Predictive evaluation of powder X-ray diffractograms of pharmaceutical formulation powders based on infrared spectroscopy

Abstract

BACKGROUND: To ensure quality and stability, monitoring systems are recommended to analyze pharmaceutical manufacturing processes. OBJECTIVE: This study was performed to predict powder X-ray diffraction (PXRD) patterns of formulation powders through attenuated total reflectance (ATR)-infrared (IR) spectroscopy in a nondestructive manner along with chemometrics. RESULTS: Caffeine anhydrate, acetaminophen, and lactose monohydrate were grinded at six weight ratios. The six sample groups were evaluated using ATR-IR spectroscopy and PXRD analysis. Partial least squares models were constructed to predict the PXRD intensities of the samples from the ATR-IR spectra. The prediction accuracy on the prepared PLS regression models was as high as R2 = 0.993. CONCLUSIONS: Linear relationships were obtained between the prediction data set and reference PXRD intensity at each degree. 2D PLS regression coefficient analysis enabled the analysis of the correlation between PXRD patterns and IR spectra.