湖北农业科学 ›› 2020, Vol. 59 ›› Issue (21): 144-146.doi: 10.14088/j.cnki.issn0439-8114.2020.21.030

• 检测分析 • 上一篇    下一篇

超高效液相色谱-串联质谱测定牛奶中喹赛多残留

马晓年, 张秀清, 陈俊秀, 欧利华   

  1. 昆明市疾病预防控制中心,昆明 650228
  • 收稿日期:2020-01-03 出版日期:2020-11-10 发布日期:2020-12-21
  • 通讯作者: 陈俊秀,(电子信箱)752110643@qq.com。
  • 作者简介:马晓年(1985-),女,云南临沧人,副主任技师,硕士,主要从事食品检验与分析工作,(电话)13888021164(电子信箱)179267837@qq.com;
  • 基金资助:
    昆明市卫生人才科技人才培养项目[2017-sw(后备)-66; 2019-sw(后备)-50]

Determination of cyadox in milk by UPLC-MS/MS

MA Xiao-nian, ZHANG Xiu-qing, CHEN Jun-xiu, OU Li-hua   

  1. Kunming Center for Disease Control and Prevention,Kunming 650228,China
  • Received:2020-01-03 Online:2020-11-10 Published:2020-12-21

摘要: 采用超高效液相色谱-串联质谱法检测牛奶中喹赛多,样品经乙酸乙酯提取,经PEP固相萃取柱净化、富集,以乙腈/甲醇(3∶11)-0.1%甲酸水为流动相,经岛津Inertsil ODS-3柱(3 μm,2.1 mm×100 mm)色谱柱分离,采用多反应检测正离子模式进行定性及定量分析。结果表明,PEP固相萃取柱具有较好的回收率,喹赛多的检出限为0.01 μg/g,定量限为0.04 μg/g,在0.384、0.960、1.920 μg 3个加标水平下回收率分别为136.0%、116.0%、62.6%。该法灵敏度高、重复性好,可满足牛奶样品中喹赛多残留的测定。

关键词: 喹赛多, 固相萃取小柱, 超高效液相色谱-串联质谱, 牛奶

Abstract: To establish a reliable pretreatment method for cyadox in milk with UPLC-MS/MS. The sample was extracted by ethyl acetate, then the results was analysed after PEP cartridge purification. The objective compounds were separated using Inertsil ODS-3column(3 μm,2.1 mm×100 mm)with acetonitrile/ methanol(3∶11) -water (0.1% formate) as mobile phase and analyzed by mass spectrometry in the positive electrospray ionization under multiple reaction monitoring mode(MRM). The results showed that PEP cartridge had good recovery rate. The detection limit of cyadox was 0.01 μg/g, limit of quantitation was 0.04 μg/g, the average recoveries for spiked levels of 0.384, 0.960,1.920 μg were 136.0%, 116.0%, 62.6%. The method is suitable for the detection of cyadox residual in milk.

Key words: cyadox, solid phase extraction colum, UPLC-MS/MS

中图分类号: