超高效液相色谱-串联质谱同位素内标法检测蜂蜜中诺氟沙星残留量的不确定度评定

Uncertainty evaluation for determination of norfloxacin residue in honey by ultra performance liquid chromatography-tandem mass spectrometry isotope internal standard method

中文关键词:  诺氟沙星  超高效液相色谱串联质谱法  蜂蜜  同位素内标法  不确定度

英文关键词:norfloxacin  ultra performance liquid chromatography-tandem mass spectrometry  honey  isotope internal standards method  uncertainty

中文摘要:

      目的 评定超高效液相色谱-串联质谱法测定蜂蜜中诺氟沙星残留量的不确定度。方法 以GB/T 23412-2009《蜂蜜中19种喹诺酮类药物残留量的测定方法》为基础, 结合CNAS-GL006《化学分析中的不确定度评估指南》, 建立数学模型, 分析不确定度来源并计算各不确定度分量得到合成标准不确定度。结果 当样品中诺氟沙星含量为5.438 μg/kg时, 得到扩展不确定度为0.915 μg/kg (k＝2)。故试样中诺氟沙星含量结果报告可表示为: (5.438±0.915) μg/kg (k＝2)。结论 标准物质及稀释过程、仪器校准对不确定度影响较大

英文摘要:

      Objective To evaluate the uncertainty for determination of norfloxacin residue in honey by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) isotope internal standard method. Methods Based on GB/T 23412-2009 Determination of residues of 19 quinlones in honey, and according to CNAS-GL006 Guidance on evaluating the uncertainty in chemical analysis, a mathematical model was established, then the sources of uncertainty were analyzed and the uncertainty components was calculated to obtain the synthetic standard uncertainty. Results When norfloxacin residue in honey was 5.438 μg/kg, the expanded uncertainty was 0.915 μg/kg (k＝2). The measurement results of norfloxacin in sample was (5.438±0.915) μg/kg (k＝2). Conclusion The major sources of uncertainty of measurement are the calibration of UPLC-MS/MS, the preparation of standards and dilution processes.