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通过式固相萃取-高效液相色谱-串联质谱法测定动物源性食品中30种食源性兴奋剂

刘川1,李佳佳1,吴雪莹2,陈燕秋1,石培育1,宋娟1,戴琴1   

  1. 1. 成都市食品检验研究院
    2. 西南大学食品科学学院
  • 收稿日期:2023-04-27 修回日期:2023-10-25 出版日期:2024-02-25 发布日期:2024-03-06
  • 通讯作者: 宋娟 E-mail:songjuan_as@163.com

Simultaneous Determination of 31 Foodborne Stimulant Drug Residues in Animal-derived Foods by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry with with pass-through solid phase extraction

LIU Chuan1, 1, Yan-Qiu CHEN1, 1,   

  • Received:2023-04-27 Revised:2023-10-25 Online:2024-02-25 Published:2024-03-06

摘要: 摘要:针对不同动物源性食品中多种食源性兴奋剂检测基质效应差异较大、干扰较多等问题,本研究建立通过式固相萃取-高效液相色谱-串联质谱法测定动物源性食品中10种蛋白同化剂、8种糖皮质激素和12种利尿剂 等食源性兴奋剂的方法,试样经5%甲酸乙腈提取,通过式固相萃取柱净化,采用液相色谱-质谱/质谱仪测定,同位素内标法定量。30种食源性兴奋剂在各自浓度范围内线性关系良好,平均回收率介于67.5%~114.3%,相对标准偏差介于0.7%~16.1%(n=6)。该方法具有灵敏度高、操作简单、检测通量大、检测效率高等特点,提高了不同复杂基质下的测量准确性,能够满足赛事用动物源性食品中30种食源性兴奋剂的检测需求。

关键词: 关键词:高效液相色谱-串联质谱, 动物源性食品, 蛋白同化剂, 糖皮质激素, 利尿剂

Abstract: Abstract: In order to solve the problems of different matrix effects and interference of foodborne doping testing in different animal-derived foods,a method was established for the determination of ten protein anabolic agents, eight glucocorticoids, and twelve diuretics in animal-derived foods by pass-through solid phase extraction -high performance liquid chromatography-tandem mass spectrometry (SPE-HPLC-MS/MS). The sample was extracted with 5% formic acid in acetonitrile, and the extract was purified by pass-through solid phase extraction before being measured by liquid chromatography-tandem mass spectrometry. The internal standard method was used for quantification. The linear relationship of 30 foodborne stimulants was good within their respective concentration ranges. The average recoveries ranged from 67.5% to 114.3%, and the relative standard deviations were between 0.7% and 16.1% (n = 6). This method has the characteristics of high sensitivity, simple operation, large detection flux and high detection efficiency, improves the measurement accuracy under different complex substrates. It can meet the detection needs of 30 kinds of foodborne stimulants in animal-derived food for sports events.

Key words: Keywords: high performance liquid chromatography-tandem mass spectrometry, animal-derived foods, protein anabolic agent, glucocorticoids, diuretics

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