Volatile compound dynamics during ripening of marmelada bola and curriola assessed by headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry

The fruits of marmelada bola (<italic>Alibertia edulis</italic>) and curriola (<italic>Pouteria ramiflora</italic>) from the Brazilian Cerrado exhibit distinct flavors and aromas. However, the mechanisms underlying aroma development during ripening are poorly understood. This study aimed to identify and monitor changes in volatile organic compounds (VOCs) at three ripening stages, i.e., mature green (MG), half-ripe (HR), and fully ripe (FR), using headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography–mass spectrometry (GC–MS). Three fibers were tested. Polydimethylsiloxane/divinylbenzene (PDMS/DVB) extracted the highest number of VOCs from both fruits. Sixteen compounds were identified in marmelada bola and 15 in curriola. Esters were the predominant chemical class, followed by alcohols in marmelada bola and terpenoids in curriola. VOCs levels generally increased with ripening, especially esters and aldehydes such as methyl hexanoate and 2-dodecenal in marmelada bola, and ethyl hexanoate and ethyl octanoate in curriola. Principal component analysis and hierarchical cluster analysis confirmed the changes in the volatile profile across ripening stages and highlighted the superior efficiency of PDMS/DVB fiber. Some compounds were only detected at specific ripening stages, suggesting their potential as ripeness markers. These results contribute to understanding the biochemical basis of aroma formation in native Cerrado fruits and may support their valorization in the food industry.