液相色谱-串联质谱法检测饲料中洛美沙星、培氟沙星、氧氟沙星、诺氟沙星残留

Determination of lomefloxacin, pefloxacin, ofloxacin and norfloxacin residues in feed by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  喹诺酮类  液相色谱-串联质谱法  饲料

英文关键词:quinolones  liquid chromatography-tandem mass spectrometry  feed

中文摘要:

      目的 建立一种可同时检测饲料中4种氟喹诺酮类药物残留的液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry, LC-MS/MS)检测分析方法。方法 试样用磷酸盐缓冲液和乙腈混合进行提取, MCX固相萃取柱净化, 以甲醇-0.1%甲酸水溶液为流动相, LC-MS/MS法检测, 同时定性、定量测定4种氟喹诺酮类抗生素残留。结果 4种氟喹诺酮类抗生素在Hypersil GOLD C18色谱柱上分离效果较好, 添加的回收率在60.3%~91.0%之间, 相对标准偏差在0.87%~5.91%之间(n=6), 方法的检测限为2 μg/kg, 定量限为5 μg/kg。结论 该方法准确、简便、快速, 能满足兽药残留分析的要求, 适合测定饲料中4种氟喹诺酮类抗生素残留。

英文摘要:

      Objective To establish a method for simultaneous determination of 4 fluoroquinolones residues in feed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods The samples were extracted by mixing phosphate buffer and acetonitrile, purified by MCX solid phase extraction column, and detected by LC-MS/MS with methanol-0.1% formic acid solution as mobile phase. Four fluoroquinolone antibiotic residues were determined qualitatively and quantitatively at the same time. Results Four kinds of fluoroquinolones had good separation effects in Hypersil GOLD C18 column. The recoveries were 60.3%-91.0%, with the relative standard deviations of 0.87%-5.91% (n=6). The limit of detection of the method was 2 μg/kg and the limit of quantitation was 5 μg/kg. Conclusion The method is accurate, simple and rapid, and can meet the requirements of veterinary drug residue analysis, which is suitable for the determination of four fluoroquinolone antibiotics residues in feed.