高效液相色谱-串联质谱法测定菠菜中5种磺胺抗生素残留的不确定度评定

Uncertainty evaluation of determination of 5 kinds of sulfonamides residues in spinach by high performance liquid chromatography-tandem mass spectrometry

目的评定高效液相色谱-串联质谱法测定菠菜中5种磺胺类抗生素含量的不确定度。方法通过建立数学模型,对高效液相色谱-串联质谱法测定菠菜中5种磺胺类抗生素含量进行不确定度评定,分析不确定度来源及其对测定过程中不确定度的相对贡献,并计算合成不确定度,最终得到菠菜中5种磺胺类抗生素的扩展不确定度。结果当菠菜中5种磺胺含量为3.6~3.7μg/kg时,在95%置信区间下,合成不确定度为0.302~0.443μg/kg,扩展不确定度为0.7~0.9μg/kg (k=2)。结论实验过程的不确定度主要来源于标准溶液配制、质谱仪电喷雾电离源和测量重复性。

Objective To evaluate the uncertainty of determination of 5 kinds of sulfonamides contents in spinach by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). Methods By establishing a mathematical model,the uncertainty of the determination of 5 kinds of sulfonamides contents in spinach was evaluated. The sources of uncertainty and their relative contribution to the uncertainty in the determination process were analyzed,and the synthetic uncertainty was calculated. Finally,the extension uncertainty of 5 kinds of sulfonamides in spinach was obtained. Results When 5 sulfonamides content was 3.6-3.7 μg/kg,the synthetic uncertainties were 0.302-0.443 μg/kg and the extended uncertainties were 0.7-0.9 μg/kg(k=2) under the 95% confidence interval. Conclusion The evaluation results show that the uncertainties of the experiments are mainly derived from standard solution preparation,electrospray ion source of HPLC-MS/MS and measurement repeatability.