摘要
经匀浆的鱼肉样品置于20mL顶空瓶中，加入氯化钠3．0g，水1mL及pH2．0硫酸溶液9mL，于40℃超声萃取30min。将顶空瓶放入带固相微萃取装置的CombiPAL全自动进样器中，于90℃温度下加热20min后，用85μm聚丙烯酸酯萃取头固相微萃取10min，于280℃热解3min，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0．05－100μg·L-1之间，方法的检出限（3S／N）为0．02μg·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4．29／6～7．19／6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 HzO and 9 mL of H2SO4 solution of pH 2.0 in a 20 mL headspaee bottle, which was then placed into the Combi PAL automatic sample injector （installed with SPME device）, heated at 90 C for 20 min and separated by SPME for 10 rain, with the 85 μm PA extractor. After pyrolysis at 280 ℃ for 3 rain, 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%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2011年第9期1026-1028,共3页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
常州市自然科学基金资助项目(CS2008209)
