Various chromatographic techniques for isolation and separation of hig
hly esterified sucrose polyesters (SPE) of olive oil are described. Hi
gh-performance size-exclusion chromatography was used to check the pur
ity of the samples, particularly to show that SPE were free from unrea
cted fatty acid methyl esters. Thin-layer chromatography (TLC), Iatros
can TLC flame-ionization detection (FID) and highperformance liquid ch
romatography (HPLC) on reversed phase were applied for separation of o
cta-, hepta- and hexaesters of sucrose. Pure fractions from the total
mixture, obtained by column chromatography, were identified by infrare
d and nuclear magnetic resonance spectroscopy. When necessary, specifi
c reactions were applied; particularly, silylation and lead acetate-di
chlorofluorescein (in toluene) spray were used to ascertain the degee
of esterification of sucrose. Finally, octa; hepta and hexaesters of s
ucrose were quantitated by silica column chromatography, TLC/FID and H
PLC on reversed-phase.