Determination of enantiomeric composition of ibuprofen in pharmaceutical formulations by partial least-squares regression of strongly overlapped chromatographic profiles

OSORIO GRISALES, J.; ARANCIBIA, J. A.; CASTELLS, C.; OLIVIERI, A. C.

JOURNAL OF CHROMATOGRAPHY B

ELSEVIER

Lugar: Amsterdam; Año: 2012 vol. 910 p. 78 - 83

0378-4347

In this report, we demonstrate how chiral liquid chromatography combined with multivariate chemometric techniques, specifically unfolded-partial least-squares regression (U-PLS), provides a powerful analytical methodology. Using U-PLS, strongly overlapped enantiomer profiles in a sample could be successfully processed and enantiomeric purity could be accurately determined without requiring baseline enantioresolution between peaks. The samples were partially enantioseparated with a permethyl-cyclodextrin chiral column under reversed-phase conditions. Signals detected with a diode-array detector within a wavelength range from 198 to 241 nm were recorded, and the data were processed by a secondorder multivariate algorithm to decrease detection limits. The R-(−)-enantiomer of ibuprofen in tablet formulation samples could be determined at the level of 0.5 mg L−1 in the presence of 99.9% of the S-(+)-enantiomorph with relative prediction error within±3%.