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液相色谱串联质谱内标法测定猪肉中沙丁胺醇的不确定度分析

Uncertainty Analysis of Salbutamol in Pork by Liquid Chromatography Tandem Mass Spectrometry with Internal Standard Method
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摘要 目的:通过液相色谱串联质谱内标法测定猪肉中沙丁胺醇的含量,探究检验过程中的影响因素,并计算各因素的不确定度,为准确测定沙丁胺醇含量提供科学指导。方法:按照《化学分析中不确定度的评估指南》(CNAS—GL06:2019)、《测量不确定度评定与表示》(JJF 1059.1—2012)和《食品安全国家标准动物性食品中β-受体激动剂残留量的测定液相色谱-串联质谱法》(GB 31658.22—2022),分析不确定度来源。结果:样品测定值为28.3μg·kg^(-1),取置信区间为95%,扩展不确定度为4.477μg·kg^(-1)(k=2)。结论:通过对仪器设备、样品制备、标准品及内标、样品重复性测定和温度等因素的评估计算,结果发现高效液相色谱仪串联质谱仪、标准曲线配制、内标物质纯度对检测结果的影响较大,在实际测量过程中,严格控制实验条件可提高检测的可靠性、准确性。 Objective:To determine the content of salbutamol in pork by liquid chromatography tandem mass spectrometry internal standard,explore the influencing factors in the testing process,and calculate the uncertainty of each factor,in order to provide scientific guidance for the accurate determination of salbutamol content.Method:Sources of uncertainty were analyzed according to CNAS—GL06:2019,JJF 1059.1—2012 and GB 31658.22—2022.Result:The sample was measured at 28.3μg·kg^(-1),the confidence interval was 95%,and the extended uncertainty was 4.477μg·kg^(-1)(k=2).Conclusion:Through the evaluation and calculation of factors such as instrument equipment,sample preparation,standard and internal standards,sample repeatability determination,and temperature,it was found that high performance liquid chromatography tandem mass spectrometry,standard curve preparation,and internal standard substance purity have a significant impact on the detection results.In the actual measurement process,strict control of experimental conditions can improve the reliability and accuracy of detection.
作者 杨翠 YANG Cui(Ganzi Institute of Food and Drug Inspection,Ganzi 626000,China)
出处 《食品安全导刊》 2023年第28期58-63,共6页 China Food Safety Magazine
关键词 液相色谱串联质谱法 不确定度 猪肉 检测 沙丁胺醇 liquid chromatography tandem mass spectrometry uncertainty pork detection salbutamol
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