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采用同位素稀释法结合固相萃取净化,建立了海产品中苯并(a)芘残留的气相色谱串联质谱(GC-MS/MS)检测方法。样品经乙腈-丙酮(体积比6∶4)溶液提取,硅胶固相萃取净化,苯并(a)芘用GC-MS/MS测定,同位素D12-苯并芘内标法定量。方法的平均回收率为93%～98%,相对标准偏差为6.2%～12.2%(n=6),定量限为0.2μg/kg。用该方法测定FAPAS烟熏鱼有证标准样品,测定值与标准值一致。
The determination of benzo [a] pyrene in seafood by gas chromatography-tandem mass spectrometry (GC-MS / MS) was established by isotope dilution combined with SPE purification. The samples were extracted with acetonitrile-acetone (6: 4 by volume), purified by silica gel SPE, GC-MS / MS and isotope D12-benzopyrene internal standard. The average recovery of the method was 93% -98% with relative standard deviation of 6.2% -12.2% (n = 6). The limit of quantification was 0.2 μg / kg. This method was used to determine the standard sample of FAPAS smoked fish, the measured value is consistent with the standard value.