超高效液相色谱-四极杆串联飞行时间高分辨质谱法筛查和确证猪肉中117种兽药残留

Screening and confirmation of 117 kinds of veterinary drugs residues in pork by ultra performance liquid chromatography-quadrupole tandem time-of-flight mass spectrometry

中文关键词:  超高效液相色谱-四极杆串联飞行时间高分辨质谱法  兽药  筛查  确证  猪肉

英文关键词:ultra performance liquid chromatography-quadrupole tandem time-of-flight mass spectrometry  veterinary drugs  screening  confirmation  pork

中文摘要:

      目的 建立应用超高效液相色谱-四极杆串联飞行时间高分辨质谱对猪肉中多种类兽药残留进行筛查和确证的定性分析方法。方法 均匀分散的样品经提取、净化后, 通过Acquity HSS T3超高效液相色谱柱 (2.1 mm×100 mm, 1.8 μm)分离, 经流动相梯度洗脱后进入高分辨质谱仪检测。在正离子模式下, 通过高分辨质谱一级全扫描对样品进行分析, 与数据库中目标化合物的精确质量数、保留时间进行匹配。对疑似阳性样品进一步通过二级碎片离子扫描进行确证。结果 建立的分析方法对目标化合物选择性良好, 检出限在1~ 80 μg/kg, 满足对快速筛查分析的方法学要求。结论 该方法简单、灵敏、分析速度快, 适用于猪肉中117种兽药化合物的筛查和确证。

英文摘要:

      Objective To establish a qualitative analysis method for screening and confirming multiple veterinary drug residues in pork by ultra performance liquid chromatography-quadrupole tandem time-of-flight mass spectrometry. Methods The uniformly dispersed samples were extracted and purified, and then separated by an Acquity HSS T3 ultra performance liquid chromatography column (2.1 mm×100 mm, 1.8 μm). The mobile phase was eluted by gradient. In positive ion mode, the samples were analyzed by full scan of high resolution mass spectrometry. Retention time and exact mass measurements of target compounds in samples were compared with those in database. Suspected positive samples were further confirmed by product ion scanning. Results The established analytical method had good selectivity for the target compounds and the detection limits were in the range of 1-80 μg/kg, meeting the methodological requirements for rapid screening analysis. Conclusion This method is simple, sensitive and rapid, and is suitable for screening and confirming 117 veterinary drug compounds in pork.