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中国精品科技期刊2020
汪春明,张洋,施鹏斐,等. 气相色谱-质谱法测定黄瓜中毒死蜱残留量的测量不确定度评定[J]. 食品工业科技,2021,42(15):204−210. doi: 10.13386/j.issn1002-0306.2020040045.
引用本文: 汪春明,张洋,施鹏斐,等. 气相色谱-质谱法测定黄瓜中毒死蜱残留量的测量不确定度评定[J]. 食品工业科技,2021,42(15):204−210. doi: 10.13386/j.issn1002-0306.2020040045.
WANG Chunming, ZHANG Yang, SHI Pengfei, et al. Uncertainty Evaluation of Chlorpyrifos Residues in Cucumber Determination by Gas Chromatography-tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(15): 204−210. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2020040045.
Citation: WANG Chunming, ZHANG Yang, SHI Pengfei, et al. Uncertainty Evaluation of Chlorpyrifos Residues in Cucumber Determination by Gas Chromatography-tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(15): 204−210. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2020040045.

气相色谱-质谱法测定黄瓜中毒死蜱残留量的测量不确定度评定

Uncertainty Evaluation of Chlorpyrifos Residues in Cucumber Determination by Gas Chromatography-tandem Mass Spectrometry

  • 摘要: 当毒死蜱检出且位于限量值附近,为了能更好地对受检样品进行判定。本研究结合自身实验室的具体操作步骤,参考CNAS-GL 006、计量检定(技术)规范等相关标准,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》,采用气相色谱-质谱法测定,外标法定量,对黄瓜中毒死蜱残留量的测定结果进行不确定度评定。结果显示:在0.10 mg/kg添加水平、95%置信区间(k=2)下,毒死蜱的测定结果可表示为:(0.10±0.01)mg/kg;其中标准溶液配制不确定度分量对毒死蜱合成不确定度的贡献最高。可见当黄瓜中的毒死蜱残留量≥0.1 mg/kg且≤0.11 mg/kg时,不能判定为不合格,而是使用误差更小的容量瓶、降低操作员的读数误差、减少移液器使用数量、缩小环境温差后,重新进行测定。

     

    Abstract: In order to make better decisions when the concentration of chlorpyrifos was located near the maximum residue limit. This study combined with the specific operation steps of our own laboratory, referred to cnas-gl 006, metrological verification (technical) specifications and other relevant standards, according to "GB 23200.113-2018 determination of 208 pesticides and metabolites residues in foods of plant origin", the uncertainties of chlorpyrifos residues in cucumber was evaluated by gas chromatography-tandem mass spectrometry(GC-MS/MS) combined with external standard quantitative method. The results showed that: at the level of 0.10 mg/kg and 95% confidence interval (k=2), the determination results of chlorpyrifos could be expressed as: (0.10 ± 0.01)mg/kg;The uncertainty component of standard solution preparation has the highest contribution to the uncertainty of chlorpyrifos. It could not be determined as unqualified when the residual amount of chlorpyrifos in cucumber ≥0.1 mg/kg and ≤ 0.11 mg/kg. It is to use the volumetric flask with smaller error,reduce the reading error of the operator,reduce the number of pipettes,and reduce the temperature difference of the environment,and then perform the measurement again. The uncertainty assessment results will minimize the possible disputes in the judging of the residue values near the maximum residue limits.

     

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