Nanoparticles are finding many research and industrial applications, yet their characterization remains a challenge. Their cores are often polydisperse and coated by a stabilizing shell that varies in size and composition. No single technique can characterize both the size distribution and the nature of the shell. Advances in analytical ultracentrifugation allow for the extraction of the sedimentation (s) and diffusion coefficients (D). Here we report an approach to transform the s and D distributions of nanoparticles in solution into precise molecular weight (M), density (ρP) and particle diameter (dp) distributions. M for mixtures of discrete nanocrystals is found within 4% of the known quantities. The accuracy and the density information we achieve on nanoparticles are unparalleled. A single experimental run is sufficient for full nanoparticle characterization, without the need for standards or other auxiliary measurements. We believe that our method is of general applicability and we discuss its limitations.
Photocrosslinking of polyethylene glycol (PEG) using exogenous agents is a convenient way to produce branched PEG from commercial sources thus avoiding the tricky synthesis of new reactive and functional polymers. In this study, we synthesized two series of new photocrosslinkers, i.e. bis-fluorophenyl azide and bis-trifluoromethyl diazirine, which under soft UV-irradiation produce reactive species (i.e. nitrene and carbene respectively) that insert into the C-H bond of the polymer backbone, building new bridges between macromolecular chains. These photocrosslinkers are different in terms of behaviour under irradiation and affinity for the target substrate (i.e. PEG). Thus, practical conditions for photocrosslinking of a 10-kDa PEG were studied and followed by NMR and size-exclusion chromatography. In particular, we investigated irradiation in bulk or in solvent, at different irradiation times, with several concentrations of PEG and photolinkers. Finally, we were able to design a procedure to obtain soluble crosslinked PEGs of 300 kDa.
In this study, a simple and direct biodetector was proposed, which was based on biotin immobilized onto a conducting polymer-coated electrode, for the detection of avidin, a highly stable glycoprotein found in egg-whites. Biotin was immobilized onto the electrode by covalent coupling to the primary amine group on the poly 3′-(3-chloro-4-amino-β-styryl)-(2,2′ : 5′,2″-terthiophene) (PCAST), and the biotin–avidin interaction was monitored by cyclic voltammetry. Incubation of the PCAST/biotin-modified-coated electrode with avidin in a phosphate buffered saline solution caused a significant change to its cyclic voltammogram, which was explained by the binding of avidin by biotin, and resulted in restricted ion transfer to and from the conducting polymer. This change was then utilized to detect avidin at 4 × 10–6 mol L–1.
Novel ECPs (electronic conducting polymers) based on amino β-styryl-substituted terthiophene (AST) were synthetized by direct electropolymerization. The ECPs were characterized by cyclic voltammetry, square-wave voltammetry, Fourier transform infrared (FTIR) spectroscopy, and X-ray photoelectron spectroscopy (XPS). The poly(amino β-styryl terthiophene) displayed cyclic and square-wave voltammograms with redox peaks that can be assigned to the aminophenyl moiety and the polyterthiophene backbone. The presence of free primary amine groups on the ECP film permitted further biological functionalization (i.e., covalent bonding of various bioreceptors on its surface). The electrochemical performance of Biotin grafted at the AST modified glassy carbon electrode was investigated to detect the Avidin protein in solution by cyclic voltammetry and square-wave voltammetry.Key words: electronic conducting polymer, electrode surface modification, biosensor, β-styryl-substitued terthiophene, functionalization, cyclic, square-wave voltammetry.
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