A new spectrofluorimetric method was developed in this study for simple determination of cadaverine (CD) (1,5-diaminopentane) in flesh of mackerel fish. This method required homogenization of the flesh, solid phase extraction (SPE) with 0.4M HCl/methanol or water/methanol (25/75v/v), centrifugation and derivation with orthophthalaldehyde (OPA). Physico-chemical parameters that affected the sensitivity of the fluorescence signal of the cadaverine-dihydrochloride/orthophthalaldehyde complex (CD/OPA), were optimised; these included reaction time, temperature, solvent system, pH and reactants concentrations (OPA/CD). The study was conducted in acetate buffer (pH 3.5 and 7) and showed low limits of detection (LOD), 0.6 and 25.5 ng. mL -1 respectively. The limits of quantification (LOQ) obtained were 3.5 ngmL -1 (pH 3.5) and 122 ngmL -1 (pH 7). The sensitivity of the results allowed its satisfactory application for quantification of cadaverine in fish.