼]

Chitosan–TiO2 shaped as macroporous aerogels, lamellar cryogels or electrospun films act synergistically as acid–base bifunctional catalysts. Depending on the topology of the material, a marked difference in the selectivity for nitroaldol condensation is observed. [less ▲]

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See detailNitroxide mediated polymerization of methacrylates at moderate temperature
Detrembleur, Christophe ULg; Jérôme, Christine ULg; De Winter, Julien et al

in Polymer Chemistry (2014), 5(2), 335-340

In this communication we report the first homopolymerization of a variety of methacrylates by an NMP process at moderate temperature (40–50 °C), using an easily accessible and inexpensive nitroxide ... [more ▼]

In this communication we report the first homopolymerization of a variety of methacrylates by an NMP process at moderate temperature (40–50 °C), using an easily accessible and inexpensive nitroxide precursor. The combination of a low temperature azo-initiator with a hindered nitroso-compound produces a mixture of hindered nitroxides in the polymerization medium that act as efficient polymerization control agents. Results of Electron Spin Resonance (ESR) spectroscopy experiments combined with mass spectrometric studies support the proposed in situ NMP mechanism. The hindered structure of the nitroxides formed in situ is believed to be responsible for the efficiency of the process by allowing it to proceed at low temperature, therefore limiting the side reactions generally observed in NMP of methacrylates. [less ▲]

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See detailPoly(acrylic acid)-block-poly(vinyl alcohol) anchored maghemite nanoparticles designed for multi-stimuli triggered drug release
Liu, Ji ULg; Detrembleur, Christophe ULg; Debuigne, Antoine ULg et al

in Nanoscale (2013), 5(23), 11464-11477

Original core/corona nanoparticles composed of amaghemite core and a stimuli-responsive polymer coating made of poly(acrylic acid)-block-poly(vinyl alcohol) macromolecules were fabricated for drug ... [more ▼]

Original core/corona nanoparticles composed of amaghemite core and a stimuli-responsive polymer coating made of poly(acrylic acid)-block-poly(vinyl alcohol) macromolecules were fabricated for drug delivery system (DDS) application. This kind of DDS aims to combine the advantage of stimuli-responsive polymer coating, in order to regulate the drug release behaviours under different conditions and furthermore, improve the biocompatibility and in vivo circulation half-time of the maghemite nanoparticles. Drug loading capacity was evaluated with methylene blue (MB), a cationic model drug. The triggered release of MB was studied under various stimuli such as pH, ionic strength and temperature. Local heating generated under alternating magnetic field (AMF) application was studied, and remotely AMF-triggered release was also confirmed, while a mild heating-up of the release medium was observed. Furthermore, their potential application as magnetic resonance imaging (MRI) contrast agents was explored via relaxivity measurements and acquisition of T2-weighted images. Preliminary studies on the cytotoxicity against mouse fibroblast-like L929 cell line and also their cellular uptake within human melanoma MEL-5 cell line were carried out. In conclusion, this kind of stimuli-responsive nanoparticles appears to be promising carriers for delivering drugs to some tumour sites or into cellular compartments with an acidic environment. [less ▲]

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