HPLC法测定熟肉制品中山梨酸的不确定度评估

Uncertainty Evaluation for the Determination of Sorbic Acid in Meat Products by High Performance Liquid Chromatography

目的:对高效液相色谱法测定熟肉制品中山梨酸含量进行不确定度评定,确定影响检测结果的关键因素,提高检验结果的准确性。方法:按照《食品安全国家标准食品中山梨酸、山梨酸和糖精钠的测定》(GB 5009.28—2016)第一法液相色谱法,对肉制品中的山梨酸含量进行测定。依据《化学分析中不确定度的评估指南》(CNAS-GL 006:2018)建立各影响因素的数学模型,对标准物质的含量、称量、标准曲线的配制、标准曲线的线性拟合,样品称量、前处理及样品重复性,以及仪器定量重复性等各因素进行了分析和评定。结果:肉制品中山梨酸残留量为52.678 mg·kg^(-1),扩展不确定度为6.519 mg·kg^(-1),测定结果表示为:X=(52.678±6.519)mg·kg^(-1)(k=2)。结论:本次不确定度的主要来源是标准曲线配制和仪器定量重复性。该评定方法为高效液相色谱法检测肉制品等复杂基质中的山梨酸含量的测量不确定度提供参考。

Objective:To evaluate the uncertainty for the determination of Sorbic Acid in meat products by High Performance Liquid Chromatography(HPLC),determine the key factors affecting the accuracy of the detection results,and improve the accuracy of the detection results.Methods:Sorbic acid in meat products were determined by HPLC according to GB 5009.28-2016,and a mathematical model was established to analyze and evaluate the sources of uncertainty such as purity of reference materials,weighing of reference materials,preparation of standard curves,weighing of samples,preparation of samples,fitting of standard curves,repeatability of sample measurement,etc.according to CNAS-GL006:2018.Results:the contents of Sorbic Acid in meat products was 52.678 mg·kg^(-1) with the extended uncertainty was 6.519 mg·kg^(-1).The determination results were expressed as X=(52.678±6.519)mg·kg^(-1)(k=2).Conclusion:The repeatability of instrument quantitative measurement and the preparation of standard curve are the main sources of measurement uncertainty,which should be controlled in the detection process.This evaluation method provides a reference for the measurement uncertainty of sorbic acid content in complex matrices such as meat products by high performance liquid chromatography.