5-(4-Pyridyl)-2-thiophenecarbaldehyde has been prepared as a new fluorescent derivatization reagent and utilized for the determination of primary alkylamines. A definite detection limit was achieved for the amines by using a method based on the combination of precolumn derivatization and postcolumn hydrolysis–detection of the original fluorescent reagent regenerated from the derivatives. Approximately a 0.1 pmol (10 μl injection)(S/N= ...