Characterization of key aroma-active terpenes in Brazilian seasonings using eco-friendly DI-SPME with GC×GC-MS and odor activity value workflow

Brazilian seasonings exhibit a rich variety of flavors that are largely attributed to terpenes. However, the systematic identification of the key aroma-active terpenes in these seasonings are poorly identified, lacking characterization by sustainable and high-resolution analytical methods. This study aimed to develop an integrated, environmentally friendly analytical protocol to characterize aroma-active terpenes in 26 traditional Brazilian seasonings. A novel solvent-minimized extraction method, hydrophilic microporous cartridge for direct immersion solid phase microextraction (HMCart-DI-SPME), was optimized by a factorial design for efficient recovery of volatile and semi-volatile terpenes. Analysis by comprehensive two-dimensional gas chromatography coupled to mass spectrometry (GC×GC/MS) identified 125 terpenes from five classes. Odor activity values (OAVs) were calculated for 48 compounds to assess their contribution to the aroma profile. Notably, high OAVs of eucalyptol, linalool, pulegone and geraniol confirmed their central role in the seasoning's sensory properties. The integrated strategy combining HMCart-DI-SPME, GC×GC/MS and OAV analysis enabled an unprecedented resolution of these complex matrices. This methodology offers an effective, environmentally friendly alternative for flavor analysis, contributing to the chemical valorization of Brazilian biodiversity. The robust data produced has significant potential applications in the food, pharmaceutical and fragrance industries.