A formulation of lactose anhydrous and starch 1500 processed in a high-shear granulator was monitored during the drying phase using an XDS Process Analyzer with an in situ near-infrared process probe. Methanol initially was added to a nominal level of 8.0% methanol to affect wet granulation. The mixture was dried by applying heat and a vacuum to the single-pot granulator and was analyzed for methanol content with a probe of novel design made for this application. Multivariate prediction models were developed for methanol with good predictive results.