超高效液相色谱-串联质谱法测定猪肉中磺胺类药物残留量

Determination of sulfonamides residues in pork 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  磺胺类  残留  猪肉

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  sulfonamides  residue  pork

中文摘要:

      目的 建立检测猪肉中磺胺氯哒嗪、磺胺间甲氧嘧啶、磺胺噻唑、磺胺嘧啶及磺胺吡啶等药物残留的超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)。方法 样品采用乙腈提取后, 浓缩提取物用正己烷脱脂净化, 正离子多反应监测(multiple reaction monitoring, MRM)测定, 外标法定量。结果 磺胺类药物在5~200 μg/L质量浓度范围内线性关系良好, 相关系数R2均大于0.996。5种磺胺的检出限均为5 μg/kg, 在添加量为10.0~150.0 μg/kg时回收率为90%~105%, 相对标准偏差(relative standard deviation, RSD)≤7%。结论 建立的方法精密度、准确度较高, 选择性好, 操作快速、简便, 能对猪肉中的磺胺类残留进行定性和定量分析。

英文摘要:

      Objective To establish a method for rapid detection of 5 sulfonamides, including sulfachloropyridazine, sulfamonomethoxine, sulfathiazole, sulfadiazine and sulfapyridine in pork by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods After the extraction of acetonitrile, the concentrated extract was purified with hexane, and the positive ion multiple reaction monitoring (MRM) was measured and the external standard method was quantified. Results Sulfonamides had good linear relationships within the range of 5~200 g/L, with correlation coefficients more than 0.996. The limits of detection (LODs) were 5 μg/kg, and the recovery rates were 90%~105% with relative standard deviations (RSDs) less than 7% when the spiked amounts were 10.0~150.0 μg/kg. Conclusion The established method is accurate, selective, rapid and simple, which can be used for qualitative and quantitative analysis of sulfonamides residues in pork This method can detect the sulfonamides residues in pork, with a better precision, higher accuracy, better specificity, and the result is satisfied.