Nuclear magnetic resonance and high-performance liquid chromatographic evaluation of polymer-based stationary phases immobilized on silica

Autor: Urban Skogsberg, Norbert Welsch, Christoph Meyer, Klaus Albert
Rok vydání: 2004
Předmět:
Zdroj: Analytical and Bioanalytical Chemistry. 382:679-690
ISSN: 1618-2650
1618-2642
DOI: 10.1007/s00216-004-2752-5
Popis: Three poly(ethylene-co-acrylic) acid copolymers (-CH(2)CH(2)-)(x)[CH(2)CH(CO(2)H)-](y) with different chain lengths and mass fractions of acrylic acid were covalently immobilized as stationary phases on silica via two variants of spacer molecules (3-aminopropyltriethoxysilane and 3-glycidoxypropyltrimethoxysilane). Different mobilities of the alkyl chains in the stationary phases were observed using (13)C solid-state NMR spectroscopy. The stationary phases with more rigid trans-ordered alkyl chains had better selectivity for geometric beta-carotene and xanthophyll isomers (provitamin A derivatives). Also, all the separations of the analytes were affected by polar interactions with the chromatographic sorbent. This was further proved by separating more polar cis/trans retinoic acid isomers (vitamin A derivatives). (13)C high-resolution/magic-angle spinning (HR/MAS) NMR measurements of the chromatographic sorbents suspended in the mobile phase confirmed a dependence of molecular shape recognition ability on alkyl chain conformation.
Databáze: OpenAIRE