Abstract: In this paper, a method of QuEChERS combining with high effective liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was established for testing phenylethanolamine A in pork and pork liver. Homogenized samples were extracted with acetonitrile, and then the supernatant fliud was defatted with n-hexane, anhydrous sodium sulfate was added to water. When N-propyl ethylenediamine (PSA) adsorbent was dispersive and solid-phase extraction purified, qualitative and quantitative analyses were conducted by HPLC-MS/MS. Taking ACQUITY UPLC BEH C18 (50 mm×2.1 mm,1.7 μm) chromatographic column and methanol-0.1% (v/v) formic acid aqueous solution as mobile phase, a gradient elution was carried out. The analytes were detected by tandem mass spectrometry under multiple reaction monitoring (MRM) mode with positive electrospray ionization (ESI+) and quantified by phenylethanolamine A-D3 as an internal label of isotope. The results showed that when phenylethanolamine A concentration was ranged between 0.1~40 μg/kg, the matrix matching standard curve linearity of pork and pork liver was good, quantitative limit was 0.1 μg/kg, and detection limit was 0.05 μg/kg.

Key words: QuEChERS, β-adrenergic agonists, phenylethanolamine A, isotope internal standard, pork, pork liver

摘要： 建立了猪肉、猪肝中苯乙醇胺A的QuEChERS结合高效液相色谱-串联质谱的检测方法。匀浆后的样品用乙腈提取后，上清液用正己烷除脂，加入无水硫酸钠除水，N-丙基乙二胺（PSA）吸附剂分散固相萃取净化后，以高效液相色谱-串联质谱（HPLC-MS/MS）进行定性和定量分析。采用ACQUITY UPLC BEH C18色谱柱(50 mm×2.1 mm,1.7 μm)，以甲醇-0.1%(v/v) 甲酸水溶液为流动相进行梯度洗脱，串联质谱在多反应监测（MRM）正离子(ESI+)模式下进行检测，以苯乙醇胺A-D3为同位素内标进行定量。结果表明，苯乙醇胺A在0.1～40 μg/kg的浓度范围内，猪肉、猪肝的基质匹配标准曲线线性关系良好，定量限为0.1 μg/kg，检出限为0.05 μg/kg。

关键词: QuEChERS, β-兴奋剂, 苯乙醇胺A, 同位素内标, 猪肉, 猪肝