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High-performance liquid chromatography with fast-scanning fluorescence detection and multivariate curve resolution for the efficient determination of galantamine and its main metabolites in serum

Culzoni, María J., Aucelio, Ricardo Q., Escandar, Graciela M.
Analytica chimica acta 2012 v.740 pp. 27-35
Alzheimer disease, acetonitrile, ammonium acetate, analytical chemistry, blood serum, cholinesterase, data collection, detection limit, fluorescence, high performance liquid chromatography, least squares, metabolites, patients, prediction, wavelengths
Based on green analytical chemistry principles, an efficient approach was applied for the simultaneous determination of galantamine, a widely used cholinesterase inhibitor for the treatment of Alzheimer's disease, and its major metabolites in serum samples. After a simple serum deproteinization step, second-order data were rapidly obtained (less than 6min) with a chromatographic system operating in the isocratic regime using ammonium acetate/acetonitrile (94:6) as mobile phase. Detection was made with a fast-scanning spectrofluorimeter, which allowed the efficient collection of data to obtain matrices of fluorescence intensity as a function of retention time and emission wavelength. Successful resolution was achieved in the presence of matrix interferences in serum samples using multivariate curve resolution-alternating least-squares (MCR-ALS). The developed approach allows the quantification of the analytes at levels found in treated patients, without the need of applying either preconcentration or extraction steps. Limits of detection in the range between 8 and 11ngmL⁻¹, relative prediction errors from 7 to 12% and coefficients of variation from 4 to 7% were achieved.