高分子印迹固相萃取法测定熏烤肉制品中16 种欧盟优控多环芳烃

Determination of 16 polycyclic aromatic hydrocarbons with European priority in smoked meat by molecularly imprinted solid-phase extraction

中文关键词:  多环芳烃  熏烤肉  高分子印记固相萃取  气相色谱-质谱法

英文关键词:polycyclic aromatic hydrocarbons  smoked meat  molecularly imprinted solid-phase extraction  gas chromatography-mass spectrometry

中文摘要:

      目的 建立高分子印记固相萃取-气相色谱质谱联用(MIPSPE-GC/MS)测定熏烤肉中 16 种欧盟优控多 环芳烃的检测方法。方法 样品经均质、超声波提取、高分子印记固相萃取柱净化后, 采用气相色谱质谱联用 仪在选择离子(SIM)扫描模式下进行测定, 内标法定量。 结果 本方法检出限为 0.07~0.24 μg/kg, 在 1~500 μg/L 范围内目标化合物具有很好的相关性, 相关系数均大于 0.999。日内及日间精密度小于 10%, 在 1、5 μg/kg 两 个加标水平下, 16 种 PAHs 回收率为 66.27 % ~ 111.61%, 相对标准偏差均小于 10%。 结论 本方法灵敏、 快速、 简便, 能满足熏烤肉制品中欧盟多环芳烃的检测要求。

英文摘要:

      Objective To establish a method for the determination of 16 polycyclic aromatic hydrocarbons with European priority in smoked meat by molecularly imprinted solid-phase extraction and gas chromatogra- phy-mass spectrometry (MIPSPE-GC/MS). Methods The homogenized sample was extracted ultrasonically with cyclohexane, cleaned up by molecularly imprinted solid-phase extraction catridge (MIPSPE), analyzed by GC/MS under the positive mode using selected ion scan (SIM). The samples were quantified with internal standard method. Results The detection limits of 16 PAHs were 0.07~0.24 μg/kg, The method showed a good linearity over the range of 1~500 μg/L for 16 polycyclic aromatic hydrocarbons with R≥0.999. The Intra-day precision was less than 10%. The recoveries of spiked samples at the level of 1 μg/kg and 5 μg/kg were in the range of 66.27 % ~ 111.61%, and the relative standard deviations were all less than 10%. Conclusion This method is quick, sensitive and it is suitable for the determination of 16 polycyclic aromatic hydrocarbons with European priority.