高效液相色谱-四极杆-飞行时间质谱法检测猪肉中22种磺胺类兽药残留

Determination of 22 sulfonamides in pork by high performance liquid chro-matography-Q-time of flight mass spectrometry

中文关键词:  高效液相色谱法  飞行时间质谱法  磺胺  猪肉

英文关键词:high performance liquid chromatography  time of flight mass spectrometry  sulfonamides  pork

中文摘要:

      目的 建立猪肉中22种磺胺类兽药残留的定性定量分析方法。方法 采用固相萃取技术处理样品, 通过高效液相色谱-四极杆-飞行时间质谱法对猪肉中的22种磺胺类药物进行分离和检测, 并对其进行方法学验证, 考察方法检测限、精密度、回收率等指标。建立磺胺类药物的精确相对分子质量数据库, 并通过碎片离子的精确质量数推测碎片结构。结果 在最低定量限到150 μg/kg范围内, 标准曲线相关性良好(r≥0.99), 所测定的22种化合物检测限为0.1~5 μg/kg, 化合物回收率在81.1%~118.0%之间, 精密度在1.9%~13.6%(n=5)之间。建立了磺胺类共22种化合物的精确相对分子质量数据库。结论 建立的方法准确、快速、灵敏度高, 结合精确相对分子质量数据库, 可应用于实际案例中磺胺类兽药残留的快速分析。

英文摘要:

      Objective To establish a novel analytical method for the analysis on 22 sulfonamides (SAs) in pork by using high performance liquid chromatography-Q-time of fight mass spectrometry （HPLC-Q-TOF MS）. Methods The analytes were extracted from the samples using acetonitrile. After separeted on C18 SPE column, samples were analyzed by HPLC-Q-TOF MS using an electrospray interface in positive ionisation mode. An accurate mass database was established for 22 SAs, and the structures of product ions were inferred by their accurate masses. Results The regression coefficients (r) for the calibration curves (LOQ~150 μg/kg) were ≥ 0.99, the LODs for 22 validated compounds were ranged from 0.1~5 μg/kg, and the recoveries were in the range of 81.1%~118.0%, and the relative standard deviations (RSD) were ranged from 1.9% to 13.6% (n=5). Conclusion The results indicated that this method is simple, rapid, sensitive and suitable for the determination of sulfonamides in pork.