The reagent 2-pyrroladehyde-4-phenyl-3-thiosemicBl'bazone(PAP1) was examined as complexing reagent for solvent extraction of copper(I1), iron(II) nickel(ll) and mercury (II). The study was carried out by spectrophotometry and liquid chromatoghraphy. The complexes indicated molar absorptivity in the range of 8.85 to 63.4xl03 I.mole-1 cm-1 and eluted from Microsorb C-18, 5um (IS0x4.6 mm id) with methanol:acetonitrile:water: sodium acetate (ImM) and tetrabutyl ammonium bromide (1mM) (60:28:10:1:1 v/v/v/v/v) using a flow rate of 1 ml/min. Detection UV was at 254 nm. The method was applied for determination of the metal in Fuleli canal water after preconcentration by complexation and solvent extraction and amounts found were within 27-250 µg/L with coefficient of variation (C.Y) within 2.7 to 5.1%. The method was also applied for determination of copper(Il), iron(Il), nickel(Il) and mercury(Il) in surface water fishes in the range 0.021-1.2 ug/g with C.V 1.1-6.4%. The obtained results indicated good correlation with flame atomic absorption spectrometry.