## 4 Conclusions  
Research on aromatic compounds in CB coffee using GC-O-MS through solid-phase extraction (HS-SPE) and headspace solid-phase microextraction (HS-SPME) has yielded significant and complementary results. HS-SPME identified a broader range of volatile compounds, whereas HS-SPE provided information that HS-SPME could not capture. This duality offers a comprehensive understanding of CB aromas and maximizes the information obtained by considering them complementary rather than competitive techniques. Thesemethodologies thoroughly analyze the aromatic compounds crucial for sensory perception. The HS-SPE system is effective and adaptable to the complex matrix of CB. The optimization of HS-SPME has led to an efficient and sensitive methodology that allows for a complete profile of volatile compounds. This approach enabled the identification of compounds with a high contribution to aroma. For HS-SPME, compounds such as 1,5-octadien-3-one, 5-methylfuran-2-carbaldehyde, 2-ethyl-3,5-dimethylpyrazine, and benzaldehyde were identified with descriptors including floral, caramel, sweet, and almond. In contrast, HS-SPE identified compounds such as 2,6-dimethylpyrazine, 2-ethyl-6-methylpyrazine, furaneol, and furfuryl alcohol, with descriptors such as chocolate, floral, coffee, and caramel. Consequently, the CB samples exhibited an aroma profile dominated by floral and sweet notes, consistent with the literature [1,5]. The overall conclusion highlights the significant contribution of both HS-SPE and HS-SPME techniques in understanding the aromatic profiles of CB coffee. Additionally, the applicability, practicality, and short analysis time of HS-SPME align with the principles of green chemistry, thereby emphasizing its efficiency and sustainability. This opens the possibility for future comparative studies and additional methodologies for aroma reconstruction through the quantification of the identified compounds, providing a solid foundation for advancing knowledge in CB aroma. The following supporting information can be downloaded at: [[https://www.mdpi.com/article/10.3390/molecules29163791/s1](https://www.mdpi.com/article/10.3390/molecules29163791/s1)]([https://www.mdpi.com/article/10.3390/molecules29163791/s1](https://www.mdpi.com/article/10.3390/molecules29163791/s1)). Table S1: Operational variables to optimize solid-phase microextraction in its headspace mode (HS-SPME) with their respective injection order obtained from the Box-Behnken design of experiments. Table S2: Results of the response parameters (total area and number of peaks) from solid- phase microextraction in its headspace mode (HS-SPME) (Agilent), with manual injection into the Agilent 6890N gas chromatograph with a flame ionization detector (FID), varying the extraction time, equilibrium time, fiber type, and sample volume based on the experimental design shown in Table 5, with two types of data handling: analysis of the entire chromatogram and segmented analysis (Segment 1: [0-15] min; Segment 2: [15-28] min; and Segment 3: [28-52] min). Table S3: Retention times (RT) and Kovats retention indices (RI) of the analyzed alkanes (C7-C30). Table S4: Compounds with Aroma that Could Not Be Identified (KI: Experimental Kovats Retention Index, MF: Modified Frequency, Compound: Tentative Compound Identified, KI(i): Theoretical Kovats Retention Index for Compound i, i: Compound i identified by NIST19. Conceptualization, E.N., E.Z., J.Z. and J.D.D. ; methodology, E.N., E.Z., J.Z. and J.D.D. ; optimization, E.N. and E.Z. ; formal analysis, E.N. and E.Z. ; investigation, E.N., E.Z., J.Z. and J.D.D. ; resources, E.N., E.Z., J.Z. and J.D.D. ; data curation, E.N., E.Z., J.Z. and J.D.D. ; writing--original draft preparation, E.N. and E.Z. ; writing--review and editing, E.N., J.Z. and J.D.D. ; visualization, E.N., E.Z., J.Z. and J.D.D. ; supervision, J.Z., S.T.-G. and C.L. ; project administration, J.Z., S.T.-G. and C.L. ; funding acquisition, S.T.-G. and C.L. All authors have read and agreed to the published version of the manuscript.