This dataset contains the raw data generated during the master’s research on the microencapsulation of liquid smoke by spray drying. The data are divided into three main parts: (1) characterization of the liquid smoke, encompassing volatile compounds analysis — with comprehensive GC-MS chromatographic fingerprints for global volatile profiling and targeted GC-FID chromatograms for estimating the area values of selected marker compounds — together with its physicochemical characterization; (2) microencapsulation process, with operating parameters and feed formulations, and mass balance of the process; and (3) characterization of the resulting microparticles, including moisture content, water activity, particle size distribution, morphology, and also GC-MS and GC-FID chromatograms. The dataset generally provides raw chromatograms (in PDF and instrument-native formats) and experimental spreadsheets, exported directly from the instruments/software without any post-processing. In cases where a file contains processed data, this is explicitly stated in its individual description.