[en] In a testing laboratory the quality system encompasses a set of activities planned and systematic, which ensure the traceability process of an analysis, which is based on the standards NBR ISO/TEC 17025. With the need for analysis of radionuclides in food products to meet the requirements of import and export, accreditation of testing on this standard becomes increasingly necessary. The Gamma Spectrometry is a technique used for direct determination of radionuclides in different matrices, among them the food, being possible the simultaneous determination of different radionuclides in the same sample without the need for a chemical separation. In the process of Accreditation the methodology validation is an important step that includes testing accuracy, traceability, linearity and recovery. This paper describes the procedures used to validate the assay for determining radionuclides using gamma spectrometry in food. These procedures were performed through analysis of a certificated reference material by the International Atomic Energy Agency (IAEA Soil 327), analysis of samples of milk powder prepared from the doping with certified liquid standards also by the results obtained in the participation of tests of proficiency in analysis of environmental samples. (author)