In this study, near-infrared (NIR) transmittance and Raman spectroscopy chemometric calibrations of the active substance content of a pharmaceutical tablet were developed using partial least-squares regression (PLS). Although the active substance contained the strongly Raman active C≡N functional group, the best results were obtained with NIR transmittance, which highlights the difference between (microscopic) surface sampling and whole tablet diffuse transmittance sampling. The tablets exist in four dosages with only two different concentrations of active substance (5 mg (5.6% w/w), and 10, 15, and 20 mg (8.0% w/w) active substance per tablet). A calibration on all four dosages resulted in a prediction error expressed as the root mean squared error of cross-validation (RMSECV) of 0.30% w/w for the NIR transmittance calibration. The corresponding error when using Raman spectra was 0.56% w/w. Specially prepared calibration batches covering the range 85-115% of the nominal content for each dosage were added to the first sample set, and NIR transmittance calibrations on this set - containing coated as well as uncoated tablets - gave a further reduction in prediction errors to 0.21-0.289% w/w. This corresponds to relative prediction errors (RMSECV/y<sub>nom</sub>) of 2.6-3.7%. This is a reasonably low error when compared to the error of the chromatographic reference method, which was estimated to 3.5%.
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