Development of a subcritical fluid extraction and GC–MS validation method for polychlorinated biphenyls (PCBs) in marine samples

This paper describes a new procedure for extracting polychlorinated biphenyls (PCBs) from marine samples using subcritical 1,1,1,2-tetrafluoroethane (R134a). The extraction procedure was optimized at temperatures varying from 20 to 70 °C and pressures ranging from 3 to 15 MPa. The volume of the co-solvent was then optimized using 1,1,1,2-tetrafluoroethane (R134a) as the subcritical phase. PCBs were characterized by GC–MS using the optimized conditions of 3 MPa, 30 °C, and a co-solvent volume of 6 mL. The average yields of PCBs from subcritical fluid extraction of spiked oyster samples were measured and found to be greater than 90%, with relative standard deviations (RSD) of less than 10%. Detection limits of this method were in the range of 0.045–0.108 ng/g of dry mass. The method was compared to Soxhlet extraction and then applied for monitoring PCBs in oysters from Qingdao, Shandong, China.

► A method for determination of PCBs in marine products was developed.
► 1,1,1,2-Tetrafluoroethane (R134a) is used as subcritical fluid.
► Several factors were employed to optimize the conditions of the extraction.
► High extraction efficiency could be obtained at low pressure and temperature.
► The proposed method was successfully applied to the real samples.