超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定动物源性产品中磺酰草吡唑及其代谢物残留量

Determination of pyrasulfotole and its metabolite residues in animal-derived products by ultra performance liquid chromatography-quadrupole/ orbitrap high resolution mass spectrometry

中文关键词:  磺酰草吡唑  代谢物  动物源性产品  超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法

英文关键词:pyrasulfotole  metabolite  animal-derived products  ultra performance liquid chromatography- quadrupole/orbitrap high resolution mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定动物源性产品中磺酰草吡唑及其代谢物残留量的分析检测方法。方法 样品经甲酸-乙腈溶液提取, 提取液先经低温冷冻除脂后, 再采用十八烷基键合硅胶、石墨化碳黑和无水硫酸镁分散固相萃取进行净化, 以Waters Acquity UPLC HSS T3色谱柱为分析柱, 甲醇-0.2%甲酸溶液为流动相进行梯度洗脱分离, 采用高分辨质谱平行反应监测扫描模式, 以正离子采集进行定性定量分析, 基质匹配外标法定量。结果 磺酰草吡唑和磺酰草吡唑-脱甲基在0.5~50.0 μg/L范围内线性关系良好, 相关系数均大于0.995。空白样品在4个加标水平下的平均回收率为82.4%~114.6%, 相对标准偏差(n=6)为3.1%~8.9%; 方法检出限为0.3 μg/kg, 定量限为1.0 μg/kg。结论 该方法操作简单快速、灵敏度高、结果准确, 可应用于动物源性产品中磺酰草吡唑及其代谢物的检测。

英文摘要:

      Objective To establish an analytical method for the determination of pyrasulfotole and its metabolite residue in animal-derived products by ultra performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry. Methods The samples were extracted with formic acid-acetonitrile solution, the extract was degreased by low temperature freezing first, and then cleaned up with stearyl bonded silica gel, graphitized carbon, and anhydrous magnesium sulfate as dispersive solid-phase extraction sorbent. The chromatographic analysis was performed on a Waters Acquity UPLC HSS T3 column with 0.2% formic acid solution and methanol as mobile phase by gradient elution, high resolution mass spectrometry parallel reaction monitoring scanning mode was used for qualitative screening and quantitative analysis by positive ion acquisition and an matrix matching external standard method was used for quantification. Results The calibration curves of pyrasulfotole and its metabolite were linear in the range 0.5?50.0 μg/L respectively, with correlation coefficients greater than 0.995. The average recoveries of blank samples at 4 levels were 82.4%?114.6%, the relative standard deviations (n=6) were 3.1%?8.9%; and the limits of detection were 0.3 μg/kg, the limits of quantitation were 1.0 μg/kg. Conclusion This method is simple, rapid, sensitive and accurate, can be used for rapid detection of pyrasulfotole and its metabolites in animal-derived products.