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Hydroxypropyl-β-cyclodextrin encapsulated stationary phase based on silica monolith particles for enantioseparation in liquid chromatography.

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Hydroxypropyl-β-cyclodextrin-encapsulated stationary phase incorporated on silica monolith particles was prepared by physical embedding, providing a new method for the development of chiral stationary phase for enantioseparation in liquid chromatography. Ground… Click to show full abstract

Hydroxypropyl-β-cyclodextrin-encapsulated stationary phase incorporated on silica monolith particles was prepared by physical embedding, providing a new method for the development of chiral stationary phase for enantioseparation in liquid chromatography. Ground silica monolith particles of about 2.0 μm were prepared via sol-gel reaction followed by differential sedimentation. Initially, the silica monolith particles were pretreated with 3-trimethoxysilyl propyl methacrylate to attach double-bonded ligands onto the surface, then a network structure was formed onto the surface of the particle using N-isopropyl acrylamide as functional monomer. Hydroxypropyl-β-cyclodextrin was encapsulated inside N-isopropyl acrylamide copolymerized layer on the surface of silica monolith particles. The effect of the amount of chiral selector on the chromatographic efficiency of the chiral stationary phase was examined. The glass lined stainless steel columns (1 mm internal diameter, 300 mm length) were packed with the stationary phase for estimation the efficiency by separation of phenylsuccinic acid, oxybutynin, equol and naproxen enantiomers in HPLC, with the resolutions of 1.54, 1.72, 2.54 and 2.31 respectively. The column to column repeatabilities through relative standard deviation were found better than 3%. The experimental results indicate that the sol-gel ground silica particles modified with β-cyclodextrin provide a promising way for the separation of chiral enantiomers. This article is protected by copyright. All rights reserved.

Keywords: stationary phase; silica monolith; monolith particles

Journal Title: Journal of separation science
Year Published: 2020

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