In the production plant of an antibiotic substance, a new fluidized-bed drier has been installed. For online process control of the drying progress and determination of the ideal drying end point, a continuous near-infrared spectroscopic (NIRS) measuring setup was implemented to rapidly and simultaneously gain all essential product information. A bypass system outside the drier combined with a robust process probe proved to provide the best sampling system geometry. The spectrometer was equipped with an additional laboratory probe for complementary offline analysis. Multivariate calibrations for product assay, water content, and residual solvent were calculated, optimized, and compared for the two probes. The final root-mean-square error of cross validation (RMSECV) for the process probe could be reduced to 0.81% for the product assay, 0.25% for water, and 0.06% for acetone. The laboratory-probe prediction values show good agreement with reference data during the testing period. The calibrations of the process probe were checked by comparing its predictions to those of the validated laboratory probe. The monitoring system could be automated to a large extent, and product quality could be improved considerably. The established technology is of high importance for the pharmaceutical industry carrying out high-throughput routine analysis because of its advantages in terms of of time and cost reductions.