High-performance liquid chromatography of amino acids, peptides and proteins. CXXIX. Ceramic-based particles as chemically stable chromatographic supports.

Abstract

Porous zirconia based particles have been modified using different derivatisation procedures. The modified particles were characterised in terms of their accessible surface areas and degree of surface coverage of the bounded or physicoated phases utilising the strong and specific adsorption of phosphate ions to the zirconia surface. The hydroxyl group density was determined by a 1H NMR technique. The particles were modified by immobilising different silanes to introduce either hydrophobic ligands or reactive groups onto the zirconia surface. In the latter case, various ligands were then covalently attached to the activated supports. Using this type of modification, n-octadecyl- (C18), carbohydrate- and Cibacron Blue F3GA-modified zirconia particles were produced. Furthermore, polymeric coated particles were prepared either by using polybutadiene or by cross-linking the carbohydrate modified sorbents. The pH stability of the different sorbents were determined in batch experiments and under chromatographic conditions. The leakage of ligands was monitored by UV absorption and by employing radioactively labelled ligands. The performance of the C18 reversed-phase modified zirconia in packed columns was also used as an indicator of changes in the surface chemistry following pH stability tests. The experimental results indicate that the Cibacron Blue F3GA dye-modified sorbent was stable up to pH 10.5, the C18 reversed-phase packing up to pH 13 and the carbohydrate-bonded phase up to pH 12. These investigations substantiate the favourable chemical and physical characteristics anticipated for surface modified zirconias for potential use as chromatographic adsorbents.