高效液相色谱-串联质谱法测定鱼粉中诺氟沙星、环丙沙星和恩诺沙星残留量的不确定度评估

Uncertainty evaluation for the determination of norfloxacin, ciprofloxacin and enrofloxacin in fish meal by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  鱼粉  诺氟沙星  环丙沙星  恩诺沙星  不确定度

英文关键词:high performance liquid chromatography-tandem mass spectrometry  fish meal  norfloxacin  ciprofloxacin  enrofloxacin  uncertainty

中文摘要:

      目的 评定高效液相色谱-串联质谱法测定鱼粉中诺氟沙星、环丙沙星和恩诺沙星药物残留量的不确定度。方法 依据GB/T 21312—2007《动物源性食品中14种喹诺酮药物残留检测方法 液相色谱-质谱/质谱法》, 建立数学模型, 计算各来源对其检测的不确定度影响, 从而得出合成不确定度和扩展不确定度。结果 当鱼粉中诺氟沙星、环丙沙星和恩诺沙星残留量为341.91、28.06、27.25 μg/kg时, 其扩展不确定度分别为38.84、5.03、3.42 μg/kg(P=95%, k=2)。结论 影响检测结果的不确定度主要来源于标准曲线拟合、标准溶液配制和样品回收率。

英文摘要:

      Objective To evaluate the uncertainty of norfloxacin, ciprofloxacin and enrofloxacin in fish meal by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods According to GB/T 21312—2007 Analysis of fourteen quinolones in food of animal origin-High performance liquid chromatography-tandem mass spectrometry method, by establishing a mathematical model, the sources of uncertainty were analyzed and the effects of different sources were measured and calculated. Results When the residues of norfloxacin, ciprofloxacin and enrofloxacin in fish meal were 341.91, 28.06 and 27.25 μg/kg, the expanded uncertainties were 38.84, 5.03 and 3.42 μg/kg, respectively (P=95%, k=2). Conclusion The uncertainties of the experiments are mainly derived form the calibration curve fitting, standard solution preparation process and the recovery rate.