Mercado-Adrover, José E.

Profile Picture

Filters

20181
Reset filters

Settings

Citations

Publication Search Results

Now showing 1 - 1 of 1
  • Thumbnail Image
    Publication
    A diffuse reflectance NIR spectroscopy method for determine drug concentration in pharmaceutical production tablets based on a PLS calibration model from manufactured tablets
    (2018-05) Mercado-Adrover, José E.; Romañach, Rodolfo J.; College of Arts and Sciences - Sciences; Torres, Wildeliz; Méndez Román, Rafael; Melendez, Enrique; Department of Chemistry; Estévez, L.Antonio
    A diffuse reflectance near-infrared (NIR) spectroscopy method was developed to determine the active pharmacological ingredient (API) in pharmaceutical production tablets from batch and continuous manufacturing processes. Tablets of six different API concentration manufactured by batch processes were used as the calibration set. Forty tablets were used for each concentration level. Partial Least Squares (PLS) regression was used to develop the calibration models. The NIR calibration model was challenged using two independent test sets of pharmaceutical production tablets with the same API concentration: one of tablets from a batch process and other tablets from a continuous process. The tablet NIR spectra were acquired using the integrating sphere from the FT-NIR spectrometer at a resolution of 32 cm-1 and 32 scans at both sides of the tablets. The Root Mean Square Error of Prediction (RMSEP), the Relative Standard Error of Prediction (RSEP), and bias were calculated to evaluate the predictive capability of the calibration models. The NIR model predict the API concentration of the tablets test set from a batch process with acceptable values. RMSEP of 0.338% (w/w) and a RSEP of 0.611% were obtained. For the continuous process tablets test set, a difference in the API concentration was found between each side of the tablets. Material segregation and the level of shear exposure in the continuous manufacturing line are possible explanations for these differences in API concentration between the tablets sides. RMSEP of 1.441 (%w/w) was obtained for the side of the tablet with the correct API concentration. RMSEP of 1.971 (%w/w) was obtained for the side with a higher API concentration than the correct amount. An overall RMSEP of 2.526 (%w/w) was obtained evaluating both sides simultaneously of the continuous process tablets. The NIR calibration model developed with a calibration test from a batch process has the ability to predict the API concentration of tablets manufactured batch and continuous process.