超高效液相色谱-串联质谱法测定乳饮料中香兰素的不确定度评定

Evaluation of uncertainty in Determination of Vanillin in Milk Beverage by Ultra Performance Liquid Chromatography Mass Spectrometry

采用液相色谱-质谱法对乳饮料中香兰素进行不确定度评定。通过整个测定过程建立不确定度测定模型来确定影响不确定度的主要来源,并对各不确定度分量进行合成和扩展,最终建立液相色谱-质谱法测定乳饮料香兰素的不确定度评定方法。结果表明,影响乳饮料中香兰素测定的主要来源为称样量、样品定容、测定浓度、测定重复性和提取回收率,其测定结果为(0.312mg/kg±0.047,K=2)。按引入的不确定度的贡献大小排序,依次为测定浓度(包括由标准品纯度、标准品称量、标准溶液的配制、校准曲线的线性拟合产生的不确定度以及仪器引入的不确定度)、提取回收率、测定重复性、样品定容、称样量,其中测定浓度中的标准溶液的配制分量引入的不确定度贡献最大。该模型的建立为检测乳饮料中香兰素的不确定度评定提供了参考依据,同时在日常的检测过程中可利用测量活动进行质量控制和质量保证,对测量结果的符合性具有重要意义。

To develop an uncertainty evaluation method of vanillin in milk beverage by ultra Performance liquid chromatography mass spectrometry.The model and sources of uncertainty were founded through analyzing the whole determination procedure.The key uncertainty factors of affecting measurement results were synthesized and expanded.The measurement result is 0.312mg/kg±0.047,K=2.The results showed that the key factors of uncertainty attributed had five factors including sample amount,sample volume,sample concentration,repeatability,extraction recovery and the standard solution of sample concentration provided most contribution than others.