双重净化法结合液质联用法快速测定鸡蛋中的磺胺类药物残留

Rapid determination of sulfonamides residues in eggs by dual-cleanup and liquid chromatography-mass spectrometry

中文关键词:  磺胺  鸡蛋  残留  液相色谱-质谱联用

英文关键词:sulfonamides  egg  residue  liquid chromatography-mass spectrometry

中文摘要:

      目的 通过双重净化法建立鸡蛋中磺胺类药物残留的液相色谱-质谱检测法。方法 样品经乙腈提取, 通过式吸附净化和阳离子交换净化, 液相色谱分离, 四极杆-静电场轨道阱质谱定性定量测定, 平行反应监测模式检测, 采用内标法定量。结果 磺胺类药物保留时间分布在3~7 min, 在0.5~20 μg/kg范围内呈现良好的线性关系, 日内、日间精密度均小于20%, 回收率为90%~110%, 定量限为0.5 μg/kg。结论 该方法快速、准确且灵敏度高, 为监测磺胺类药物在鸡蛋中的残留监控提供了快速准确的技术手段。

英文摘要:

      Objective To a establish dual-cleanup method for the determination of sulfonamides residues in egg by liquid chromatography-high resolution mass spectrometry. Methods The samples were extracted by acetonitrile, purified by pass-through cleanup and cation exchange solid phase extraction, separated by liquid chromatography, qualitatively and quantitatively determined by quadrupole-orbitrap mass spectrometry, detected by parallel reaction monitoring mode, and quantified by internal standard method. Results The retention time of sulfonamides ranged from 3 and 7 min, and showed a good linear relationship in the range of 0.5 to 20 μg/kg. The precisions were less than 20% between day and day, the recoveries were 90% to 110%, and the limit of quantitative was 0.5 μg/kg. Conclusion The method is rapid, accurate and sensitive, which provides a rapid and accurate technical means for monitoring the residues of sulfonamides in eggs.