An accurate and simple analytical technique for low levels of fallout Pu in the environment was developed using an anion exchange resin. To develop the reliable determination of Pu isotopes in soil samples, decomposition of soil matrix, plutonium oxidation state adjustment on the anion exchange column and source preparation of Pu isotopes have been carried out. The optimum method of Pu isotopes with an anion exchange has been validated by application to IAEA-Reference soils.