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Synthesis and Characterization of Superparamagnetic Nanoparticles View metadata, citation and similar papers at core.ac.uk brought to you by CORE provided by Archive Ouverte en Sciences de l'Information et de la Communication Synthesis and characterization of superparamagnetic nanoparticles coated with fluorescent gold nanoclusters Xavier Le Guével, Eva-Marie Prinz, Robert Müller, Rolf Hempelmann, Marc Schneider To cite this version: Xavier Le Guével, Eva-Marie Prinz, Robert Müller, Rolf Hempelmann, Marc Schneider. Synthesis and characterization of superparamagnetic nanoparticles coated with fluorescent gold nanoclusters. Journal of Nanoparticle Research, Springer Verlag, 2012, 14 (4), pp.727. hal-02337892 HAL Id: hal-02337892 https://hal.archives-ouvertes.fr/hal-02337892 Submitted on 6 Nov 2019 HAL is a multi-disciplinary open access L’archive ouverte pluridisciplinaire HAL, est archive for the deposit and dissemination of sci- destinée au dépôt et à la diffusion de documents entific research documents, whether they are pub- scientifiques de niveau recherche, publiés ou non, lished or not. The documents may come from émanant des établissements d’enseignement et de teaching and research institutions in France or recherche français ou étrangers, des laboratoires abroad, or from public or private research centers. publics ou privés. J Nanopart Res (2012) 14:727 DOI 10.1007/s11051-012-0727-6 RESEARCH PAPER Synthesis and characterization of superparamagnetic nanoparticles coated with fluorescent gold nanoclusters Xavier Le Gue´vel • Eva-Marie Prinz • Robert Mu¨ller • Rolf Hempelmann • Marc Schneider Received: 26 June 2011 / Accepted: 5 January 2012 Ó Springer Science+Business Media B.V. 2012 Abstract Multifunctional nanoparticles (NPs) com- kept the original fluorescence property of the metal bining the superparamagnetism of Mn-Zn ferrite and clusters with 211-fold increase of the red emission the fluorescence property of gold nanoclusters (NCs) (k = 690 nm) compared to the uncoated NPs. These have been prepared by wet chemistry. Magnetic NPs NPs can be moved with a permanent magnet despite a synthesized by co-precipitation method were coated 72-wt% increase of the non-magnetic fraction due to several times with oppositely charged polyelectrolytes the PE coating and the protein adsorption. (PEs) using the layer-by-layer technique. Common techniques (Fourier transform infrared spectroscopy, Keywords Nanoparticles Á Gold Á Nanoclusters Á electron microscopy, zeta potential, etc.) indicated the Fluorescence Á Superparamagnetism Á Biomedicine monodispersity and the stability of the coated NPs providing a positive charged surface. Fluorescent gold NCs bound to a standard protein bovine serum Introduction albumin were adsorbed on the surface of the magnetic NPs. Structural investigations proved the presence of In recent years, multifunctional nanoscaled particu- small gold clusters (*2 nm) in a shell surrounding the lates in a single entity have attracted great attention for magnetic nanomaterial. The stable nanocomposite their diagnostic and biomedical application (Alexiou et al. 2006; Jain et al. 2008; Liong et al. 2008; Sukhorukov and Mohwald 2007; Zhang et al. 2007). Electronic supplementary material The online version of Especially, the combination of magnetic and optical this article (doi:10.1007/s11051-012-0727-6) contains imaging into a nanostructured system would greatly supplementary material, which is available to authorized users. inspire and support in vitro diagnosis as well as the in X. Le Gue´vel (&) Á M. Schneider vivo monitoring of living cells and then open up the Pharmaceutical Nanotechnology, Saarland University, unique possibility of controlled target-directed appli- Saarbru¨cken, Germany cations (Kim et al. 2009; Koole et al. 2009). These e-mail: [email protected] nanosystems offer a promising approach to serve as all E.-M. Prinz Á R. Hempelmann in one diagnostic and nano-sized drug delivery Department of Physical Chemistry, Saarland University, carriers. For example, in the last few years, several Saarbru¨cken, Germany researchers demonstrated the potential to combine MRI contrast agent and fluorescent organic dyes that R. Mu¨ller Institute of Photonic Technology, P.O. Box 100239, Jena, can allow the detection of cancer through non-invasive Germany MRI and the optical guide during surgery (Veiseh 123 Page 2 of 10 J Nanopart Res (2012) 14:727 et al. 2005; Bridot et al. 2007; Lee et al. 2010). Such nanomaterial for biological applications is the bio- bifunctional nanocomposites have been prepared by compatibility of Mn-Zn ferrite (Beji et al. 2010) and several routes notably by a combination of colloidal gold NCs labeled to bovine serum albumin (BSA) iron oxide nanocrystals with different classes of (Retnakumari et al. 2010) for possible in vivo fluorophores such as organic dyes and inorganic experiments. semiconductor nanocrystals (so-called quantum dots) Therefore, combining the strong magnetic proper- and give promising hope for advanced therapies (Corr ties of ferrite, the ability of PEs to load model drugs et al. 2008; Kim et al. 2006; Landmark et al. 2008; and protect the NPs with proteins containing small and Liong et al. 2008; Quarta et al. 2008; Tamanaha et al. photostable fluorescent markers offer an interesting 2008; Yang et al. 2008). Moreover, one very potent approach to design a new kind of ‘‘smart’’ delivery approach is the layer-by-layer (LBL) assembly of systems. oppositely charged polyelectrolytes (PEs) from aque- ous solution on a host surface, such as charged flat substrates (Lvov et al. 1993; Yoo et al. 1998)or Experimental nanoparticles (NPs) (Shenoy et al. 2003; Sun et al. 2009; Wang et al. 2008; Schneider and Decher 2008), All chemicals were purchased from Sigma-Aldrich to fabricate ultrathin films and multilayer structures of (Germany) and were used without any further purifi- tunable properties for coatings (Schneider and Decher cation. Ultrapure water (18.2 MX) was used in all 2008), electrical materials (Sun et al. 2001), sensors experiments. (Whitney et al. 2005), and drug delivery (Reum et al. A scheme of the synthesis protocol of the multi- 2010). However, some issues have to be tackled functional nanocomposite is depicted in Fig. 1. regarding (i) the fluorescence sensitivity hindered by First, mNPs with the composition Mn0.8Zn0.2Fe2O4 the strong quenching of the fluorophore by the called mNPs were synthesized by the chemical co- magnetic core, (ii) the drug loading efficiency of the precipitation method (Auzans et al. 1999; Alexiou nanomaterials (Labouta and Schneider 2010), and (iii) et al. 2006). Briefly, 40 mL of 0.04 mol FeCl3Á6H2O the protection of the payload which should not be solution was heated up to 80 °C and then mixed with a degraded too fast by catalytic-enzymatic processes. solution of 0.016 mol of MnCl2Á4H2O and 0.004 mol We describe in this article a simple route to design ZnCl2 dissolved in 8.8 mL water. The mixed solution magnetic fluorescent NPs using ferrofluid suspensions was added under vigorous stirring to 200 mL boiling of Mn-Zn ferrites coated with PE multilayers. solution of NaOH (0.25 M). The black suspension was Fluorescent property is brought by adsorbing gold stirred for 1 h at 90 °C. The precipitate was separated nanoclusters (NCs) covalently labeled to a standard with a permanent magnet and washed twice with protein on the surface of these magnetic nanoparticles water. To achieve a ferrofluid which is stable in water, (mNPs). Fluorescent noble metal (Ag, Au) NCs have it is necessary to provide a sufficient stabilization, e.g., emerged as a new family of fluorescent markers, and electrostatic repulsion between the particles. This several studies demonstrated the potential of those implies two steps: an acid treatment of the particle clusters capped in different templates [polymers surface followed by the stabilization with nitrate ions. (Duan and Nie 2007; Zhang et al. 2005; Lin et al. 2009), dendrimers (Zheng et al. 2003, 2007), or proteins (Le Guevel et al. 2011a; Retnakumari et al. 2010; Xie et al. 2009)] for biolabeling, imaging, and sensing. Those clusters have shown remarkable photo- physical properties such as intense fluorescence emission, strong photostability, and high Stokes-shift. Additionally, these clusters are smaller than quantum dots (\2 nm) with a fluorescence tunable in the all visible range due to size-dependent fluorescence (Wu and Jin 2010; Zheng et al. 2007; Zhu et al. 2008). Fig. 1 Scheme of the synthesis of magnetic NPs coated with Another key point regarding the application of this fluorescent gold NCs stabilized in BSA 123 J Nanopart Res (2012) 14:727 Page 3 of 10 Therefore, a 2-M HNO3 solution was added to the 3 mL AuBSA (15 mg/mL) under stirring for 30 min. washed particles and stirred at room temperature for The pH of the AuBSA was adjusted to 8 in order to 6 min. In parallel, 60 mL of an aqueous solution promote the electrostatic interaction between the containing 0.02 mol Fe(NO3)3Á9H2O and 8.5 mL of a magnetic NPs—positively charged—and the gold 0.008 mol MnCl2Á4H2O and 0.002 mol ZnCl2 was NCs-labeled BSA. Then, the mixture was centrifuged prepared at 80 °C. The two solutions were mixed and two times at high speed (15,000 rpm) and resuspended subsequently added to the particle suspension. The in water. The new solution mNPs-PE-AuBSA (5 mg/ resulting solution was stirred for 30 min at 80 °C. The mL) has a dark brown color and was kept refrigerated stabilized particles called mNPs were separated with a before characterization. permanent magnet and taken up in 200 mL of water. X-ray powder diffraction (XRD) patterns were In order to obtain stable ferrofluids at pH 7, the nitrate obtained with a Siemens D 500 diffractometer, using ions have been exchanged with citrate ions using a a Cu-Ka radiation (k = 1.54 A˚ ) at room temperature. dialysis against 0.01 M citrate solution for 7 days. The They were recorded in the range 20°-70° (2H) with a solution was then dialyzed against distilled water for typical step size of 0.02°.
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