SummaryChiral2,2',3,5',6-pentachlorobiphenyl (PCB 95),2,2',3,3',4,6'-hexachlorobiphenyl (PCB 132) and 2,2',3,4',5',6-hexachlorobiphenyl (PCB 149) were quantified in Atlantic Ocean shark liver samples (C. codolepis) by gas chromatography-mass spectrometry (GC-MS) and their enantiomeric ratios were studied by multidimensional gas chromatography (MDGC) with an achiral-chiral column combination and detected by ECD and MS/SIM. The concentration range of the chiral PCBs was from 2 to 6 ng/g (fresh weight), which represents 2-6 % of the total PCB mean concentration. The investigations revealed a small enantiomeric bias of PCB 132 in most of the samples studied (ER = 0.75-0.89, ee = 6-14%), while PCB 95 and PCB 149 were present in racemic or almost racemic form.