Abstract: GC was applied to the determination of 10 polychlorinated biphenyls in seawater with large volume solid phase extraction.The seawater sample was extracted by large volume sampler and cleanert PS solid phase extraction column.Extracting flow rate found was 5.0 mL·min-1,and acetone was used as eluent.The analytes were separated on Agilent HP-5 quartz capillary chromatographic column (30 m×0.32 mm,0.25 μm) and detected by μECD.Linear relationships between values of peak area and mass concentration of 10 polychlorinated biphenyls were kept in the same range within 10.0 μg·L-1,with detection limits (3S/N) in the range of 0.002 3-0.012 μg·L-1.Values of RSD′s (n=7) found were in the range of 0.9%-1.3%.Tests for recovery were made by standard addition method at the concentration levels of 0.5,1.5,4.0 μg·L-1,giving values of recovery in the range of 80.7%-127%.