This paper describes a novel method that combines acetic anhydride derivatization with gas chromatography–electron ionization tandem mass spectrometry (GC–EI/MS/MS) for the sensitive and selective determination of piperazine in chicken and pig tissues. Samples were extracted using an accelerated solvent extraction (ASE) apparatus, purified by solid-phase extraction (SPE) and derivatized with acetic anhydride. This optimized method was validated according to the requirements defined by the European Union and the Food and Drug Administration. At the limit of quantification (LOQ) spiked levels of 50.0, 100.0, 500.0, 1000.0 and 2000.0 μg/kg, the average recoveries of piperazine in chicken and pig tissues were 77.46–96.26%, with relative standard deviations (RSDs) of 1.55–6.64%. The intra-day RSDs were 1.39–5.92%, and the inter-day RSDs were 2.24–8.39%. The limits of detection (LODs) and the LOQs were 1.4–1.6 μg/kg and 4.8–5.2 μg/kg, respectively. The decision limits (CC_α) were 102.02–105.17 μg/kg, and the detection capabilities (CC_β) were 104.03–109.09 μg/kg. Finally, the new approach was verified for the quantitative determination of piperazine in 30 commercial chicken and pig tissues from local supermarkets.

本文介绍了一种结合乙酸酐衍生化与气相色谱-电子电离串联质谱（GC-EI / MS / MS）的新方法，用于灵敏和选择性地测定鸡肉和猪组织中的哌嗪。使用加速溶剂萃取（ASE）仪器萃取样品，通过固相萃取（SPE）纯化并用乙酸酐衍生化。根据欧盟和美国食品药品监督管理局（Food and Drug Administration）定义的要求，对该优化方法进行了验证。在定量限（LOQ）加标水平为50.0、100.0、500.0、1000.0和2000.0μg/ kg时，鸡肉和猪组织中哌嗪的平均回收率为77.46–96.26％，相对标准偏差（RSD）为1.55– 6.64％。日内RSD为1.39–5.92％，日间RSD为2.24–8.39％。检出限（LOD）和LOQ分别为1.4–1.6μg/ kg和4.8–5.2μg/ kg。决策限制（抄送_α）为102.02-105.17微克/千克，和检测能力（CC _β）为104.03-109.09微克/千克。最后，验证了该新方法用于定量测定当地超市的30种商品鸡和猪组织中哌嗪的含量。