该研究评定气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)测定花椒中氯菊酯的不确定度。依据GB 23200.113—2018《食品安全国家标准 植物源性食品中208种农药及其代谢物残留量的测定 气相色谱-质谱联用法》对测定过程中可能产生的不确定度进行分析和计算,创建相应的不确定度数学模型,进而合成相对不确定度和扩展不确定度。结果表明,标准工作液配制和标准曲线拟合是GC-MS/MS法测定花椒中氯菊酯不确定度的主要来源,分析仪器和样品前处理过程是不确定度的次要来源。在GC-MS/MS法测定氯菊酯和其他拟除虫菊酯过程中,应规范标准溶液的配制,选取拟合线性高的标准曲线进行校正。
The uncertainty of determination of permethrin in Zanthoxylum bungeanum by gas chromatography-tandem mass spectrometry (GC-MS/MS) was evaluated. According to the national standard GB 23200.113—2018, the possible uncertainty in the determination process was analyzed and calculated, and the corresponding mathematical model of uncertainty was established. Then the relative uncertainty and expanded uncertainty were synthesized. The results showed that the preparation of the standard working solution and standard curve fitting were the main factor of uncertainty in the determination of permethrin in Zanthoxylum bungeanum by GC-MS/MS, while analytical instruments and sample pretreatment were the secondary factor of uncertainty. In the determination of permethrin and other pyrethroids by GC-MS/MS, the preparation of standard solution should be standardized, and the standard curve with high fitting linearity should be selected for correction.
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