气相色谱-串联质谱法测定三七中五氯硝基苯残留量的不确定度评定

目的评定气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)测定三七中的五氯硝基苯残留量的不确定度。方法根据JJF1059-1999《测量不确定度评定与表示》中有关规定,建立了不确定度评定的数学模型,对各分量在构成合成不确定度时的影响率进行分析。结果本方法不确定度控制的关键在于控制好样品的标准曲线和检测过程中的随机效应。当三七中五氯硝基苯残留量为0.034 mg/kg,扩展不确定度为0.0039 mg/kg,五氯硝基苯残留量表示为(0.034±0.0039)mg/kg(k=2)。结论该评定方法清晰合理,可用于三七中五氯硝基苯残留的不确定度评定。

Evaluation of uncertainty in determination of quintozene in pseudo-ginseng by gas chromatography-tandem mass spectrometry

Objective To evaluate the uncertainty in determination of quintozene residues in pseudo-ginseng by gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods According to JJF1059-1999 Evaluation and Expression of Uncertainty in Measurement, a mathematical model of uncertainty was established, and the influencing rate of each component on composing uncertainty was analyzed. Results The key uncertainties resulted from sample standard curve and random effects in the process of detection. When the quintozene residues content in pseudo-ginseng was 0.034 mg/kg, the expanded uncertainty was 0.0039 mg/kg, and the quintozene residues content was expressed as (0.034±0.0039) mg/kg (k=2). Conclusion This method is clear and reasonable, which can be used for the evaluation of uncertainty of quintozene residues in pseudo-ginseng.