Researchers often face limitations when drying solvent mixtures in purification workflows, as traditional freeze dryers are incompatible with organic solvents. This article investigates the adaptation of centrifugal evaporators for combined evaporation–lyophilization processes. Using model systems containing water and acetonitrile, optimized multi-stage methods were established to achieve rapid, uniform drying with powder-like sample consistency. The findings demonstrate that hybrid centrifugal lyophilization significantly reduces processing time and enhances reproducibility, offering a scalable, high-throughput solution for analytical and preparative laboratories.