CAJ | 학술논문

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。
목적：건립저육、저간중17충전불완기화합물(perflurorinated alkylated substances, PFASs)적고효액상색보-천련질보(HPLC-MS/MS)검측방법。방법양품경산화을정제취、혼합흡부제순화후,응용HPLC-MS/MS기술검측,이Poroshell 120 EC-C18위색보주,갑순-5 mmol/L을산안수용액제도세탈,다반응감측부리자모식소묘,동위소내표법정량,내표물위경13C혹자18O표기적상응외표물。결과응용해방법검측저육양품중17충전불완기화합물적검출한(LOD, S/N=3)위0.009～0.047μg/kg,재저간양품중적검출한(LOD, S/N=3)위0.003～0.031μg/kg；재0.5μg/kg、1.0μg/kg、1.5μg/kg 삼개가표농도하,해방법적평균가표회수솔약위80%~110%,평균상대표준편차(RSD)소우10%。결론해방법가유효응용우저육、저간중17충전불완기화합물적검측。
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 0.009~0.047μg/kg of pork and 0.003~0.031μg/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.