GC Determination of Pentachlorophenol in Fish with Separation by SPME

The homogenized fish sample was extracted ultrasonically at 40 ℃ for 30 min in a solution containing 3.0 g of NaCl, 1 mL of H2O and 9 mL of H2SO4 solution of pH 2.0 in a 20 mL headspace bottle, which was then placed into the Combi PAL automatic sample injector (installed with SPME device), heated at 90 ℃ for 20 min and separated by SPME for 10 min, with the 85 μm PA extractor. After pyrolysis at 280 ℃ for 3 min, and separation on HP-5 capillary column, content of pentachlorophenol (PCP) was determined by GC with ECD. Linearity range of mass concentration of PCP was found between 0.05-100 μg·L-1, and the detection limit (3S/N) was found to be 0.02 μg·L-1. Recovery was tested at 3 concentration levels of 1.0, 5.0, 50.0 μg·kg-1, results of recovery found were in the range of 81.2%-89.4%, with values of RSD′s (n=6) ranged from 4.2% to 7.1%.