The production of palm sugar (Arenga pinnata) traditionally involves four main stages, including tapping, cooking, cooling and moulding. Regional differences in processing methods and the use of natural preservatives during sap tapping in Indonesia are expected to influence its chemical composition and sensory quality. This study investigated the volatile compound profiles and sensory attributes of palm sugar from Bangka, Central Bangka, West Bangka, and Pangkal Pinang, and examined their correlations. Volatiles were analyzed using headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry (HS-SPME/GC–MS), and sensory attributes were evaluated through quantitative descriptive analysis (QDA). A total of seventy-six volatile compounds were identified, such as heterocyclics, aldehydes, ketones, alcohols, esters, phenols, acids, sulfur compounds, hydrocarbons, and amines. The use natural preservatives significantly affected pH and ash content, whereas moisture levels remained unaffected by processing conditions. Principal component analysis (PCA) revealed distinct regional sensory profiles. Palm sugar from Bangka (jackfruit wood, Ca(OH)2), Central Bangka (mangosteen leaves), and West Bangka (resak wood) was characterized by coconut flavor, coconut aroma, and sweetness. In contrast, Central Bangka samples prepared with ube-ube roots exhibited sweet potato and honey-like notes with smoky and woody characteristics, while Pangkal Pinang palm sugar was dominated by caramel flavor and bitterness. Partial least squares (PLS) regression demonstrated positive correlations between volatile compounds and sensory attributes of flavor, aroma, and taste, with the exception of sourness. These findings indicate that traditional processing and preservation practices greatly influence the chemical and sensory quality of palm sugar.
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