An accurate, inexpensive and less laborious liquid–liquid extractive spectrophotometric procedure for the determination of Zinc in aqueous media has been developed. 1-phenyl-1-hydrazonyl-2-oximino propane – 1,2 – dione (HPHOPD) reagent was used for extractive spectrophotometric determination of Zinc (II). HPHOPD reagent formed a complex with Zinc (II) in n-butanol. Comprehensive study was carried out for maximum extraction conditions. Maximum extraction was obtained at pH 8.5. The extracted species has absorption maxima at 415 nm and obeyed Beer's law over the range 1 – 20 ppm of Zinc. The molar absorptivity at this wave length is 0.156 × 103 Lit Mol-1cm-1. The proposed method is selective for Zinc (II) and was satisfactorily applied to the determination of the total Zinc in food and pharmaceutical samples.