RESUMEN
This work presents an evaluation of the analytical performance of three different portable near-infrared (NIR) instruments (denominated Port.1, Port.2 and Port.3) for quantifying mebendazole polymorphs (A, B and C) in pharmaceutical raw materials using multivariate calibration models. The performance of the portable instruments was compared with a benchtop one (FT-NIR Frontier spectrometer). In addition, calibration transfer between the benchtop and one of the portable instruments was also performed. For polymorph A, the Port.1 presented the lowest RMSEP value (1.01% w/w) even when compared to the FT-NIR instrument. For polymorphs B and C, the same Port.1 instrument presented RMSEP values of 2.09% w/w and 2.41% w/w, respectively, which were statistically similar to those obtained with the benchtop instrument. The LOD ranges (3.9-5.5 for polymorph A, 3.6-5.1 for polymorph B and 5.7-7.7 for polymorph C) obtained with the Port.1 was higher than those achieved with the benchtop NIR instrument, with high spectral resolution, signal-to-noise ratio and better wavelength reproducibility. Calibration transfer was performed between the benchtop NIR and Port.1 instruments. According to the results, the transferability of models is possible. The results obtained for complete recalibration of the portable instrument and those for the benchtop are comparable. The methods developed demonstrated a flexible, easy, cheap and fast way for quality control of MBZ polymorphs in incoming material, mainly in pharmaceutical laboratory chains.
Asunto(s)
Mebendazol/análisis , Control de Calidad , Espectroscopía Infrarroja Corta/normas , Calibración/normas , Cristalización , Mebendazol/química , Preparaciones Farmacéuticas/análisis , Espectroscopía Infrarroja Corta/métodos , Difracción de Rayos X/métodos , Difracción de Rayos X/normasRESUMEN
Principal component analysis was applied to XRD data from a series of Mg(OH)2 samples prepared under different hydrothermal conditions from bischofite (MgCl2.6H2O) and carnallite (KCl.MgCl2.6H2O), owing to differences in full width at half-maximum (fwhm) as well as in the intensity ratio I001/I101 of the respective diffraction peaks. According to the PCA results, the four principal components are able to explain 93% of the total variance and the samples can be classified into four main groups. For instance, the principal component PC1 can be interpreted as the crystallite size along the 101 direction since it is related to the fwhm of this peak. On the other hand, PC3 is related to orientation effects along 001 and 101 directions as it is dominated by the relative intensities of the two peaks. Finally, a comparison of the scanning electron microscopy images of the samples classified in each group revealed that in most of the cases a distinct morphology predominates within each group, which can be explained on the basis of the brucite growth mechanism.