Enantiomeric analysis of overlapped chromatographic profiles in the presence of interferences. Determination of ibuprofen in apharmaceutical formulation containing homatropine

PADRO, JUAN MANUEL; OSORIO-GRISALES, JAIVER; ARANCIBIA, JUAN A.; OLIVIERI, ALEJANDRO C.; CASTELLS, CECILIA B.*; CASTELLS, CECILIA B.*

JOURNAL OF CHROMATOGRAPHY - A

ELSEVIER SCIENCE BV

Lugar: Amsterdam; Año: 2016 vol. 1467 p. 255 - 260

0021-9673

In this work, we studied the combination of chemometric methods with chromatographic separations as astrategy applied to the analysis of enantiomers when complete enantioseparation is difficult or requireslong analysis times and, in addition, the target signals have interference from the matrix. We presentthe determination of ibuprofen enantiomers in pharmaceutical formulations containing homatropineas interference by chiral HPLC-DAD detection in combination with partial least-squares algorithms. Themethod has been applied to samples containing enantiomeric ratios from 95:5 to 99.5:0.5 and coelutionof interferents. The results were validated using univariate calibration and without homatropine. Relativeerror of the method was less than 4.0%, for both enantiomers. Limits of detection (LOD) and quantifica-tion (LOQ) for (S)-(+)-ibuprofen were 4.96 × 10−10and 1.50 × 10−9mol, respectively. LOD and LOQ forthe R-(−)-ibuprofen were LOD = 1.60 × 10−11mol and LOQ = 4.85 × 10−11mol, respectively. Finally, thechemometric method was applied to the determination of enantiomeric purity of commercial pharma-ceuticals. The ultimate goal of this research was the development of rapid, reliable, and robust methodsfor assessing enantiomeric purity by conventional diode array detector assisted by chemometric tools.