乳业科学与技术 ›› 2024, Vol. 47 ›› Issue (2): 0-0.

• 分析检测 •    

QuEChERS-超高效液相色谱-四极杆/静电场轨道阱质谱法测定牛羊奶及乳粉中21种兽药

张申平,秦宇,顾颖娟   

  1. 上海市质量监督检验技术研究院/国家市场监管重点实验室(乳及乳制品检测与监控技术)
  • 收稿日期:2024-04-10 修回日期:2024-06-05 出版日期:2024-03-01 发布日期:2024-06-18
  • 通讯作者: 张申平
  • 基金资助:
    液体乳中兽药及其代谢物残留的高通量快速筛查技术研究

Determination of 21 kinds of Veterinary Drugs in Cow and Goat milk and Milk Powder by QuEChERS with Ultra Performance Liquid Chromatography-Quadrupole/Orbitrap Mass Spectrometry

  • Received:2024-04-10 Revised:2024-06-05 Published:2024-03-01 Online:2024-06-18

摘要: 采用QuEChERS方法处理样品,使用超高效液相色谱-四极杆/静电场轨道阱质谱(Ultra performance liquid chromatography-quadrupole/orbitrap mass spectrometry, UPLC-Q/Orbitrap MS)进行测定,建立牛羊奶及乳粉中21种兽药的分析方法。通过优化色谱条件、质谱参数和前处理条件,确定了最佳测试方法。样品经乙腈盐析超声提取后,采用N-丙基乙二胺(PSA)和C18净化,经Accucore RP-MS色谱柱(100 mm×2.1 mm,2.7 μm)分离,UPLC-Q/Orbitrap MS测定。结果显示,21种兽药在各自线性范围内具有良好的线性关系,相关系数(r2)均大于0.99;方法定量限(Limits of quantification, LOQ)为0.5 μg/kg;在0.5、2、10 μg/kg加标水平下的平均回收率为67.2%~110.2%,相对标准偏差(Relative standard deviation, RSD)为3.6%~17.4% (n=6)。该方法简便灵敏,适用于牛羊奶及乳粉中21种兽药的同步检测。

关键词: QuEChERS, 静电场轨道阱质谱, 抗虫药, 消炎药, 激素药物

Abstract: A method for the determination of 21 veterinary drugs in cow and goat milk and milk powder was established by QuEChERS combined with ultra performance liquid chromatography-quadrupole/orbitrap mass spectrometry (UPLC-Q/Orbitrap MS). The optimum test method was determined by optimizing chromatographic conditions, mass spectrometry parameters and pre-treatment conditions. The samples were extracted by acetonitrile salt-out under ultrasonication, and then purified by n-propyl ethylenediamine(PSA) and C18. The target analytes were separated by Accucore RP-MS column (100 mm×2.1 mm, 2.7 μm), and determined by UPLC-Q/Orbitrap MS. 21 kinds of veterinary drugs showed good linear relationship in their linear range, and the correlation coefficient (r2) was greater than 0.99. The Limits of quantification (LOQ) were 0.5 μg/kg. The average recoveries at 0.5, 2 and 10 μg/kg were 67.2%-110.2%, and the relative standard deviation (RSD) was 3.6%-17.4% (n=6). The method is simple and sensitive, and suitable for simultaneous detection of 21 kinds of veterinary drugs in cow and goat milk and milk powder.

Key words: QuEChERS, Orbitrap mass spectrometry, antiparasitics, antiphlogistics, glucocorticoids