高效液相色谱-串联质谱法测定食用油脂中合成辣椒素的不确定度评估  

Uncertainty Evaluation of Synthetic Capsaicin in Edible Oils and Fats by HPLC-tandem Mass Spectrometry

作　　者：李姣 LI Jiao(Tibet Autonomous Region Inspection and Research Institute for Food and Drug Control,Lasa 850000,China)

机构地区：[1]西藏自治区食品药品检验研究院,西藏拉萨850000

出　　处：《食品安全导刊》2022年第2期91-94,99,共5页China Food Safety Magazine

基　　金：西藏自治区自然科学基金项目(XZ2019ZR G-166)。

摘　　要：目的:评定高效液相色谱-串联质谱法测定食用油脂中合成辣椒素含量的不确定度,提高测定结果的准确度和可信度,找出对不确定度影响最大的关键性因素。方法:依据CNAS-GL 006:2019化学分析中不确定度的评估指南和《测量不确定度评定与表示》(JJF 1059.1—2012),采用高效液相色谱-串联质谱法测定食用油脂中合成辣椒素含量,建立不确定度评定的数学模型,通过对标准品溶液配制、样品溶液的配制、测量重复性以及标准曲线拟合这4个方面引入的不确定度进行分析,确定各个不确定度分量,得到扩展不确定度。结果:按置信区间为95%,合成辣椒素含量为(0.374±0.044)μg/kg,k=2。结论:测量结果的不确定度的主要来源是样品测量重复性引入的,其次是标准品溶液和样品溶液的配制,其他分量引入的不确定度相对较小。Objective:To evaluate the uncertainty of synthetic capsaicin content in edible oil by HPLC-tandem MS,improve the accuracy and credibility of the measurement results,and find out the key factors that have the greatest impact on the uncertainty.Methods:Synthetic capsaicin content in edible oils was determined by HPLCtandem mass spectrometry according to CNAS-GL 006:2019 Guidelines for Evaluation of Uncertainty in Chemical Analysis and Evaluation and presentation of Measurement Uncertainty by JJF 1059.1-2012,establish a mathematical model of uncertainty evaluation,analyze the uncertainty introduced in standard solution preparation,sample solution preparation,measurement repeatability,and standard curve fitting,and determine each uncertainty component,get the extended uncertainty.Results:According to the 95%confidence interval,the synthetic capsaicin content is(0.374±0.044)μg/kg,k=2.Conclusion:The main source of uncertainty in measurement results is the introduction of sample measurement repeatability,followed by the preparation of standard solution and sample solution,and the uncertainty introduced by other components is relatively small.

关 键 词：食用油脂 合成辣椒素 高效液相色谱-串联质谱法 不确定度 

分 类 号：O657.63[理学—分析化学] TS227[理学—化学]