Synthesis and characterization of triple acid stationary phases for cation exchange chromatography using click chemistry and atom transfer radical polymerization
Year: 2025
Type: article
Abstract: Triple acid cation exchangers were synthesized by a combination of atom transfer radical polymerization (ATRP) and alkyne azide click chemistry. Oxidized monodisperse PS/DVB particles were functionalized stepwise with carboxylic, phosphonic and sulfonic acid groups to prepare stationary phases with unique selectivities.The amount of sulfonic acid groups was varied while the amount of carboxylic and phosphonic acid groups remained constant, resulting in a set of stationary phases for trend analysis. The presence of sulfonic acid groups gives a good selectivity for the monovalent standard cations, while stationary phases without sulfonic acid groups show a coelution of monovalent ions. Furthermore, the presence of sulfonic acid groups results in a retention gap between mono and divalent ions, which can be used to separate target analytes inside the gap between these mono and divalent matrix ions.The relevant inorganic matrix cations Li+, Na+, NH4+, K+, Mg2+ and Ca2+ were separated together with mono-, di-, trimethylamin and tetramethylammonium in 45 minutes using a nitric acid gradient elution and suppressed conductivity detection. The retention gap between the monovalent and divalent ions was used to elute the analytes together with these ubiquitous matrix ions.Nine organic arsenic and selenium species were used as test analytes to characterize the mixed mode properties of the stationary phases. A good compatibility with organic solvents and electrospray mass spectrometry detection (ESI-MS) suitable operation conditions were observed. Secondary interactions of the analytes with the stationary phases were observed by varying the acetonitrile content in the mobile phase.
Source: Journal of Chromatography A
Authors: Luca Schipplick, Andreas Seubert
Institution: Philipps University of Marburg
Language: English
Subfield: Spectroscopy
Field: Chemistry
Domain: Physical Sciences
Open Access status: hybrid
Estimated APC paid: $4,040
OpenAlex ID: W4416442449