Determination of 7 indicative polychlorinated biphenyls in fish and shellfish by isotope internal standard-gas chromatography-triple quadruple mass spectrometry
Objective To establish a gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS)method for the determination of 7 indicative polychlorinated biphenyls(PCBs)in fish and shellfish.Methods Homogenized fish and shellfish samples were dehydrated with anhydrous Na2SO4,PCBs were ultrasonically extracted with n-hexane+dichlo-romethane(2∶1),and the extract was purified by acidified silica gel dispersion solid phase extraction(DSPE)and alka-line alumina solid phase extraction column.After concentration,the target analytes were separated on DB-XLB chromato-graphic column,analyzed by GC-MS/MS under multiple reaction monitoring(MRM)scanning mode,and quantified by i-sotope internal standard method.Results In this method,the calibration curves for all target analytes showed good linearity in the range of 0.5-20.0 μg/L(r＞0.999),the limit of determination was 0.010 μg/kg by sampling 2 g.The average recov-eries of the 7 indicative PCBs were from 86.1％to 104.1％at three spiked levels of 0.60,10.0 and 18.0µg/L,and the rel-ative standard deviations(RSD,n=6)was from 0.30％to 5.59％.Conclusion The method is simple,accurate,reliable,and suitable for the determination of 7 indicative PCBs in fish and shellfish samples.
Indicative polychlorinated biphenylsGas chromatography-triple quadrupole mass spectrometryIsotope in-ternal standard methodFish and shellfish
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