in the Amazonas, Caqueta, Putumayo, and Guaviare regions, where fruit butter is primarily exported to Brazil for use in the cosmetic industry [5]. Copoazu fruit is renowned for its excellent texture, flavor, and aroma, with its economic value derived from the utilization of its pulp, seeds, and peel [6]. The fruit has therapeutic potential attributed to its nutritional and bioactive properties that are beneficial to human health, making it valuable in the food, cosmetic, and pharmaceutical industries. The pulp, mucilaginous in texture and ranging in color from white to creamy yellow, is marketed fresh or processed into products such as jams, ice creams, juices, and yogurt [3]. It is rich in starch, pectin, polysaccharides, and dietary fiber, but primarily insoluble fiber, which enhances the sensory and textural qualities of dairy products [7]. The seeds are a significant source of fats and fatty acids, including oleic, linoleic, and stearic acids, which hold dietary importance [8]. These properties led to the production of a chocolate analog called \"cupulate\" or \"cupulado\" [2; 9]. Volatile organic compounds (VOCs) are critical quality indicators and commercial attributes that influence the sensory acceptability of fruits and their derived products, particularly in shaping organoleptic characteristics such as flavor and aroma [10]. During ripening, VOCs' synthesis and regulation are governed by metabolic pathways, making the ripening stage a key determinant of fruit sensory characteristics [11]. A detailed understanding of the volatile profile during ripening enables the identification of compounds with industrial relevance [12], thereby enhancing the value of the fruit and its derivatives as functional food products. Research on copoazu's VOCs highlights esters as the predominant group, followed by terpen and alcohols, with notable compounds including ethyl butanoate, ethyl hexanoate, and linalool [13]. Several extraction techniques, such as vacuum distillation, solid-phase extraction, and liquid-liquid extraction, have been employed to analyze such compounds [13; 14; 15; 16; 17]. However, these methods often involve multiple steps, the use of contaminating reagents, and lengthy analysis times. In contrast, headspace solid phase microextraction (HS-SPME) offers a solvent-free, cost-effective alternative, with enhanced sensitivity, selectivity, and versatility. These techniques integrate extraction, concentration, desorption, and sampling into single step, streamlining complex sample pretreatment procedures for efficient VOC determination [18; 19]. Optimizing HS-SPME factors such as extraction time and temperature, salting-out effects, sample quantity, equilibration time, and temperature typically involves a one-factor-at-a-time (OFAT) approach [20]. However, this method has certain limitations, including the requirement for numerous experiments, the inability to identify factors interactions, and difficulties in achieving a global optimal response. The Design of Experiments (DoE) is a multivariate statistical approach that addresses these limitations by enabling the simultaneous evaluation of individual and interactive variables, reducing time and cost while determining optimal parameter settings [21; 22; 23]. Response Surface Methodology (RSM), a commonly employed tool in DoE, provides visual representations of optimal values, identifies process inefficiencies, and assesses relationships between factors and responses [24; 25]. Gas chromatography-mass spectrometry (GC-MS) is a robust, reproducible, and automated analytical technique widely used to analyze VOCs across various matrices. However, the large volumes of multidimensional data generated by GC-MS analysis can be challenging to process. Therefore, multivariate statistical methods are essential for gaining a deeper understanding of the volatile profiles and condensing these extensive datasets. Volatilomics, an emerging field in omics sciences, focuses on studying plant, fruit, and microbial biochemistry by analyzing VOC composition.