液相色谱-串联质谱法检测牛肉中苯乙醇胺A残留量不确定度评定
Uncertainty evaluation in measuring phenylethanolamine A in beef by liquid chromatography tandem mass spectrometry
倪永付 1王志宏 2白翔 1王登远 3王勇1
作者信息
- 1. 济宁海关综合技术服务中心,济宁 272000
- 2. 龙口海关综合技术服务中心,龙口 265700
- 3. 金乡县检验检测中心,金乡 272200
- 折叠
摘要
目的 对液相色谱-串联质谱法检测牛肉中苯乙醇胺A残留测量不确定度进行分析并评定.方法 通过分析检测过程和数学模型,确定苯乙醇胺A残留量的不确定度主要来源:检测设备带来的不确定度、标准品和样品称量带来的不确定度、实验室温度带来的不确定度、移取及定容体积带来的不确定度、样品前处理带来的不确定度、实验重复性带来的不确定度.结果 计算给出了各分量测量不确定度,并合成液相色谱-串联质谱法检测牛肉中苯乙醇胺A残留量相对标准不确定度urel=0.11,测定结果的扩展不确定度U(X)=0.11 μg/kg.液相色谱-串联质谱法检测牛肉中苯乙醇胺A残留量检测结果:X=(0.51±0.11)μg/kg,k=2.结论 检测设备对苯乙醇胺A残留量测量不确定度影响最大,样品前处理、实验重复性、移取及定容体积次之,日常检测中应重点关注仪器设备状况,及时进行核查与校准,规范实验过程、移取与定容操作,尽量减小上述因素对测量不确定度的影响.
Abstract
Objective Analyze and evaluate the measurement uncertainty of phenylethanolamine A residue in beef using liquid chromatography tandem mass spectrometry.Methods By analyzing the detection process and mathematical model,the main sources of uncertainty in the residual amount of phenylethanolamine A are determined:uncertainty caused by detection equipment,uncertainty caused by standard and sample weighing,uncertainty caused by laboratory temperature,uncertainty caused by transfer and constant volume,uncertainty caused by sample pretreatment,and uncertainty caused by experimental repeatability.Results The measurement uncertainty of each component was calculated and the relative standard uncertainty(urel=0.11)was synthesized for the detection of phenylethanolamine A residue in beef by liquid chromatography-tandem mass spectrometry.The expanded uncertainty of the determination results was U(X)=0.11 μg/kg.The detection result of measuring phenylethanolamine A in beef by liquid chromatography tandem mass spectrometry was:X=(0.51±0.11)μg/kg,k=2.Conclusion The detection equipment had the greatest impact on the measurement uncertainty of phenylethanolamine A residue,followed by sample pre-treatment,experimental repeatability,and transfer and constant volume.In daily testing,attention should be paid to the condition of the instruments and equipment,timely verification and calibration should be carried out,the experimental process,transfer and constant volume operation should be standardized,so that to minimize the impact of the above factors on measurement uncertainty as much as possible.
关键词
液相色谱-串联质谱法/牛肉/苯乙醇胺A/不确定度Key words
liquid chromatography tandem mass spectrometry/beef/phenylethanolamine A/uncertainty引用本文复制引用
出版年
2024
NETL
NSTL
万方数据