气相色谱-三重四极杆质谱法测定蔬菜中氟虫腈残留量的不确定度评定

Uncertainty evaluation of determination of fipronil in vegetables by gas chromatography-triple quadrupole mass spectrometry

中文关键词:  气相色谱-三重四极杆质谱法  氟虫腈  不确定度  蔬菜  内标法

英文关键词:gas chromatography-triple quadrupole mass spectrometry  fipronil  uncertainty  vegetables  internal standard method

中文摘要:

      目的 对气相色谱-三重四极杆质谱法测定蔬菜中氟虫腈残留量的方法进行不确定度评估。方法 根据JJF 1059.1-2012《测量不确定度评定与表示》和JJF 1135-2005《化学分析测量不确定度评定》中有关规定, 建立了用内标法测定蔬菜中氟虫腈残留量不确定度评估的数学模型, 对测定中的不确定度来源进行分析和评估。结果 对不确定的分量进行量化和合成, 结果表明, 当蔬菜中氟虫腈残留量为0.02 mg/kg时, 扩展不确定度为0.0096 mg/kg, 氟虫腈残留量表示为(0.02±0.0096) mg/kg (k=2)。结论 实验过程中的不确定度主要来源于标准溶液的配制和样品的稀释等过程, 本评估方法可为气相色谱-三重四极杆质谱法的不确定评估提供 依据。

英文摘要:

      Objective To evaluate the uncertainty of determination of pesticide fipronil in vegetables by gas chromatography-triple quadrupole mass spectrometry. Methods According to JJF 1059.1-2012 Evaluation and Expression of Uncertainty in Measurement and JJF 1135-2005 Evaluation of Uncertainty in Chemical Analysis Measurement, a mathematical model was established for the uncertainty evaluation of fipronil in vegetables with internal standard method. The sources of uncertainty that may be introduced were analyzed. Results Each component of uncertainty was quantified for the calculation of the combined uncertainty, the results showed that an expanded uncertainty of 0.0096 mg/kg (k=2) was obtained for the determination of the presence of (0.02±0.0096) mg/kg fipronil in vegetables. Conclusion The uncertainties of the determination mainly come from the preparation of standard curve and the dilution process of samples. This study can provide a reference for uncertainty evaluation of GC-MS/MS analysis.