液相色谱-串联质谱法测定蜂蜜中8种大环内酯类药物残留的不确定度评定

Uncertainty evaluation for determination of 8 kinds of macrolide residues in honey by liquid chromatography-tandem mass spectrometry

中文关键词:  不确定度  大环内酯类药物  液相色谱-串联质谱法  蜂蜜

英文关键词:uncertainty  macrolide  liquid chromatography-tandem mass spectrometry  honey

中文摘要:

      目的 对液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)测定蜂蜜中8种大环内酯类药物残留的测量不确定度进行评定。方法 根据JJF1059.1-2012《测量不确定度评定与表示》, 对LC-MS/MS法测定蜂蜜中大环内酯类药物残留的测量不确定度进行评定, 建立数学模型, 确定不确定度的来源和大小, 最终进行合成和扩展。结果 本方法中测量不确定度的主要来源为校准曲线拟合、仪器的定量校准和回收率的精密度。当包含因子k=2时, 螺旋霉素、替米考星、竹桃霉素、红霉素、泰乐菌素、吉他霉素、交沙霉素、罗红霉素的测定结果分别为: (9.02±0.81)、(9.26±0.63)、(9.79±0.68)、(9.47±0.59)、(9.75±0.82)、(9.16±0.70)、(9.59±0.60)、(9.84±0.68) μg/kg。结论 本方法可为评定食品源中大环内酯类药物残留量的测定结果和方法的可靠性提供科学依据; 在实际检测过程中, 痕量残留分析要得到精确、可靠的测量结果, 需要有良好的仪器维护、完善的样品前处理过程和实验人员的精准操作。

英文摘要:

      Objective To evaluate the measurement uncertainty for determination of macrolide residues in honey by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods According to JJF1059.1-2012 Evaluation and expression of uncertainty in measurement, the measurement uncertainty for determination of macrolide residues in honey by LC-MS/MS was evaluated, mathematical model was established, and sources and sizes of uncertainty were also analyzed. Finally, the synthetic and expanded uncertainties were calculated. Results The major sources of uncertainty were calibration curves fitting, quantitative calibration of instrument and precision of recovery. When including factor was k=2, determination results of spiramycin, tilmicosin, oleandomycin, erythromycin, tylosin, kitasamycin, josamycin and roxithromycin were (9.02±0.81), (9.26±0.63), (9.79±0.68), (9.47±0.59), (9.75±0.82), (9.16±0.70), (9.59±0.60), (9.84±0.68) μg/kg, respectively. Conclusion The established method can provide scientific basis for evaluation of the reliability of the measurement methods and results of macrolide residues in food. In order to get accurate and reliable measurement results, it is necessary for trace residual analysis to have good equipment maintenance, perfect sample pretreatment process and personnel’s precise operation in the process of the actual detection.