A method for analysis of hydroxylated metabolites of polychlorinated biphenyls (OH-PCBs) was developed and adopted to the previously described method for determination of PCBs and methylsulfonyl-PCBs (MeSO2-PCBs) in human liver and adipose tissue. The concentrations of OH-PCBs (14 congeners), MeSO2-PCBs (24 congeners), and PCBs (17 congeners) in five paired samples of human liver and adipose tissue are reported. The sum of OH-PCB congeners was higher in liver (7-175 ng/g lipids) than in adipose tissue (0.3-9 ng/g lipids). In both liver and adipose tissue, 2,2',3,4,4',5'-hexachloro-3'-biphenylol (3'-OH-CB138) and 2,2',3,3',4,5'-hexachloro-4'-biphenylol (4'-OH-CB130) were the predominant hydroxylated PCB metabolites. The sum of OH-PCB congeners were of the same order of magnitude as those of methylsulfonyl metabolites of PCB in the same samples, 12 to 358 ng/g lipids and 2 to 9 ng/g lipids in liver and adipose tissue, respectively. The levels of PCBs were similar in liver and adipose tissue, 459 to 2,085 ng/g lipids and 561 to 2,343 ng/g lipids, respectively. The sum of OH-PCBs and the sum of MeSO2-PCBs correlated to the sum of PCBs. The determined PCB metabolites constituted 3 to 26% of total PCB concentration in the liver and 0.3 to 0.8% of total PCBs in the adipose tissue samples.