Simultaneous determination of phenytoin, barbital and caffeine in pharmaceuticals by absorption (zero-order) UV spectra and first-order derivative spectra--multivariate calibration methods.

The quantitative predictive abilities of partial least squares (PLS-1) and principle component regression (PCR) on absorption (zero-order) UV spectra are compared with the results obtained by the use of these multivariate calibration methods on first-order derivative spectra. Both approaches were satisfactorily applied to the simultaneous determination of these drugs in synthetic and pharmaceutical mixtures. Significant advantages were found in the simultaneous determination of phenytoin, barbital and caffeine in binary and ternary mixtures, by application of different multivariate calibration methods when the calibration matrix was performed using the first-order derivative spectra. The proposed method was validated by applying it to the analysis of binary and ternary mixtures of phenytoin, barbital and caffeine. Determinations were made over the concentration ranges of 0.24-22.0, 0.01-27.0 and 0.049-27.0 microg ml(-1) for phenytoin, barbital and caffeine, respectively, in the binary and 0.45-22.0, 0.05-26.0 and 0.05-20.0 microg ml(-1) for phenytoin, barbital and caffeine, respectively, in the ternary mixtures. The relative standard errors in the determinations were less than 3% in most cases.