Evaluation of Uncertainty in Determination of Sildenafil in Functional Food by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry
郭巧云 1龚子珊 1谢鑫宝 2张静 3徐亮4
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作者信息
1. 天津医学高等专科学校,天津 300222
2. 天津医科大学,天津 300070
3. 天津海关动植物与食品检测中心,天津 300457
4. 天津医学高等专科学校,天津 300222;天津医科大学,天津 300070
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摘要
基于超高效液相色谱-串联质谱法(Ultra High Performance Liquid Chromatography-Tandem Mass Spectrome-try,UPLC-MS/MS)对保健食品中西地那非添加量进行了不确定度评估.通过对样品量取、标准物质溶液的配制、标准曲线拟合、样品稀释定容、重复性测量等实验过程中引入的不确定度进行评定和分析,计算得到在保健食品中的西地那非的总量为0.7878 mg/L时,扩展不确定度为0.0795 mg/L,包含因子k为2.引起测量不确定度的因素主要是标准物质溶液的配制(相对标准不确定度为0.0433)、最小二乘法拟合标准工作曲线(相对标准不确定度为0.0226),其次为样品的量取、定容、稀释以及测量重复性.该评估模型可为采用UPLC-MS/MS测定西地那非的不确定度评定提供参考.
Abstract
In this study,the uncertainty of sildenafil addition in functional foods was evaluated based on Ultra-high Per-formance Liquid Chromatography-Tandem Mass Spectrometry(UPLC-MS/MS).By evaluating and analyzing the uncer-tainty introduced in the experimental process of sample measurement,standard material solution preparation,standard curve fitting,sample dilution and volume determination,and repeatability measurement,the expanded uncertainty was 0.0795 mg/L and the coverage factor k was 2 when the total amount of sildenafil in functional food was 0.7878 mg/L.The measurement uncertainty was mainly caused by the preparation of standard solution preparation(urel(C)=0.0433)and the least square fitting standard working curve(urel(y)=0.023),then by the sample weighing,dilution and detection.The eval-uation system could be used to provide a reference for the uncertainty evaluation of the determination of sildenafil in func-tional food by UPLC-MS/MS.
关键词
不确定度/超高效液相色谱-串联质谱法(UPLC-MS/MS)/西地那非/保健食品/外标法
Key words
uncertainty/Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry(UPLC-MS/MS)/sildenafil/functional food/external standard method
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