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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0.009~0.047μg/kg,在猪肝样品中的检出限(LOD,S/N=3)为0.003~0.031μg/kg;在0.5μg/kg、1.0μg/kg、1.5μg/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。
Objective To establish a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method for the determination of 17 perflurorinated alkylated substances (PFASs) in pork and pork liver. Methods The samples were extracted with acidified acetonitrile and purified by mixed adsorbents. The samples were analyzed by HPLC-MS / MS. Poroshell 120 EC-C18 column and methanol-5 mmol / L ammonium acetate aqueous solution were used for gradient elution. Scanning, isotope internal standard method, the internal standard for the 13C or 18O labeled corresponding external standard. Results The detection limit (LOD, S / N = 3) of the 17 perfluoroalkyl compounds in pork samples was 0.009 ~ 0.047 μg / kg, The average spike recoveries of this method ranged from 80% to 110% at three spiked concentrations of 0.5μg / kg, 1.0μg / kg and 1.5μg / kg, Mean relative standard deviation (RSD) was less than 10%. Conclusion The method can be effectively applied to the detection of 17 perfluoroalkyl compounds in pork and liver.