In this study, a high vacuum flavor extraction (HVE) device was developed to address the limitations of traditional extraction methods, such as extended extraction times and artifact generation during high-temperature processes. Firstly, the repeatability and precision of the HVE method were evaluated through quantitative analysis of twelve volatile odor compounds across seven replicate extractions using gas chromatography–flame ionization detection (GC-FID). The results showed that the HVE system achieved a mean relative standard deviation (RSD) of 11.60 ± 1.79% and a recovery rate of 90.55 ± 4.56%, demonstrating its precision and reproducibility. Secondly, the performance of HVE was compared with solvent-assisted flavor evaporation (SAFE) and simultaneous distillation–extraction (SDE) for extracting flavor compounds from fried tilapia mince. The results indicated that HVE was more effective, particularly in extracting aldehydes and pyrazines, which are key contributors to the flavor profile. Finally, sensory evaluations supported these findings, showing that the odor profiles obtained through HVE were most similar to the original sample, with a similarity score of 72.55%, compared to 69.25% for SAFE and 60.29% for SDE. These findings suggest that HVE is a suitable method for the extraction and analysis of volatile compounds in complex food matrices such as fried tilapia mince.