HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY OF AMINO-ACIDS, PEPTIDES AND PROTEINS .129. CERAMIC-BASED PARTICLES AS CHEMICALLY STABLE CHROMATOGRAPHIC SUPPORTS
Hj. Wirth et al., HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY OF AMINO-ACIDS, PEPTIDES AND PROTEINS .129. CERAMIC-BASED PARTICLES AS CHEMICALLY STABLE CHROMATOGRAPHIC SUPPORTS, Journal of chromatography, 646(1), 1993, pp. 129-141
Porous zirconia based particles have been modified using different der
ivatisation procedures. The modified particles were characterised in t
erms 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 gr
oup density was determined by a H-1 NMR technique. The particles were
modified by immobilising different silanes to introduce either hydroph
obic ligands or reactive groups onto the zirconia surface. In the latt
er case, various ligands were then covalently attached to the activate
d supports. Using this type of modification, n-octadecyl- (C18), carbo
hydrate- and Cibacron Blue F3GA-modified zirconia particles were produ
ced. Furthermore, polymeric coated particles were prepared either by u
sing polybutadiene or by cross-linking the carbohydrate modified sorbe
nts. The pH stability of the different sorbents were determined in bat
ch experiments and under chromatographic conditions. The leakage of li
gands was monitored by UV absorption and by employing radioactively la
belled ligands. The performance of the C18 reversed-phase modified zir
conia in packed columns was also used as an indicator of changes in th
e surface chemistry following pH stability tests. The experimental res
ults indicate that the Cibacron Blue F3GA dye-modified sorbent was sta
ble 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 substantia
te the favourable chemical and physical characteristics anticipated fo
r surface modified zirconias for potential use as chromatographic adso
rbents.