title: Determination of enantiomeric composition of ibuprofen in pharmaceutical formulations by partial least-squares regression of strongly overlapped chromatographic profiles.
abstract: 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-β-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 second-order 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%.
authors.affiliation: Laboratorio de Separaciones Analíticas, División Química Analítica, Universidad Nacional de La Plata, 47 y 115-1900 La Plata, Argentina.
authors.forename: Jaiver Osorio
authors.initials: JO
authors.lastname: Grisales
authors.forename: Juan A
authors.initials: JA
authors.lastname: Arancibia
authors.forename: Cecilia B
authors.initials: CB
authors.lastname: Castells
authors.forename: Alejandro C
authors.initials: AC
authors.lastname: Olivieri
mesh_terms: D000465:Algorithms; D002626:Chemistry, Pharmaceutical; D002853:Chromatography, Liquid / Q000379:methods*; D007052:Ibuprofen / Q000737:chemistry*; D016018:Least-Squares Analysis; D013237:Stereoisomerism; D013607:Tablets / Q000737:chemistry
chemical_list: D013607:Tablets; D007052:Ibuprofen