Coffee, one of the most widely consumed commodities globally, embodies a sensory experience deeply rooted in social, cultural, and hedonic contexts. The cold brew (CB) method, characterized by cold extraction, is a refreshing and unique alternative to traditional coffee. Despite its growing popularity, CB lacks defined preparation parameters and comprehensive analysis of its aromatic composition. In this study, we aimed to obtain a representative extract of the volatile matrix of CB and characterize the aroma of sensory-active compounds using advanced techniques such as headspace–solid-phase Microextraction (HS-SPME) and headspace-solid-phase extraction (HS-SPE) for volatile compound extraction, followed by gas chromatography–olfactometry–mass Spectrometry (GC-O-MS) for compound identification. Optimization of the HS-SPME parameters resulted in the identification of 36 compounds, whereas HS-SPE identified 28 compounds, which included both complementary and similar compounds. In HS-SPME, 15 compounds exhibited sensory activity with descriptors such as floral, caramel, sweet, and almond, whereas seven exhibited sensory activity with descriptors such as chocolate, floral, coffee, and caramel. This comprehensive approach to HS-SPME and HS-SPE aroma extraction with GC-O-MS offers an efficient methodology for characterizing the aroma profile of CB, paving the way for future research and quality standards for this innovative coffee beverage.

The objective of the present work is to characterize the aroma of “Cerrado” cashew (Anacardium othonianum Rizz.) and cagaita (Eugenia dysenterica) pulps. For this, we used headspace (HS) and two extraction methods (solid-phase extraction, SPE and solid-phase microextraction, SPME), as well as gas chromatography-olfactometry (GC-O) and gas chromatography-mass spectrometry (GC-MS) for identification of aroma compounds. While SPME was more efficient and extracted 17 and 21 compounds for “Cerrado” cashew and cagaita pulps, respectively, the SPE method extracted 13 compounds for both pulps. SPME showed higher modified frequency (MF), that is, compounds perceived with higher intensity and by number of judges during olfactometry. On the other hand, the results obtained in this work showed that the extraction techniques seem complementary, since some compounds were not identified by SPE, but were identified by SPME, and vice versa.