Enantiomeric analysis of overlapped chromatographic profiles in the presence of interferences. Determination of ibuprofen in a pharmaceutical formulation containing homatropine.
In this work, we studied the combination of chemometric methods with chromatographic separations as a strategy applied to the analysis of enantiomers when complete enantioseparation is difficult or requires long analysis times and, in addition, the target signals have interference from the matrix. We present the determination of ibuprofen enantiomers in pharmaceutical formulations containing homatropine as interference by chiral HPLC-DAD detection in combination with partial least-squares algorithms. The method has been applied to samples containing enantiomeric ratios from 95:5 to 99.5:0.5 and coelution of interferents. The results were validated using univariate calibration and without homatropine. Relative error of the method was less than 4.0%, for both enantiomers. Limits of detection (LOD) and quantification (LOQ) for (S)-(+)-ibuprofen were 4.96×10-10and 1.50×10-9mol, respectively. LOD and LOQ for the R-(-)-ibuprofen were LOD=1.60×10-11mol and LOQ=4.85×10-11mol, respectively. Finally, the chemometric method was applied to the determination of enantiomeric purity of commercial pharmaceuticals. The ultimate goal of this research was the development of rapid, reliable, and robust methods for assessing enantiomeric purity by conventional diode array detector assisted by chemometric tools.
LIDMA (Laboratorio de Investigación y Desarrollo de Métodos Analíticos) y División Química Analítica, Universidad Nacional de La Plata, 47 y 115 (1900) La Plata, Argentina.
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Padró
LIDMA (Laboratorio de Investigación y Desarrollo de Métodos Analíticos) y División Química Analítica, Universidad Nacional de La Plata, 47 y 115 (1900) La Plata, Argentina.
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Osorio-Grisales
Departamento de Química Analítica, Facultad de Ciencias Bioquímicas y Farmacéuticas, Universidad Nacional de Rosario, Instituto de Química de Rosario (IQUIR-CONICET), Suipacha 531, Rosario S2002LRK, Argentina.
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Arancibia
Departamento de Química Analítica, Facultad de Ciencias Bioquímicas y Farmacéuticas, Universidad Nacional de Rosario, Instituto de Química de Rosario (IQUIR-CONICET), Suipacha 531, Rosario S2002LRK, Argentina.
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Olivieri
LIDMA (Laboratorio de Investigación y Desarrollo de Métodos Analíticos) y División Química Analítica, Universidad Nacional de La Plata, 47 y 115 (1900) La Plata, Argentina. Electronic address: castells@isis.unlp.edu.ar.
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Castells
D000465:Algorithms; D002138:Calibration; D002626:Chemistry, Pharmaceutical / Q000379:methods*; D002851:Chromatography, High Pressure Liquid; D004338:Drug Combinations; D007052:Ibuprofen / Q000032:analysis* / Q000737:chemistry*; D016018:Least-Squares Analysis; D057230:Limit of Detection; D004364:Pharmaceutical Preparations / Q000032:analysis* / Q000737:chemistry / Q000592:standards*; D015203:Reproducibility of Results; D013237:Stereoisomerism; D014326:Tropanes / Q000737:chemistry*
D004338:Drug Combinations; D004364:Pharmaceutical Preparations; D014326:Tropanes; C100236:homatropine; D007052:Ibuprofen
Chiral analysis; Ibuprofen enantiomeric purity; Interferences; Liquid chromatography; Multivariate calibration