摘要
建立同时测定猪肉中萘啶酸、恶喹酸、依诺沙星、氟甲喹、诺氟沙星、环丙沙星、洛美沙星、丹诺沙星、恩诺沙星、氧氟沙星、沙拉沙星、二氟沙星、麻保沙星、培氟沙星、司帕沙星、奥比沙星16种喹诺酮类药物残留的超高效液相-串联质谱(ultra performance liquid chromatography-tandem mass spectrophy,UPLC-MS/MS)的检测方法。样品采用乙酸-乙腈(1∶99,V/V)一次性振荡提取,用弱阴离子固相萃取柱净化,内标法定量。结果表明:16种喹诺酮药物的检出限为0.2μg/kg,定量限为0.8μg/kg,空白猪肉中添加2.0、5.0、10.0μg/kg水平,16种喹诺酮的回收率在70%~120%。该方法分析速度快、样品前处理干净、杂质污染少,可用于猪肉样品中喹诺酮类的残留检测。
An efficient ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method was established for the analysis of residues of 16 quinolones(danofloxacin, difloxacin, lomefloxacin, pefloxacin, enoxacin, orbifloxacin, marbofloxacin, sparfloxacin, oxolinic acid, nalidixic acid, ofloxacin, norfloxacin, flumequine, enrofloxacin, sarafloxacin, and ciprofloxacin) in pork. Samples were extracted with 1% acetic acid-acetonitrile, and the extract was subjected to chromatographic separation on a weak anion solid-phase extraction column. Quantification of 16 quinolones was achieved by UPLC-MS/MS using internal standard method. The detection limit and quantification limit of the method were 0.2 μg/kg and 0.8 μg/kg respectively for all 16 quinolones. The average recoveries of 16 quinolones in blank pork at three spiked levels of 2.0, 5.0 and 10.0 μg/kg ranged from 70% to 120%, with relative standard deviation(RSD) less than 6%. The method had the advantages of fast analysis, clean sample pretreatment and less pollution. Therefore, it can be used for the detection of quinolone residues in pork.
出处
《肉类研究》
北大核心
2016年第5期36-41,共6页
Meat Research
关键词
喹诺酮
超高效液相色谱-串联质谱
猪肉
残留
quinolones
ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
pork
residue