超高效液相色谱-串联质谱测定保健食品中西地那非的不确定度评估  

Evaluation of Uncertainty in Determination of Sildenafil in Functional Food by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：郭巧云 龚子珊 谢鑫宝 张静 徐亮 Guo Qiaoyun;Gong Zishan;Xie Xinbao;Zhang Jing;Xu Liang(Mass Spectrometry Application Technology Lab,Tianjin Medical College,Tianjin 300222,China;Tianjin Medical University,Tianjin,300070,China;Animal,Plant and Food Testing Center,Tianjin Customs District,Tianjin 300457,China)

机构地区：[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

出　　处：《廊坊师范学院学报（自然科学版）》2024年第4期82-88,共7页Journal of Langfang Normal University(Natural Science Edition)

基　　金：国家自然科学基金(81402889)。

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。In this study,the uncertainty of sildenafil addition in functional foods was evaluated based on Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry(UPLC-MS/MS).By evaluating and analyzing the uncertainty 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 evaluation system could be used to provide a reference for the uncertainty evaluation of the determination of sildenafil in functional 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 

分 类 号：O657.63[理学—分析化学]