Determination of Indicator Polychlorinated Biphenyls in Aquatic Products by Double Depuration/Gas Chromatography
  
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DOI:10.3969/j.issn.1004-4957.年份.月份
KeyWord:double depuration  gas chromatography(GC)  polychlorinated biphenyls(PCBs)  residues  aquatic products
  
AuthorInstitution
DING Li-ping,CAI Chun-ping,WANG Dan-hong 1.福清出入境检验检疫局技术中心;2.福建出入境检验检疫局技术中心
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Abstract:
      To study the residues of seven kinds of indicator polychlorinated biphenyls in aquatic products,a method was established for the determination of trace polychlorinated biphenyls in aquatic products by double depuration coupled with gas chromatography(GC).With the mixture of acetone-n-hexane(1∶4) as extract,the samples were extracted,purified by adding concentrated sulfuric acid followed by clean up with silica gel in dispersive solid phase extraction protocol,and then analyzed by gas chromatography.Under the optimized chromatographic conditions,the analysis was carried out on an HP-5 quartz capillary column(30 m×0.32 mm×0.25 μm) at a flow rate of 0.80 mL/min,and the sample volume was 1.00 μL.Monitored with an electron-capture detector,all the target analytes were separated by “temperature-programming ”.Good linearities were obtained in the range of 10-500 μg/kg for seven indicators of polychlorinated biphenyls(PCBs) with correlation coefficients greater than 0.99.For different matrices,the limits of detection(S/N=3) and limits of quantitation(S/N=10) were in the ranges of 0.72-4.1 μg/kg and 2.4-13.7 μg/kg,respectively.At three spiked levels of 10,20,100 μg/kg,the average recoveries of seven indicators of polychlorinated biphenyls(PCBS) from butterfish,shrimp and mussel samples ranged from 76.5% to 104.8% with RSDs of 1.6%-10.4%.The method was simple,rapid and accurate,and could be used for the routine analysis of indicator polychlorinated biphenyls(PCBs) in aquatic products.
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