In this paper, we proposed a rapid, precise, accurate, and reproducible methodology using capillary zone electrophoresis (CZE) with dynamically coated capillaries for separation and determination of tobacco-specific nitrosamines (TSNAs), a group of strong carcinogens found only in tobacco products.For the determination of these alkaloids, dynamic coating of the capillary surface is accomplished using a commercially available reagent kit with a polycation coating CElixir Reagent A, followed by polyanion coating CElixir Reagent B (pH 2.5).