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Efficient Method for the Concentration Determination of Fmoc Groups Incorporated in the Core-Shell Materials by Fmoc–Glycine
Abstract
In this paper, we described the synthesis procedure of TiO2@SiO2 core-shell modified with 3-(aminopropyl)trimethoxysilane (APTMS). The chemical attachment of Fmoc–glycine (Fmoc–Gly–OH) at the surface of the core-shell structure was performed to determine the amount of active amino groups on the basis of the amount of Fmoc group calculation. We characterized nanostructures using various methods: transmission electron microscope (TEM), scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA) and X-ray photoelectron spectroscopy (XPS) to confirm the modification effectiveness. The ultraviolet-visible spectroscopy (UV-vis) measurement was adopted for the quantitative determination of amino groups present on the TiO2@SiO2 core-shell surface by determination of Fmoc substitution. The nanomaterials were functionalized by Fmoc–Gly–OH and then the fluorenylmethyloxycarbonyl (Fmoc) group was cleaved using 20% (v/v) solution of piperidine in DMF. This reaction led to the formation of a dibenzofulvene–piperidine adduct enabling the estimation of free Fmoc groups by measurement the maximum absorption at 289 and 301 nm using UV-vis spectroscopy. The calculations of Fmoc loading on core-shell materials was performed using different molar absorption coefficient: 5800 and 6089 dm3 × mol−1 × cm−1 for λ = 289 nm and both 7800 and 8021 dm3 × mol−1 × cm−1 for λ = 301 nm. The obtained results indicate that amount of Fmoc groups present on TiO2@SiO2–(CH2)3–NH2 was calculated at 6 to 9 µmol/g. Furthermore, all measurements were compared with Fmoc–Gly–OH used as the model sample
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Authors (6)
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Elzbieta Szczepanska
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Beata Grobelna
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Amanda Kulpa
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Tadeusz Ossowski prof. dr hab. inż.
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Pawel Niedzialkowski
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Details
- Category:
- Articles
- Type:
- artykuły w czasopismach
- Published in:
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MOLECULES
no. 25,
ISSN: 1420-3049 - Language:
- English
- Publication year:
- 2020
- Bibliographic description:
- Szczepanska E., Grobelna B., Ryl J., Kulpa A., Ossowski T., Niedzialkowski P.: Efficient Method for the Concentration Determination of Fmoc Groups Incorporated in the Core-Shell Materials by Fmoc–Glycine// MOLECULES -Vol. 25,iss. 17 (2020), s.3983-
- DOI:
- Digital Object Identifier (open in new tab) 10.3390/molecules25173983
- Verified by:
- Gdańsk University of Technology
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