Near-infrared reflection spectroscopy (NIRS) as a successful tool for simultaneous identification and particle size...

A successful application of NIR spectroscopy (NIRS) in combination with multivariate data analysis (MVA) for the simultaneous identification and particle size determination of amoxicillin trihydrate particles was developed. Particle size analysis was ascertained by NIRS in diffuse reflection mode on different particle size fractions of amoxicillin trihydrate with D90 particle diameters ranging from 6.9 to 21.7 μm. The present problem of fractionating the powder into good enough size fractions to achieve a stable calibration model was solved. By probing dried suspensions measurement parameters were optimized and further combined with the best suitable chemometric operations. Thereby the quality of established regression models could be improved considerably. A linear coherence between particle size and absorbance signal was found at specific wavenumbers. Satisfactory clustering by particle size was achieved by principal component analysis (PCA) whereas partial least squares regression (PLSR) and principal component regression (PCR) was compared for quantitatively calibrating the NIRS data. PLSR turned out to predict unknown test samples slightly better than PCR.