A method has been developed for the extraction and preconcentration of copper, nickel, cadmium and zinc from water samples with 6-methyl-2-pyridinecarboxaldehyde-4-phenylsemicarbazone (MPPSC) into chloroform at pH9. Chloroform was evaporated and the residue was digested in nitric acid. After adjustment of volume, metal ions were determined using air-acetylene flame atomic absorption spectrometer. The recovery of metal ions were 95-100% with coefficient of variation (C.V) within 3.2%. Preconcentration obtained was 12-30 times. The method was applied for the determination of the metal ions in drinking water of Hyderabad city and Jamshoro.