<p>Smokeless tobacco (ST) is consumed globally and plays a significant role in health, culture, and consumption. This study analyzes heavy metals, active ingredients, and adulteration in ST products from two origins. It introduces advanced spectroscopic techniques to reveal the molecular composition, providing insights into health impacts and cultural significance. Inductively coupled plasma mass spectrometry (ICP-MS) and gas chromatography-mass spectrometry (GC–MS) were used to analyze the Sudanese and Yemeni varieties of ST. The heavy metal analysis included arsenic (As), selenium (Se), silver (Ag), cadmium (Cd), antimony (Sb), mercury (Hg), thallium (Tl), and lead (Pb). GC–MS was used to detect the active ingredients and adulterants. Principal component analysis (PCA) and hierarchical cluster analysis (HCA) were used for chemometrics. Qualitative analysis of ST samples from Sudan (S) and Yemen (Y) highlighted different active ingredient compositions, with Sudanese samples showing a broader range than the Yemeni samples. No adulteration was detected in any of the samples, indicating their purity. The heavy metal concentrations varied notably with As, Se, and Hg levels. PCA results showed distinct variable loadings for three components. The convergence of the rotation method in five iterations indicated result stability. Component 1 explained 35.382% of the variance, component 2 explained 31.025%, and component 3 explained 22.314%, cumulatively accounting for 88.721%. HCA grouped samples into distinct clusters based on heavy metal content. These findings provide insights into the composition, purity, heavy metal levels, and interrelationships of Sudanese and Yemeni smokeless tobacco samples, enhancing our understanding of their chemical characteristics.</p>