经匀浆的鱼肉样品置于20 mL顶空瓶中,加入氯化钠3.0 g,水1 mL及pH 2.0硫酸溶液9 mL,于40 ℃超声萃取30 min。将顶空瓶放入带固相微萃取装置的Combi PAL全自动进样器中,于90 ℃温度下加热20 min后,用85 μm聚丙烯酸酯萃取头固相微萃取10 min,于280 ℃热解3 min,用HP-5毛细管柱分离后,用气相色谱法(电子捕获检测器)测定五氯酚的含量。五氯酚的线性范围在0.05~100 μg·L-1之间,方法的检出限(3S/N)为0.02 μg·L-1。在3个浓度水平(1.0,5.0,50.0 μg·kg-1)上对方法的回收率进行试验,测得回收率在81.2%~89.4%之间,测定值的相对标准偏差(n=6)在4.2%~7.1%之间。

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%.