Aromas play a crucial role in shaping consumer acceptance of food products. Investigating the volatile organic compounds (VOCs) produced during fermentation provides insight into which microorganisms or substrates generate specific VOCs and how these compounds influence sensory perception and consumer preference. This chapter describes a reproducible protocol for identifying and evaluating the VOCs in solid-state fermented foods using headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry (HS-SPME-GC–MS) and sensory evaluation via check-all-that-apply (CATA). Using tempeh as a model, combining analytical analysis with sensory analysis allows us to better characterize the fermented product.