Chemie und Prozesstechnik
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Light-emitting nanoparticles like semiconductor nanocrystals (termed quantum dots, QDs) are promising candidates for biosensing and bioimaging applications based on their bright and stable photoluminescent properties. As high-quality QDs are often synthesized in organic solvents, strategies needed to be developed to render them water-dispersible without affecting their optical properties and prevent changes in postmodification steps like the biofunctionalization with antibodies or DNA. Despite a large number of studies on suitable surface modification procedures, the preparation of water-soluble QDs for nanobiotechnology applications still presents a challenge. To highlight the advantages of surface silanization, we systematically explored the influence of the core/multishell architecture of CdSe/CdS/ZnS QDs and the silanization conditions on the optical properties of the resulting silanized QDs. Our results show that the optical properties of silica-coated CdSe/CdS/ZnS QDs are best preserved in the presence of a thick CdS (6 monolayers (ML)) intermediate shell, providing a high photoluminescence quantum yield (PL QY), and a relatively thick ZnS (4.5 ML) external shell, effectively shielding the QDs from the chemical changes during silica coating. In addition to the QD core/shell architecture, other critical parameters of the silica-coating process, that can have an influence on the optical properties of the QD, include the choice of the surfactant and its concentration used for silica coating. The highest PL QY of about 46% was obtained by a microemulsion silica-coating procedure with the surfactant Brij L4, making these water-dispersible QDs to wellsuited optical reporters in future applications like fluorescence immunoassays, biomedicine, and bioimaging.
Mass spectrometry-based methods play a crucial role in the quantification of the main iron metabolism regulator hepcidin by singling out the bioactive 25-residue peptide from the other naturally occurring N-truncated isoforms (hepcidin-20, -22, -24), which seem to be inactive in iron homeostasis. However, several difficulties arise in the MS analysis of hepcidin due to the sticky character of the peptide and the lack of suitable standards. Here, we propose the use of amino- and fluoro-silanized autosampler vials to reduce hepcidin interaction to laboratory glassware surfaces after testing several types of vials for the preparation of stock solutions and serum samples for isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS). Furthermore, we have investigated two sample preparation strategies and two chromatographic separation conditions with the aim of developing an LC-MS/MS method for the sensitive and reliable quantification of hepcidin-25 in serum samples. A chromatographic separation based on usual acidic mobile phases was compared with a novel approach involving the separation of hepcidin-25 with solvents at high pH containing 0.1% of ammonia. Both methods were applied to clinical samples in an intra-laboratory comparison of two LC-MS/MS methods using the same hepcidin-25 calibrators with good correlation of the results. Finally, we recommend an LC-MS/MS-based quantification method with a dynamic range of 0.5–40 μg/L for the assessment of hepcidin-25 in human serum that uses TFA-based mobile phases and silanized glass vials.