Premium
Alkylated poly(styrene‐divinylbenzene) monolithic columns for μ‐HPLC and CEC separation of phenolic acids
Author(s) -
Kučerová Zdenka,
Szumski Michal,
Buszewski Boguslaw,
Jandera Pavel
Publication year - 2007
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200700346
Subject(s) - divinylbenzene , monolith , styrene , monolithic hplc column , copolymer , chemistry , solvent , van deemter equation , theoretical plate , chromatography , porosity , grafting , high performance liquid chromatography , materials science , organic chemistry , polymer , catalysis
Macroporous poly(styrene‐divinylbenzene) monolithic columns were prepared in fused silica capillaries of 100 μm id by in‐situ copolymerization of styrene with divinylbenzene in the presence of propan‐1‐ol and formamide as the porogen system. The monoliths were subsequently alkylated with linear alkyl C‐18 groups via Friedel‐Crafts reaction to improve the retention and chromatographic resolution of strongly polar phenolic acids. A new thermally initiated grafting procedure was developed in order to shorten the time of the alkylation process. The grafting procedure was optimized with respect to the reaction temperature, time, the grafting reactant concentration, and the solvent used. The type of solvent and the grafting temperature are the most significant factors affecting the hydrodynamic properties, porosity, and efficiency of the columns. While the equivalent particle diameter of the grafted column increased, the capillary‐like flow‐through pore diameter decreased in comparison to non‐alkylated monoliths. The hydrodynamic permeability of the monolith decreased, but the monolithic column still permitted fast μ‐HPLC separations.