超高效液相色谱-串联质谱法测定畜禽肉中17种磺胺类药物残留

Determination of 17 kinds of sulfonamide residues in livestock and poultry meat by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  磺胺类  超高效液相色谱-串联质谱法  畜禽肉

英文关键词:sulfonamide  ultra performance liquid chromatography-tandem mass spectrometry  livestock and poultry meat

中文摘要:

      目的 建立超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定畜禽肉组织中17种磺胺类药物残留的方法。方法 样品经乙腈提取、浓缩, 正己烷脱脂后在正离子模式下以电喷雾电离串联质谱进行测定, 外标法定量。结果 17 种磺胺类药物在 5 μg/L~100 μg/L范围内线性良好, 相关系数＞0.99, 方法检出限为2 μg/kg, 定量限为5 μg/kg。在10、20、 100 μg/kg的添加水平下, 17种磺胺类药物的平均回收率在84.0%~114.2%之间, 相对标准偏差(relative standard deviation, RSD, n=6)在0.59%~7.96%之间。结论 本方法快速、准确、灵敏, 可应用于畜禽肉中17种磺胺类药物残留的同时检测。

英文摘要:

      Objective To establish an analytical method for determination of 17 kinds of sulfonamide residues in livestock and poultry meat by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted and enriched by acetonitrile and determined by multiple reaction monitoring (MRM) mode with electrospray ionization source, then quantified by external standard method. Results All of the analytes showed good linearity in the range of 5 μg/L~100 μg/kg and the correlation coefficients (r2) were all above 0.99. The limits of detection (LODs) for the derivatized sulfonamide residues were 2 μg/kg and the limits of quantification (LOQs) were 5 μg/kg. The average recoveries for the blank samples at 3 spiked levels (10, 20, 100 μg/kg) ranged from 84.0% to 114.2%, with the relative standard deviations (RSDs, n=6) of 0.59%~7.96%. Conclusion The proposed method is rapid, accurate and sensitive, which is suitable for simultaneous detecting of 17 kinds of sulfonamide residues in livestock.