title: Optimization of poly(methyl styrene-co-bis(p-vinylbenzyl)dimethylsilane)-based capillary monoliths for separation of low, medium, and high molecular-weight analytes.
abstract: Poly(methyl styrene-co-bis(p-vinylbenzyl)dimethylsilane)-based monolithic capillary columns were optimized for separation of low, medium, and high molecular-weight analytes. The morphology and consequently the chromatographic performance of these monoliths were tuned by changes in the volume-ratio of monomer to macroporogen, establishing good monolithic flow-through and retention pores. Two monoliths were prepared and analyzed by reversed-phase chromatographic separation of low molecular-weight analytes such as alkyl benzenes and β-blockers, as well as medium and high molecular-weight analytes such as peptides and proteins, respectively. The microstructure was studied by scanning electron microscopy (SEM), and by inverse-size exclusion chromatography (ISEC). Monolith 1 demonstrated a high retention of alkyl benzenes, which coeluted from the column at the washing step of absolute acetonitrile; yet this monolith established a baseline separation of 9-peptide and 8-protein mixtures. Monolith 2 demonstrated efficient separation of the three analyte groups of different molecular weights. Six alkyl benzenes and five β-blockers were base-line separated in less than 5 and 2min, respectively, with good resolution and very small values of peak width at half height. Moreover, a comparable performance of efficient separation of the 9-peptide mixture and a fast separation of 5- and 8-protein mixtures were achieved. Both monoliths were characterized by high mechanical strength, high permeability, and excellent reproducibility.
authors.affiliation: Department of Chemistry, Al-Azhar University-Gaza, Gaza, Palestine. Electronic address: s.lubbad@alazhar.edu.ps.
authors.forename: Said H
authors.initials: SH
authors.lastname: Lubbad
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D002623:Chemistry Techniques, Analytical / Q000295:instrumentation* / Q000379:methods*; D002850:Chromatography, Gel; D056148:Chromatography, Reverse-Phase; D008855:Microscopy, Electron, Scanning; D008970:Molecular Weight; D010455:Peptides / Q000302:isolation & purification; D010539:Permeability; D011506:Proteins / Q000302:isolation & purification; D015203:Reproducibility of Results; D020058:Styrene / Q000737:chemistry*
chemical_list: D000097:Acetonitriles; D010455:Peptides; D011506:Proteins; D020058:Styrene; C032159:acetonitrile
keywords: Alkyl benzenes; Monolith; Peptides; Permeability; Poly(methyl styrene-co-bis(p-vinylbenzyl)dimethylsilane); Proteins; β-blockers