An evaluation of specific polychlorinated biphenyl (PCB) congener residues in human adipose tissue was conducted to compare the ability of gas chromatography with electron capture detection (GC) and gas chromatography/mass spectrometry (GC/MS) to quantitate specific PCB congeners. Adipose tissue samples collected from 76 persons, 40 males, living in five cities of the Great Lakes region were analyzed for 16 PCB congeners by GC/ECD and GC/MS. The GC/ECD system used SPB-5 and SPB-35 bonded phase fused silica capillary columns. The GC component of the GC/MS system used SPB-5 and DB-17 bonded phase fused silica columns. The concentrations of 2,4,4',5-tetrachlorobiphenyl, 2,2',4,4',5-pentachlorobiphenyl, 2,3',4,4',5-pentachlorobiphenyl (74472370), 2,2',3,4,4',5,5'-heptachlorobiphenyl, 2,2',3,4',5,5',6-heptachlorobiphenyl, 2,2',3,3',4,4',5,5'-octachlorobiphenyl, 2,2',3,3',4',5,5',6-octachlorobiphenyl (68194172), 2,2',3,3',4,4',5,5',6-nonachlorobiphenyl (40186729), and decachlorobiphenyl (2051243) were essentially similar whether obtained by GC/ECD or GC/MS and ranged up to 263 nanograms per gram. The concentrations of the other compounds mostly penta and chlorinated congeners measured by GC/ECD were significantly higher than when measured by GC/MS. The most reliable data were obtained with GC/MS using the DB-17 column. The poorer precision in the GC/ECD systems was due to poor resolution resulting from coelution of some of the analytes. The authors conclude that when determining PCB congeners in human adipose tissue GC/MS using a more polar column such as DB-17 gives the best results. When using GC alone, the ability of the column to resolve PCB congeners should be verified.