高效液相色谱法测定食品中栀子黄的不确定度评定

Uncertainty evaluation for determination of gardenia yellow in cake by high performance liquid chromatography

按照国家标准GB 5009.149-2016《食品安全国家标准食品中栀子黄的测定》的检测原理和方法,采用高效液相色谱法测定蛋糕中的栀子黄,标准规定了食品中栀子黄的代表性成份为藏花素和藏花酸。根据CNAS-GL06《化学分析中不确定度的评估指南》和JJF 1059.1-2012《测量不确定度评定与表示》的规定,建立数学模型,分析高效液相色谱法测定蛋糕中的藏花素和藏花酸含量的不确定度来源,并对各个不确定度分量进行量化,计算合成标准不确定度和扩展不确定度:糕点中藏花素测定结果为(0.060±0.006)g/kg,k=2,p=95%;藏花酸的测定结果为(0.026±0.002)g/kg,k=2,p=95%。评定结果发现在评估的6个不确定度分量中,影响检测结果不确定度的主要分量为标准溶液配制引入的不确定度、标准校正曲线拟合引入的不确定度。实验中可通过减小这些不确定度分量来提高检测结果的可靠性。

According to the principle and method of National standard GB 5009.149-2016,to determination of gardenia yellow in cake by high performance liquid chromatography,The standard stipulates that the representative ingredients of gardenia yellow in food are crocin and crocetin.A mathematical model is established according to CNAS-GL06＇s guidelines for evaluation of uncertainty in chemical analysis and JJF 1059.1-2012＇s evaluation and expression of measurement uncertainty. Analysis of the source of uncertainty in the determination of crocin and crocetin in cake by high performance liquid chromatography.Quantizing the components of each uncertainty,calculating the uncertainty of the synthetic standard and the expansion uncertainty.The content of crocin were （0.060±0.006） g/kg,k=2,p=95%, and the content of crocetin were （0.026±0.002）g/kg, k=2, p=95%.In 6 uncertainty components,The main components that affect the uncertainty of the detection results are Uncertainty in the introduction of standard solution preparation and The uncertainty introduced by the standard correction curve fitting. In the experiment, the reliability of the test results can be improved by reducing these uncertainty components.