超高效液相色谱-串联质谱法测定动物源性食品中硝基咪唑类药物及其代谢物的残留量的研究

Determination of nitroimidazoles and their metabolites residues in foodstuffs of animal origin 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  硝基咪唑药物及其代谢物  动物源性食品

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  nitroimidazoles and their metabolites  foodstuffs of animal origin

中文摘要:

      目的 建立超高效液相色谱-串联质谱法测定动物源性食品中硝基咪唑类药物及其代谢物的分析方法。方法 试样经三氯乙酸溶液提取, MCX固相萃取小柱净化, 5%的甲醇水(V/V)溶液复溶。电喷雾正离子模式电离, 多反应监测模式检测, 基质匹配内标法定量。结果 硝基咪唑及其代谢物在0.25~50 ng/mL范围内线性关系良好, 相关系数均大于0.9915, 加标回收率为73.5%~120.4%; 相对标准偏差在2.4%~13.4%之间, 定量限为0.1~0.5 μg/kg。结论 本方法简便、灵敏, 适用于动物源性食品中硝基咪唑类药物及其代谢物残留的定性、定量分析。

英文摘要:

      Objective To establish a method for the determination of nitroimidazoles and their metabolites in animal foods by ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with trichloroacetic acid solution, cleaned with MCX column, and then reconstituted with 5% methanol aqueous solution (V/V). The samples were determination by mass spectrometry with electrospray ion source in the positive mode, monitored by the multiple reaction monitoring (MRM) mode, and then quantified by the matrix matching of internal standard calibration. Results The linear relationship of nitroimidazole and its metabolites was good in the range of 0.25?50 ng/mL, the correlation coefficient was greater than 0.9915, and the standard recovery was 73.5%?120.4%. The RSD ranged from 2.4% to 13.4% and the quantitative limit was 0.1 to 0.5 μg/kg. Conclusion This method is simple and sensitive, and can be applied to qualitative and quantitative analysis of nitroimidazoles and their metabolites residues in foodstuffs of animal origin.