Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1497, Issue -, Pages 172-179Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2017.03.070
Keywords
Monolithic capillary column; Nano-HPLC; Chiral separation; Click polymerization; Thiol-ene click reaction; Composite m aterial
Funding
- Struktur- und Innovationsfonds Baden-Wurttemberg (SI-BW)
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This work reports on the proof-of-principle of preparation of novel one step in-situ functionalized monolithic polysiloxane-polymethacrylate composite materials in capillary columns for enantioselective nano-HPLC using a thiol-ene click reaction. Quinine carbamate as functional monomer and ethylene dimethacrylate as crosslinker were both used as ene components in a thermally initiated double click-type polymerization reaction with poly(3-mercaptopropyl)methylsiloxane as thiol component in presence of 1-propanol as porogenic solvent. Elemental analysis and on-capillary fluorescence measurement proved the successful incorporation of the functional chiral monomer into the polymer. Scanning electron microscopy images revealed a macroporous polymer morphology which is typical for a nucleation and growth mechanism of pore formation. The individual microglobules appear relatively spherical and smooth indicating a non-porous nature. Nano-HPLC experiments of the chiral monolithic capillary column provided successful enantiomer separation of N-3,5-dinitrobenzoylleucine as test compound in polar organic elution mode clearly documenting the successful implementation of the proposed concept towards new functionalized monolithic composite materials. (C) 2017 Elsevier B.V. All rights reserved.
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