›› 2013, Vol. 40 ›› Issue (S1): 50-54.

• 安全检测 • 上一篇    下一篇

QuEChERS-UPLC-MS/MS快速测定生鲜牛乳中的氟喹诺酮类药物残留

曲斌1, 朱志谦1, 陆桂萍1, 蒋天梅1, 耿士伟1, 郭良雪2   

  1. 1. 江苏省畜产品质量检验测试中心, 江苏南京 210036;
    2. 安捷伦科技(中国)有限公司, 上海 200080
  • 收稿日期:2013-05-29 出版日期:2013-09-30 发布日期:2013-11-29
  • 作者简介:曲斌(1979-),男,辽宁人,博士,研究方向:兽药残留分析新技术新方法。

Rapid Determination of Fluoroquinolones Residues in Raw Bovine Milk by UPLC-MS/MS via QuEChERS Pretreatment Method

QU Bin1, ZHU Zhi-qian1, LU Gui-ping1, JIANG Tian-mei1, GENG Shi-wei1, GUO Liang-xue2   

  1. 1. Jiangsu Quality Inspection and Testing Center for Animal Products, Nanjing 210036, China;
    2. Agilent technologies (China) Co., Ltd., Shanghai 200080, China
  • Received:2013-05-29 Online:2013-09-30 Published:2013-11-29

摘要: 本试验建立了生鲜牛乳中8种氟喹诺酮类药物的超高效液相色谱串联质谱的测定方法。生鲜牛乳经QuEChERS萃取剂提取,QuEChERS净化剂净化后,经氮气流吹干浓缩后,以超高效液相色谱串联质谱测定,稳定同位素内标法定量。本方法对氟喹诺酮类药物的测定线性范围为2.0~100 μg/kg。在2.0、10、100 μg/kg低、中、高3个浓度的回收率为80%~120%。批内、批间精密度小于20%。本方法简便、快速、灵敏,适用于生鲜牛乳中氟喹诺酮类药物残留的大批量筛选和定量测定。

关键词: 超高效液相色谱-串联质谱; QuEChERS; 氟喹诺酮; 生鲜牛乳; 残留

Abstract: An UPLC-MS/MS method was developed and established for rapid determination of fluoroquinolones residues in raw bovine milk. The sample was extracted by QuEChERS extraction Kit, and cleaned up by QuEChERS clean-up tube. An aliquot sample of 5 mL was concentrated by nitrogen gas. The analytes were determined by UPLC-MS/MS and quantified by stable isotope internal standard. The results showed good linearity in the ranges of 2.0 to 100 μg/kg for all fluoroquinolones. The method recoveries were between 80% and 120%, and also the precisions were lower than 20%. The method is simple, rapid, and sensitive. It is suitable for screening of fluoroquinolones residues in raw bovine milk and quantitative determination.

Key words: UPLC-MS/MS; QuEChERS; fluoroquinolone; bovine milk; residue

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