Uncertainty Evaluation of Determination of Methomyl Residues in Potato by High Performance Liquid Chromatography-Tandem Mass Spectrometry
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摘要:
为提高马铃薯食品安全检测结果的准确性，利用高效液相色谱−串联质谱法对马铃薯中灭多威进行测定，分析具体试验过程，建立数学模型，确定各测量不确定度分量并进行比较。当马铃薯中灭多威残留量1.3 μg/kg时，其扩展不确定度0.84 μg/kg（
k =2）。结果表明，在各测量不确定度分量中，仪器本身、标准曲线绘制、试验方法重复性所带来的不确定度占主要因素。-
关键词:
- 马铃薯 /
- 灭多威 /
- 高效液相色谱−串联质谱法 /
- 不确定度 /
- 残留
Abstract:In order to improve accuracy of potato food safety detection results, high performance liquid chromatography-tandem mass spectrometry was used to determine methomyl in potato, analyze specific experimental process, establish a mathematical model, determine and compare components of measurement uncertainty．When residue of aphid phosphorus in potato was 1.3 μg/kg, expanded uncertainty was 0.84 μg/kg（
k =2）．Results showed that among measurement uncertainty components, uncertainty caused by instrument itself, standard curve drawing and experimental repeatability were main factors． -
表 1 灭多威残留量测量结果
Table 1. Measurement results of methomyl residues
测量次数 样品质量/g 测量浓度/
（ng·mL−1）灭多威残留量/
（μg·kg−1）1 7.50 10.2219 1.3629 2 7.52 9.9811 1.3273 3 7.50 9.8347 1.3113 4 7.56 10.1625 1.3442 5 7.59 9.7534 1.2850 6 7.59 9.2946 1.2246 7 7.50 9.9790 1.3305 平均值 7.54 9.8896 1.3123 
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表 2 各浓度峰面积结果
Table 2. Peak area results for each concentration
浓度/（ng·mL−1） 峰面积Ai $ a{C}_{i}+b $ A1 A2 A3 $ \overline{{A}_{i}} $ 10 806.281 804.256 820.422 810.320 818.489 20 1576.404 1580.145 1584.596 1580.382 1517.824 25 1817.460 1811.496 1821.578 1816.845 1867.492 50 3637.827 3630.459 3642.459 3636.915 3615.829 125 8842.513 8837.589 8849.259 8843.120 8860.842 $ \overline{{C}_{i}} $ 46 —
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表 3 加标回收率测定结果
Table 3. Determination results of recovery rate of methomyl
序号 称样量/g 加标量/（μg·kg−1） 测定值/（μg·kg−1） 回收率/% 平均值/% 1 7.5213 2.9250 2.7994 95.7 93.7 2 7.5001 2.9333 2.7367 93.3 3 7.5016 2.9327 2.7284 93.0 4 7.5065 2.9308 2.6359 89.9 5 7.6125 2.8900 2.6316 91.1 6 7.5241 2.9239 2.8647 98.0 7 7.5492 2.9142 2.7626 94.8
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