QuEChERS结合超高效液相色谱-串联质谱法测定牛肉及其组织中巴喹普林残留

Simultaneous determination of baquiloprim residues in beef and its tissues by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  QuEChERS  巴喹普林  牛肉及其组织

英文关键词:QuEChERS  baquiloprim  beef and its tissues

中文摘要:

      目的 建立一种QuEChERS前处理结合超高效液相色谱-串联质谱法定量检测牛肉及其组织中磺胺类抗菌增效剂巴喹普林残留量的快速分析方法。方法 样品经1%氨水-甲醇（2:8, V:V）超声提取后，使用QuEChERS试剂盒净化，超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)检测，内标法定量分析。结果 在0.5~20.0 ng/mL质量浓度范围内线性关系良好，线性相关系数为0.9996；检出限为1.0~2.0 μg/kg，定量限为3.0~6.0 μg/kg；巴喹普林在7种牛肉组织中均表现为基质减弱效应，在牛肝中基质效应最强，基质效应（matrix effect, ME）为75.45%，在其他基质中基质效应不明显。经同位素内标校正后，巴喹普林在所有基质中的回收率为101%~111%；3个添加水平的平均回收率为89.71%~103.94%，相对标准偏差（relative standard deviation, RSD）为0.95%~6.58% ；QuEChERS在7种基质中的整体回收效率优于C18、MCX、HLB固相萃取柱。结论 该方法灵敏度高、精密度好、准确度高、前处理简便，可以作为牛肉及其组织中巴喹普林残留量的快速检测方法。

英文摘要:

      Objective To establish a QuEChERS-ultra-high performance liquid chromatography tandem mass spectrometry method for the quantitative determination of baquiloprim residues in beef and its tissues. Methods After ultrasonic extraction with 1% ammonia-methanol (2:8, V:V) , the sample was purified using QuEChERS kit, detected by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), which quantified by internal standard method. Results The linear relationship exhibited excellent correlation within the concentration range of 0.5-20.0 ng/mL, with a coefficient of 0.9996. The limits of detection ranged from 1.0 to 2.0 μg/kg, while the limits of quantitation ranged from 3.0 to 6.0 μg/kg. Baquiloprim showed matrix attenuating effect in all the 7 types of beef tissues, and the strongest matrix effect was found in the bovine liver with a matrix effect (ME)of 75.45%, while the matrix effect was not obvious in the other matrices. The recoveries of baquiloprim in all matrices were 101%-111% after isotope internal standard correction; the average recoveries of the 3 spiked levels were 89.71%-103.94% with the relative standard deviations (RSD) of 0.95%-6.58%; and the overall recovery efficiencies of QuEChERS were better than that of the C18, MCX, and HLB solid-phase extraction columns in the 7 matrices. Conclusion This method is sensitive, precise, accurate and easy to use, and can be used as a rapid method for the determination of baquiloprim residues in beef and its tissues.