QuEChERS-HPLC-MS/MS测定猪肉猪肝中苯乙醇胺A

Determination of Phenylethanolamine A in Pork and Pork Liver Using Qu ECh ERS-HPLC-MS/MS

建立了猪肉、猪肝中苯乙醇胺A的Qu ECh ERS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,1.7μm),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0.1~40μg/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0.1μg/kg,检出限为0.05μg/kg。

In this paper,a method of Qu ECh ERS 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.