Abstract: This study investigated the differences in physicochemical properties and volatile aroma components between fresh Hotan red grapes (GR) and their dried products including dried raisins without drying agent pretreatment (NDAR) and drying agent-pretreated raisins (DAR). The results indicated that the color of raisins darkened after drying, with an increase in red-yellow values (a^*/b^*). The contents of reducing sugars, titratable acids, and ascorbic acid increased significantly. However, drying agent pretreatment reduced the lightness (L^*) and further enhanced the red-yellow values (a^*/b^*) of raisins. Additionally, it increased the reducing sugar content while decreasing titratable acidity and ascorbic acid levels. Electronic nose (E-nose) radar fingerprint plots exhibited distinct response patterns. Through qualitative and quantitative analysis of volatile compounds, 99, 109, and 108 volatile compounds were detected in GR, NDAR, and DAR, respectively. The dominant volatile classes were alcohols (48.45%) in GR, aldehydes (58.46%) in NDAR, and ketones (45.00%) in DAR. Drying agent pretreatment led to the degradation and disappearance of D-limonene, a 2.88% reduction in the relative content of aldehydes and ketones, and altered the concentrations of characteristic aroma compounds in raisins. Based on OAV (Odor Activity Value) > 1, pretreatment with drying agents weakened the concentrations of furfural, 5-methylfurfural, and nine other key aroma compounds. Furthermore, 16 key aroma compounds were screened using ROAV (Relative Odor Activity Value) ≥ 1, and three critical compounds—decanal, E-2-nonenal, and ethyl 2-methylbutyrate were identified (VIP > 1), playing a crucial role in distinguishing GR, NDAR, and DAR. While GR exhibited a significantly different aroma profile compared to NDAR and DAR, the overall aroma characteristics of NDAR and DAR were similar, but NDAR had more pronounced fruity and sweet aromas than DAR. This study elucidates the differences in physicochemical properties and volatile aroma compounds between Hotan Red grapes, drying agent pretreatment and drying agent-pretreated raisins, which provides data support and a theoretical foundation for optimizing subsequent drying processes and enhancing the flavor characteristics in Hotan Red raisin production.