液相色谱-串联质谱法测定牛奶中氯霉素残留量的不确定度评定

Uncertainty evaluation of chloramphenicol in milk by high performance liquid chromatography-tandem mass spectrometry

目的采用液相色谱-串联质谱法对牛奶中氯霉素的残留量进行不确定度评定。方法根据GB29688-2013《牛奶中氯霉素残留量的测定液相色谱-串联质谱法》建立数学模型,根据JJF 1059.1-2012《测量不确定度的评定与表示》对测量结果的各不确定度来源进行分析和量化。结果本方法的不确定度主要来自于标准曲线的建立及测定结果重复性。当氯霉素的添加水平为0.1064 ng/g时,氯霉素的结果可表示为0.1064±0.0457 ng/g(k=2)。结论该评定方法清晰合理,简便准确,可适合液相色谱-串联质谱法对牛奶中氯霉素的残留量测定的不确定度评定。

Objective To evaluate the uncertainty in determination of chloramphenicol in milk by high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）. Methods According to GB 29688-2013 The determination of chloramphenicol in milk by high performance liquid chromatography-tandem mass spectrometry, the uncertainty model was established. According to JJF 1059-1999 Evaluation and expression of uncertainty in measurement, the main sources of the uncertainty resulted from the determination process were discussed and calculated. Results The major uncertainty sources were curve calibration and the repeatability test. When the chloramphenicol content in dairy products was 0.1064 ng/g, the uncertainty was 0.0457 ng/g, and the chloramphenicol content was expressed as （0.10644-0.0457） ng/g （k=2）. Conclusion The evaluation method is reasonable, clear, simple and accurate, which is suitable for the evaluation of uncertainty of chloramphenicol in milk determined by HPLC-MS/MS.