MULTIVARIATE CALIBRATION IN THE DETERMINATION OF ACETYLATED ALDOSES BY GLC

An improved g.l.c. method for the analysis of acetylated aldoses is described. Fast acetylation (acetic anhydride-1-methylimidazole) can be performed directly on the acidic aldose hydrolysate in a one-vessel operation. Factors most likely to influence the ratios of isomers in the reaction solutions at the time of derivatisation were studied. The derivatisation procedure was modified to minimise these effects. Quantification can be based either on linear regression of peaks for single isomers of each sugar or on all peaks by designed calibration standards and partial least-squares regression (PLSR). The latter calibration gives slightly better reproducibility and stability. PLSR can also be used when the chromatographic separation is poor. The results and the reproducibility of the two calibration methods for the peracetates were compared with alditol acetate analysis for four plant materials. © 1990.