超高效液相色谱-串联质谱法测定葡萄中多菌灵和嘧菌酯残留量的不确定度分析

Uncertainty evaluation of determination of carbendazim and azoxystrobin residues in grape by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  QuEChERS  超高效液相色谱-串联质谱法  多菌灵  嘧菌酯  不确定度

英文关键词:QuEChERS  ultra performance liquid chromatography-tandem mass spectrometry  carbendazim  azoxystrobin  uncertainty

中文摘要:

      目的 评定超高效液相色谱串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定葡萄中的多菌灵和嘧菌酯的不确定度。方法 样品经QuEChERS方法净化后浓缩, 经ACQUITY BEH C18色谱柱分离, 流动相梯度洗脱, 多反应监测模式检测。根据JJF 1059.1-2012《测量不确定度评定与表示》对不确定来源进行分析, 建立数学模型, 计算各不确定度分量, 合成扩展不确定度。结果 当葡萄中多菌灵、嘧菌酯含量分别为0.356、0.046 mg/kg时, 在95%的置信区间下, 其扩展不确定度分别为±0.033、±0.005 mg/kg(k=2)。结论 本方法主要不确定来源为标准工作溶液配制和样品重复测定(多菌灵); 标准工作溶液配制和标准曲线拟合(嘧菌酯), 其他因素影响较小。

英文摘要:

      Objective To evaluate the uncertainty of determination of carbendazim and azoxystrobin residues in grape by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The grape samples were purified with the method of QuEChERS and concentrated, then separated by an ACQUITY BEH C18 column with mobile phase gradient elution, and detected by multiple-reaction monitoring model. According to JJF 1059.1-2012 Measurement uncertainty evaluation and presentation, the uncertainty sources of the determination were analyzed, the mathematical model was established, the uncertainty components were calculated, and the uncertainty of the synthetic extension was obtained. Results When the contents of carbendazim and azoxystrobin in grape were 0.356 mg/kg and 0.046 mg/kg, the extended uncertainties were ±0.033 mg/kg and ±0.005 mg/kg (k=2) under the 95% confidence interval. Conclusion The main sources of uncertainty in this method are those generated in the preparation of standard solution and the repeated determination (carbendazim), preparation of standard solution and the curve fitting (azoxystrobin), and other factors have little effect.