液相色谱-气压光电电离源质谱法同时测定电子电气产品中16种多环芳烃残留

Simultaneous Quantitative Determination of 16 Polycyclic Aromatic Hydrocarbons (PAHs) by HPLC-APPI-MS/MS

  • 摘要: 采用HPLC-APPI-MS/MS法同时测定电子电器产品中橡胶,塑料等材料中的16种多环芳烃(PAHs)残留量。样品经粉碎后,用甲醇提取,通过C18小柱过柱净化,以液相色谱分离,大气压光电电离源离子化电离串联质谱进行检测,采用多反应监测模式同时测定16种多环芳烃浓度。该方法定量下限(LOQ,S/N>10)为0.1~0.2 μg•g-1,回收率为72.0%~89.6%,变异系数小于10%。在0.1~10.0 μg•L-1浓度范围内,峰面积与浓度呈良好线性(r: 0.993 2~0.999 2)。

     

    Abstract: An HPLC-APPI(+)MS-MS method was developed by solid phase extraction decontamination for the residue determination of PAHs. The sample was extracted by the methyl alcohol after comminution and operating for decontamination by C18 cartridges. Samples were detected by a gradient elution flowing with a APPI positive mode detector at MRM(naphthalene m/z 128, acenaphthylene m/z 152, acenaphthene m/z 154, fluorene m/z 166, phenanthrene m/z 178, anthracene m/z 178, fluoranthene m/z 202, pyrene m/z 202, benz(a)anthracene m/z 228, chrysene m/z 228, benzo(b)fluoranthene m/z 252, benzo(k)fluoranthene m/z 252, benzo(a)pyrene m/z 252, benzo(g,h,I)perylene m/z 276, indeno(1,2,3,c,d)pyrene m/z 276, dibenz(a,h)anthracene m/z 278). The LOQs (S/N>10)of 16 PAHs residues in the negative meat sample are 0.10.2 mg•kg-1. The recovery values is 72.0%-89.6%. The response for 16 PAHS is linear in the range of 0.1-10.0 μg•L-1, and the correlation coefficient is excellent(r: 0.993 2-0.999 2).

     

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