该研究利用超高效液相色谱-四极杆-静电场轨道离子阱高分辨质谱技术，对12种氯化烟碱类药物及其代谢产物色谱信息、分子离子质荷比和二级碎裂片段的质荷比进行采集，解析了碎裂途径，建立了氯化烟碱类药物及其代谢产物标准数据库，筛选特征碎裂片段；采用数据非依赖扫描模式，获取可追溯的样品质谱信息，构建了乳制品中氯化烟碱类药物及其代谢产物的非定向筛查方法。该方法确定限和检测容量分别为0.01 μg/kg~0.33 μg/kg与0.03 μg/kg~0.59 μg/kg，回收率为84%~104%，其相对标准偏差为4.4%~7.1%。将所建立的方法用于81个批次巴氏杀菌乳中氯化烟碱类药物及其代谢产物的筛查工作当中，发现样品中含有未检出的啶虫脒-代谢物-IM-1-4，含量为0.32 μg/kg。结果显示该方法快速、简便，可实现乳制品中氯化烟碱类药物及其代谢产物准确定性和精准定量。

In this study, UHPLC quadrupole-orbitrap mass spectrometry was used to collect the chromatographic information, mass charge ratio of molecular ions and mass charge ratio of secondary fragmentation fragments of 12 kinds of chloronicotinoids and their metabolites, the fragmentation pathway was analyzed, the standard database of chloronicotinoids and their metabolites were established, and characteristic fragments were screened; The independent data scanning mode was used to obtain the traceable mass spectrum information of samples, and a non targeted screening method for chloronicotinoids and their metabolites in dairy products was established. The determination limit and the detection capacity of this method were in range of 0.01 μg/kg~0.33 μg/kg and 0.03 μg/kg~0.59 μg/kg, respectively. The recoveries were 84%~104%, and the relative standard deviations were 4.4%~7.1%. The established method was applied to the screening of chloronicotinoids and their metabolites in 81 batches of pasteurized milk. It was found that the samples contained acetamiprid-metabolite-IM-1-4, which was not detected, and the content was 0.32 μg/kg. The results showed that the method was rapid and simple, and could realize the accurate qualitative and quantitative analysis of chloronicotinoids and their metabolites in dairy products.

国家市场监督管理总局科技计划项目（2019MK070）