| Article ID | Journal | Published Year | Pages | File Type |
|---|---|---|---|---|
| 1230196 | Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy | 2014 | 8 Pages |
•A MIRS method for simultaneous determination of 3 API in veterinary tablets.•siPLS improved the model by empirically selecting the discriminant spectral regions.•Model development without prior access to excipient composition of the formulations.•Analyses of 3 real (commercial) samples in a situation of multi-product calibration.•The proposed MIRS method is more than ten times faster than the HPLC one.
This paper describes the development and validation of a new multivariate calibration method based on diffuse reflectance mid infrared spectroscopy for direct and simultaneous determination of three veterinary pharmaceutical drugs, pyrantel pamoate, praziquantel and febantel, in commercial tablets. The best synergy interval partial least squares (siPLS) model was obtained by selecting three spectral regions, 3715–3150, 2865–2583, and 2298–1733 cm−1, preprocessed by first derivative and Savitzky–Golay smoothing followed by mean centering. This model was built with five latent variables and provided root mean square errors of prediction (RMSEP) equal or lower than 0.69 mg per 100 mg of powder for the three analytes. The method was validated according the appropriate regulations through the estimate of figures of merit, such as trueness, precision, linearity, analytical sensitivity, bias and residual prediction deviation (RPD). Then, it was applied to three different veterinary pharmaceutical formulations found in the Brazilian market, in a situation of multi-product calibration, since the excipient composition of these commercial products, which was not known a priori, was modeled by an experimental design that scanned the likely content range of the possible constituents. The results were verified with high performance liquid chromatography with diode array detection (HPLC–DAD) and high performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) and were in agreement with the predicted values at 95% confidence level. The developed method presented the advantages of being simple, rapid, solvent free, and about ten times faster than the HPLC ones.
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