Journal
JOURNAL OF SEPARATION SCIENCE
Volume 45, Issue 17, Pages 3286-3300Publisher
WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.202200268
Keywords
(3-aminopropyl)silatrane; hydrolytic stability; silica functionalization; solid-state NMR spectroscopy; stationary phase characterization
Categories
Funding
- Projekt DEAL
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This study reports a novel stable-bonded amino silica stationary phase obtained by crosslinking surface aminopropyl moieties. The new phase exhibited superior hydrolytic stability and showed excellent separation performance in the separation of therapeutically effective sulfonamides and carbohydrates.
The present work reports on a novel stable-bonded amino silica stationary phase obtained by crosslinking of surface aminopropyl moieties using triglycidyl isocyanurate. The obtained cross-linked amido-amino network silica material exhibited superior hydrolytic stability compared to classical 3-aminopropyl phases and showed, inter alia, excellent separation of nine therapeutically effective sulfonamides in hydrophilic interaction/weak anion exchange chromatography elution mode. Additionally, the separation of carbohydrates was investigated under classical hydrophilic interaction chromatography conditions as well proving the suitability of the novel phase for such applications. For the evaluation of the hydrolytic stability the prepared material, as well as two commercially available benchmark columns and a set of in-house synthesized amino-modified materials, were exposed to harsh aqueous mobile phase conditions for in total of 50 h at elevated temperature. In this context, the materials were examined by elemental analysis, (C-13 and( 29)Si cross-polarization/magic angle spinning) solid-state nuclear magnetic resonance, and a chromatographic test before and subsequent to the exposure to these stress conditions. Lastly, the new stationary phase was classified in comparison to a set of commercially available stationary phases by principal component analysis of resultant retention factors gained from chromatographic standard tests.
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