超高效液相色谱-串联质谱法同时检测动物源性食品中22种兽药残留

Simultaneous determination of 22 kinds of veterinary drug residues in animal-derived food by ultra performance liquid chromatography- tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  动物源性食品  兽药残留

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  animal-derived food  veterinary drug residues

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定猪肉、牛肉、鸡肉、水产等动物源性食品中6种β2-受体激动剂类、8种磺胺类、氯霉素、氟苯尼考、金刚乙胺、金刚烷胺、孔雀石绿、隐色孔雀石绿、地西泮、地塞米松22种兽药残留量的方法。方法 样品分别用乙腈、2%甲酸乙腈和90%乙腈水(含1%甲酸)提取, 提取液在40 ℃下氮气吹干后用10%乙腈水(含5%甲酸)溶液复溶, 采用C18色谱柱分离, 以电喷雾离子源在正、负离子多反应监测模式下进行测定。结果 22种兽药用2%甲酸乙腈作为提取溶剂时, 回收率均较高; 在0.2~40.0 μg/kg的浓度范围内呈现良好的线性关系, r均大于0.998, 定量限范围为0.2~1.0 μg/kg; 加标水平为1、5、10 μg/kg时, 回收率在62.6%~120.0%之间, 相对标准偏差为1.4%~11.0%。结论 该方法简单、快速、准确、灵敏, 极大地提高了多兽药残留的检测效率, 适用于食品安全突发事件应急处置中多兽药残留的快速分析, 对动物源性食品中药物残留的监控具有很重要的现实意义。

英文摘要:

      Objective To establish a method for the simultaneous determination of 22 kinds of veterinary drug residues, including 6 kinds of β2-agonist residues, 8 kinds of sulfonamides, chloramphenicol, florfenicol, rimantadine, amantadine, malachite green, leucomalachite green, diazepam and dexamethasone in animal-derived foods such as pork, beef, chicken, aquatic products and other animal derived foods by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Samples were extracted with acetonitrile, 2% formic acid acetonitrile and 90% acetonitrile (containing 1% formic acid) and redissolved with 10% acetonitrile (containing 5% formic acid) after nitrogen blowing at 40 ℃. The samples were separated by C18 column and determined by electrospray ion source in positive and negative ion multi-reaction monitoring mode. Results When 2% formic acid acetonitrile was used as solvent for the extraction of 22 kinds of veterinary drugs, the recoveries of all components were high; the linear relationships were good in the range from 0.2 to 40.0 μg/kg, with r>0.998, and the limits of quantification were 0.2?1.0 μg/kg; the recoveries were ranged from 62.6% to 120.0% with the relative standard deviations of 1.4%?11.0% with 3 spiked levels of 1, 5 and 10 μg/kg. Conclusion The proposed method is simple, fast, accurate and sensitive, which greatly improves the detection efficiency of multiple veterinary drug residues. It is suitable for rapid analysis of multiple veterinary drug residues in food safety emergencies, and has important practical significance for monitoring drug residues in animal-derived foods.