AbstractIn this study, we successfully employed a 19F‐labeled cyclopalladium probe to achieve simultaneous differentiation and detection of various amines and N‐heterocyclic compounds. This method features a broad detection window, facilitating the discrimination and multi‐component analysis of structural analogs and isomers through the generation of characteristic 19F NMR signals with distinct chemical shifts. The utility of this approach is demonstrated in monitoring chemical reactions and identifying components in food, beverages, and cosmetics.