Abstract: In the present study, a highly sensitive Gas Chromatographic-Mass Spectrometric (GC-MS) method and single-step extraction procedure have been developed for the determination of nicotine level in Hookah tobacco products samples. The principle focus of the developed method is the lower limit of detection (0.025 ng mL–1) and a wide linear range (0.03-17000 ng mL–1) achieved that can have important implications in the determination of nicotine in any investigated samples. In addition, the accuracy and precision values of the method were in the range of 98.07-103.81 and 0.2660-1.7712%, respectively. While the extraction recovery of nicotine, when spiked to hookah tobacco products was ranged from 94.85-98.00%. The present chromatographic method showed higher sensitivity, linearity precision and accuracy, when compared with the reported chromatographic methods. Finally, the hookah tobacco products samples were used to evaluate the method applicability for the determination of nicotine.