中国农业科技导报 ›› 2018, Vol. 20 ›› Issue (10): 131-137.DOI: 10.13304/j.nykjdb.2017.0592

• 方法与技术创新 • 上一篇    下一篇

QuEChERS-HPLC-MS/MS测定猪肉猪肝中苯乙醇胺A

刘艳1,汪建明1*,王敏2,周剑2,闻路红3*,赵鹏3   

  1. 1.天津科技大学食品工程与生物技术学院, 天津 300457; 2.中国农业科学院农业质量标准与检测技术研究所, 农业部农产品质量安全重点实验室, 北京 100081; 3.广州市华粤行仪器有限公司, 广州 511400
  • 收稿日期:2017-09-06 出版日期:2018-10-15 发布日期:2017-11-02
  • 通讯作者: *通信作者:汪建明,教授,博士生导师,主要从事动植物的生物蛋白及应用研究。E-mail: wjm-1115@126.com;闻路红,教授级高级工程师,主要从事食品安全应用研究。E-mail: wenluhong@cii-tech.com
  • 作者简介:刘艳,硕士研究生,研究方向为动物资源开发与功能食品研究,E-mail:liuyan9ly@163.com。
  • 基金资助:
    广州市番禹区创新领军团队项目(2017-R01-5);中国农业科学院科技创新工程项目资助。

Determination of Phenylethanolamine A in Pork and Pork Liver Using QuEChERS-HPLC-MS/MS

LIU Yan1, WANG Jianming1*, WANG Min2, ZHOU Jian2, WEN Luhong3*, ZHAO Peng3   

  1. 1.Institute of Food Engineering and Biotechnology, Tianjin University of Science and Technology, Tianjin 300457; 2.Key Laboratory of Agri-food Safety and Quality, Ministry of Agriculture and Rural Affairs; Institute of Quality Standard and Testing Technology, Chinese Academy of Agricultural Sciences, Beijing 100081; 3.Hua Yue Enterprise Holdings Ltd., Guangzhou 511400, China
  • Received:2017-09-06 Online:2018-10-15 Published:2017-11-02

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

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