固相萃取净化-超高效液相色谱-串联质谱法测定动物肌肉组织中46种抗生素残留

Determination of 46 kinds of antibiotic residues in animal muscle tissues by solid-phase extraction purification-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  喹诺酮  磺胺  硝基咪唑  超高效液相色谱-串联质谱  肌肉组织

英文关键词:quinolones  sulfonamides  nitroimidazole  ultra performance liquid chromatography-tandem mass spectrometry  solid-phase extraction purification  muscle tissues

中文摘要:

      目的 建立超高效液相色谱-串联质谱法同时测定动物肌肉组织中22种磺胺类、15种喹诺酮类、9种硝基咪唑类, 共46种抗生素残留检测方法。方法 样品经90%乙腈水溶液提取, 通过PRiME HLB固相萃取柱净化, 经氮吹浓缩并转换溶剂, 采用超高效液相色谱-串联质谱仪进行测定。使用0.1%甲酸水-乙腈为流动相进行梯度洗脱, 采用多反应监测模式进行检测, 外标法定量。结果 46种抗生素在各自浓度范围内线性关系好, 定量限为1~5 μg/kg, 平均回收率为60.2%~106.8%, 相对标准偏差为0.2%~12.2%。结论 该方法具有检测效率高、通量高等特点, 能满足动物肌肉组织中磺胺类、喹诺酮类、硝基咪唑类药物快速筛查需求。

英文摘要:

      Objective To establish a method for the simultaneous determination of 46 kinds of antibiotic residues including 22 kinds of sulfonamides, 15 kinds of quinolones, 9 kinds of nitroimidazoles in animal muscle tissues by ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted by 90% acetonitrile aqueous solution, purified by PRiME HLB solid-phase extraction column, concentrated by nitrogen blowing and converted to solvent, and determined by ultra performance liquid chromatography-tandem mass spectrometry. The mobile phase consisted of 0.1% formic acid in water and acetonitrile, with gradient elution. Detection was performed in multiple reaction monitoring mode, and quantification was carried out using the external standard method. Results The 46 kinds of antibiotics showed good linear relations within their respective concentration ranges, with limits of quantitation ranging from 1-5 μg/kg. The average recovery rates were 60.2% to 106.8%, and the relative standard deviations were 0.2% to 12.2%. Conclusion This method features high detection efficiency and high throughput, and can meet the rapid screening requirements of sulfonamides, quinolones and nitroimidazoles in animal muscle tissues.