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目的建立气相色谱法(gas chromatography,GC)测定大豆油中有机氯农药残留结果的不确定度评定的数学模型。方法依据JJF 1059.1-2012《测量不确定度评定与表示》,全面考虑测量过程中的不确定度来源,对大豆油中有机氯农药残留的不确定度进行评定。结果当取样量为1.0 g,k=2(置信度为95%)时,检测出大豆油中六六六(hexachlorocyolohexane,HCH)和滴滴涕(dichlorodiphenyltrichloroethane,DDT)含量。α-HCH、β-HCH、γ-HCH、δ-HCH、o,p’-DDT和p,p’-DDT的含量分别为:(0.66±0.090)、(1.32±0.104)、(0.52±0.074)、(0.35±0.066)、(0.12±0.032)和(0.051±0.014)mg/kg。结论 GC法测定大豆油中有机氯农药残留的不确定度主要来源于测定结果重复性,其次为标准工作液的配制及色谱峰面积引起的不确定度,其他因素的影响相对较小。
OBJECTIVE To establish a mathematical model for evaluating the uncertainty of determination of organochlorine pesticide residues in soybean oil by gas chromatography (GC). Methods According to JJF 1059.1-2012 Evaluation and Expression of Uncertainty in Measurement, the uncertainty of the organochlorine pesticide residues in soybean oil was assessed by considering the sources of the uncertainty during the measurement. Results The content of hexachlorocyclohexane (HCH) and dichlorodiphenyltrichloroethane (DDT) in soybean oil was detected when the sample volume was 1.0 g and k = 2 (confidence was 95%). The contents of α-HCH, β-HCH, γ-HCH, δ-HCH, o, p’-DDT and p, p’-DDT were 0.66 ± 0.090, 1.32 ± 0.104 and 0.52 ± 0.074, ), (0.35 ± 0.066), (0.12 ± 0.032) and (0.051 ± 0.014) mg / kg, respectively. Conclusion The uncertainty of determination of organochlorine pesticide residues in soybean oil by GC method mainly comes from the repeatability of the determination results followed by the formulation of standard working solution and the uncertainty caused by the chromatographic peak area. The influence of other factors is relatively small.