汪志威, 周思齐, 李非里, 齐沛沛, 王祥云, 狄珊珊, 徐浩, 王新全. 实验室农药残留检测的测量不确定度评定——以GB 23200.8—2016测定草莓中4种农药残留为例[J]. 农药学学报, 2020, 22(1): 105-114. DOI: 10.16801/j.issn.1008-7303.2019.0057
    引用本文: 汪志威, 周思齐, 李非里, 齐沛沛, 王祥云, 狄珊珊, 徐浩, 王新全. 实验室农药残留检测的测量不确定度评定——以GB 23200.8—2016测定草莓中4种农药残留为例[J]. 农药学学报, 2020, 22(1): 105-114. DOI: 10.16801/j.issn.1008-7303.2019.0057
    WANG Zhiwei, ZHOU Siqi, LI Feili, QI Peipei, WANG Xiangyun, DI Shanshan, XU Hao, WANG Xinquan. Evaluating the uncertainty of measurement of pesticide residue detection—a case study of four pesticide residues in strawberry by GB 23200.8—2016[J]. Chinese Journal of Pesticide Science, 2020, 22(1): 105-114. DOI: 10.16801/j.issn.1008-7303.2019.0057
    Citation: WANG Zhiwei, ZHOU Siqi, LI Feili, QI Peipei, WANG Xiangyun, DI Shanshan, XU Hao, WANG Xinquan. Evaluating the uncertainty of measurement of pesticide residue detection—a case study of four pesticide residues in strawberry by GB 23200.8—2016[J]. Chinese Journal of Pesticide Science, 2020, 22(1): 105-114. DOI: 10.16801/j.issn.1008-7303.2019.0057

    实验室农药残留检测的测量不确定度评定——以GB 23200.8—2016测定草莓中4种农药残留为例

    Evaluating the uncertainty of measurement of pesticide residue detection—a case study of four pesticide residues in strawberry by GB 23200.8—2016

    • 摘要: 自2018年《CNAS-GL006化学分析中不确定度的评估指南》颁布后,不确定度计算方法的需求日益增强。本研究依据GB 23200.8—2016《水果和蔬菜中500种农药及相关化学品残留量的测定 气相色谱-质谱法》,采用气相色谱-质谱法,结合内标定量法,对草莓中丙溴磷、亚胺硫磷、五氯硝基苯和氯氟氰菊酯的残留进行了测量不确定度的详细评定,共涉及标准品纯度、储备液配制、工作液配制、称样量和前处理过程5个B类评定分量,以及标准溶液峰面积、样品溶液峰面积和添加回收率3个A类评定分量。结果显示:在0.08 mg/kg添加水平下,丙溴磷、亚胺硫磷、五氯硝基苯和氯氟氰菊酯的测量合成相对标准不确定度依次为3.55%、3.22%、2.20%和3.66%,样品溶液峰面积和添加回收率2个A类不确定度分量对4种农药合成不确定度的贡献较高,其中丙溴磷、亚胺硫磷和氯氟氰菊酯均超过60%,五氯硝基苯超过31%。本研究中4种农药在草莓样品中的测量结果在95%的置信限 (k = 2) 内可表示为:丙溴磷,0.085 ± 0.006 mg/kg;亚胺硫磷,0.084 ± 0.005 mg/kg;五氯硝基苯,0.079 ± 0.003 mg/kg;氯氟氰菊酯,0.082 ± 0.006 mg/kg。不确定度评定结果将最大限度地减少待测物在最大残留限量附近的残留值判定可能存在的争议。

       

      Abstract: Since “CNAS-GL006 guidelines of uncertainty in chemical analysis” was published in 2018, the demand for calculation method of uncertainty has been increasing. According to "GB 23200.8—2016 determination of 500 pesticides and related chemical residues in fruits and vegetables by gas chromatography-mass spectrometry", the uncertainties of profenofos, phosmet, quintozene and cyhalothrin residues in strawberries were evaluated by gas chromatography-mass spectrometry (GC-MS) combined with internal standard quantitative method. Five B-type evaluation components, including standard purity, stocking solution, working solution, sample weighing and pretreatment process, and three A-type evaluation components, including standard solution peak area, sample solution peak area and recovery, were studied. Results showed that the relative combined standard uncertainties of profenofos, phosmet, quintozene and cyhalothrin at the spiking level of 0.08 mg/kg were 3.55%, 3.22%, 2.20% and 3.66%, respectively. Two A-type evaluation components of sample solution peak area and recovery had great contribution in the combined uncertainty of four pesticide residues, which was higher than 60% for profenofos, phosmet and cyhalothrin, and higher than 31% for quintozene. In this study, the detection results of four insecticides in strawberry samples in 95% confidence interval could be expressed as profenofos: 0.085 ± 0.006 mg/kg, phosphorus: 0.084 ± 0.005 mg/kg, quintozin: 0.079 ± 0.003 mg/kg, and cyhalothrin: 0.082 ± 0.006 mg/kg (k = 2). The uncertainty assessment results will minimize the possible disputes in the judging of the residue values near the maximum residue limts.

       

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