高效液相色谱法测定糕点中安赛蜜的不确定度评定  

Uncertainty Evaluation for Determination of Acesulfame Potassium in Patisseriesamples by High Performance Liquid Chromatography

作　　者：舒静 邹力 范芳芳 魏宁果 李媛 王珺 SHU Jing;ZOU Li;FAN Fangfang;WEI Ningguo;LI Yuan;WANG Jun(Shaanxi Institute of Supervision&Testing on Product Quality,Xi’an 710048)

机构地区：[1]陕西省产品质量监督检验研究院,西安710048

出　　处：《食品工业》2024年第8期262-266,共5页The Food Industry

摘　　要：评定高效液相色谱法测定糕点中安赛蜜的不确定度。依据GB 5009.140—2023《食品安全国家标准食品中乙酰磺胺酸钾的测定》测定糕点中安赛蜜含量,分析测定过程中的不确定度来源,并通过建立数学模型量化不确定度分量,全面评估及合成计算该试验过程中的不确定度。结果表明,测得糕点中安赛蜜的质量分数为5.86±0.11mg/kg (k=2)。测定过程的不确定度来源主要有标准储备液、标准曲线的配置、标准曲线的拟合、试样的称重、定容体积、试验加标回收率及重复性测定等。其中,标准储备液本身的不确定度对该试验结果的合成不确定度贡献最大,试样称重对试验结果的合成不确定度贡献最小。试验方法可反映高效液相色谱法测定糕点中安赛蜜的置信度和准确性,为日常实际检验工作提供参考。Evaluate the uncertainty of determination of acesulfame potassium in patisserie samples by high performance liquid chromatography(HPLC).According to GB 5009.140—2023 National Food Safety Standard Determination of Potassium Acetosulfonate in Food,the content of acesulfame in pastries has been determined.Guide to the evaluation and expression of uncertainty in measurement,the sources of uncertainty in HPLC determination of acesulfame potassium in patisserie samples have been fully analyzed.Furthermore,the combined uncertainties and expanded uncertainties have been calculated based on the established mathematical models.Results showed that The content of acesulfame potassium in patisserie could be shown as 5.86±0.11 mg/kg(k=2).The sources of uncertainty in the measurement process mainly include the standard stock solution,the configuration of standard curves,the fitting of standard curves,the determination of sample repeatability,the constant volume of the sample,the spiked recovery rate of the experiment and the repeatability testing.However,the uncertainty of the standard reserve solution itself contributes the most to the final synthesis uncertainty,and the factor of sample weighing has the smallest contribution.This method can reflect the confidence and accuracy of using high-performance liquid chromatography to determine acesulfame in pastries,and providing reference for daily practical inspection work.It provided reference for daily practical testing work.

关 键 词：高效液相色谱法 糕点 安赛蜜 不确定度 

分 类 号：O657.72[理学—分析化学] TS213.23[理学—化学]