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 masss pectrometry,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2μg/kg,定量限为5μg/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。
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.
作者
史艳艳
高琳
李俊
何志霞
SHI Yan-Yan;GAO Lin;LI Jun;HE Zhi-Xia(Tianjin Veterinary Drug and Feed Supervision Institute, Tianjin 300402, China;Institute of Feed Research of Chinese Academy of Agricultural Sciences, Beijing 100081, China)
出处
《食品安全质量检测学报》
CAS
2019年第11期3367-3375,共9页
Journal of Food Safety and Quality
关键词
喹诺酮类
液相色谱-串联质谱法
饲料
quinolones
liquid chromatography-tandem mass spectrometry
feed
