This study aimed of examining of the applicability of the SIS (Selected Ion Storage) and the MS/ MS (Tandem Mass Spectrometry) methods for analyzing organochlorine pesticide (OCs) residues and PCBs in human specimens. The samples of human abdominal adipose tissue, women's breast adipose tissue, and human milk were used as study material. The samples were analyzed using the gas chromatography method with EC and MS detectors. MS/MS and SIS mode allow to eliminate system-based (e.g., column, septum) ions and the biological samples extract impurities' ions from the background to achieve the analytical system sensitive enough for trace analysis of organochlorine compounds in human specimens.