猪肉、猪肝中 17 种全氟烷基化合物的HPLC-MS/MS 测定

Determination of 17 perflurorinated alkylated substances in pork and pork liver by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  全氟烷基化合物  高效液相色谱-串联质谱法  猪肉  猪肝

英文关键词:perflurorinated alkylated substances  high performance liquid chromatography-tandem mass spectrometry  pork  pork liver

中文摘要:

      目的 建立猪肉、猪肝中17种全氟烷基化合物(perflurorinated alkylated substances, PFASs)的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。方法 样品经酸化乙腈提取、混合吸附剂纯化后, 应用HPLC-MS/MS技术检测, 以Poroshell 120 EC-C18为色谱柱, 甲醇-5 mmol/L乙酸铵水溶液梯度洗脱, 多反应监测负离子模式扫描, 同位素内标法定量, 内标物为经13C或者18O标记的相应外标物。结果 应用该方法检测猪肉样品中17种全氟烷基化合物的检出限(LOD, S/N=3) 为0.009～0.047 μg/kg, 在猪肝样品中的检出限(LOD, S/N=3) 为0.003～0.031 μg/kg; 在0.5 μg/kg、1.0 μg/kg、1.5 μg/kg三个加标浓度下, 该方法的平均加标回收率约为80%~110%, 平均相对标准偏差(RSD)小于10%。结论 该方法可有效应用于猪肉、猪肝中17种全氟烷基化合物的检测。

英文摘要:

      Objective To establish the determination of 17 perflurorinated alkylated substances (PFASs) in meat and liver of pork by high-performance liquid chromatography-tandem mass spectrometry (HPLC- MS/MS). Methods Samples were extracted using acidic acetonitrile, and purified by hybrid adsorbent, and detected by HPLC-MS/MS technology. The chromatographic separation was achieved on a Poroshell 120 EC-C18 column, using a mixture of methanol and 5 mmol/L ammonium acetate as gradient elution solvent. The 13C or 18O-labeled PFAS standards were used for quantification of PFASs and analyzed by UPLC-MS/MS ESI(-) under MRM mode with the internal standard method. Results The developed method showed a limit of detection of 0.009～0.047 μg/kg of pork and 0.003～0.031 μg/kg of pork liver. Mean recoveries (3 replicates) for 17 PFASs in a negative sample spiked at the levels of 0.5, 1.0 and 2.0 μg/kg ranged from about 80% to 110 %, with average relative standard derivation (RSDs) less than 10%. Conclusion The proposed method can be used effectively in detection of 17 PFASs in pork and pork liver.