Preservatives used in smokeless tobacco products may include sodium propionate, potassium sorbate or sodium benzoate. In order to meet the requirements of regulatory agencies, there is a need for analytical methods to measure low-level preservatives. A fast and efficient method was developed and validated for the determination of these preservatives in smokeless tobacco products by GC/MS. Acidified methanol was used for sample extraction. Chromatographic separations were performed using Stabilwax-DA GC column (30 m × 0.25 mm × 0.25 µm). The carrier gas was helium with a flow rate of 0.9 mL/min. The injection volume was 0.5 µL using splitless injection mode. The separation was performed using an oven temperature gradient from 50 °C to 220 °C. Mass spectrometry data were acquired in selected ion monitoring mode. This study highlights the results from the parameters used to successfully validate the method.