The aim of this study was to assess the suitability of the perirenal fatty tissue for the determination of an organochlorine pesticide. Fatty tissue samples were prepared by the matrix solid phase dispersion (MSPD) method, and pesticide levels were determined by gas chromatography on capillary column using an electron capture detector. Results were confirmed by gas chromatography/mass spectrometry (GC/MS) system. The results showed that the perirenal fatty tissue contained significantly higher levels of hexachlorobenzene (HCB) than the dorsal fatty tissue (P < 0.01). All the levels were below the criteria for maximum residue limits established by Croatia and the EU.