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Two-Dimensional Diffusion-Ordered NMR Spectroscopy as a Tool for Monitoring Functionalized Carbon Nanotube Purification and Composition

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Center of Excellence for Nanostructured Materials (CENMAT), Dipartimento di Scienze Farmaceutiche and INSTM UdR Trieste, Università degli Studi di Trieste, Piazzale Europa 1, 34127 Trieste, Italy
Protos Research Institute, Via Flavia 23/1, c/o Sviluppo Italia, 34148, Trieste, Italy
§ Polymer Conjugation Department, EURAND S.p.A, Area Science Park, Padriciano 99, 34149 Trieste, Italy
CNRS, Institut de Biologie Moléculaire et Cellulaire, Laboratoire d’Immunologie et Chimie Thérapeutiques, 67000 Strasbourg, France
* Address correspondence to [email protected], [email protected]
Cite this: ACS Nano 2010, 4, 4, 2051–2058
Publication Date (Web):April 1, 2010
https://doi.org/10.1021/nn100257h
Copyright © 2010 American Chemical Society

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    Abstract

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    Functionalized carbon nanotube (CNT) derivatives are currently under thorough investigation in different biomedical investigations. In this field of research, the composition of sample either in terms of covalently attached or physisorbed moieties can greatly affect the observed results and hamper the comparison between different studies. Therefore, the availability of a fast and reliable analytical technique to assess both the type of interaction (covalent vs noncovalent) and the composition of CNT conjugates is of great importance. Here we describe that the two-dimensional diffusion-ordered (DOSY) NMR spectroscopy is extremely useful to discriminate between conjugated and unconjugated polyethylene glycol groups in samples obtained by condensation with oxidized single-walled carbon nanotubes (SWNTs). This fast and nondestructive technique allows us to follow the removal of unconjugated polyethylene glycol chains during the purification. In particular, DOSY analysis reveal that about 1/3 (wt %) of the polyethylene glycol used for the condensation remained physisorbed to functionalized SWNTs after dialysis. Complete elimination of physisorbed polyethylene glycol was achieved using diafiltration.

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    Detailed experimental procedure, instrumental and software settings, full TGA data results, supporting diffusion-based and other conventional NMR results, TEM characterization of the D2O solution content. This material is available free of charge via the Internet at http://pubs.acs.org.

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