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u_(rel)=0.11,测定结果的扩展不确定度U(X)=0.11μg/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。
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(u_(rel)=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)=0.11μg/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.
作者
倪永付
王志宏
白翔
王登远
王勇
NI Yong-Fu;WANG Zhi-Hong;BAI Xiang;WANG Deng-Yuan;WANG Yong(Comprehensive Technical Service Center of Jining Customs,Jining 272000,China;Comprehensive Technical Service Center of Longkou Customs,Longkou 265700,China;Inspection and Testing Center of Jinxiang County,Jinxiang 272200,China)
出处
《实验室检测》
2024年第2期14-17,共4页
Laboratory Testing
关键词
液相色谱-串联质谱法
牛肉
苯乙醇胺A
不确定度
liquid chromatography tandem mass spectrometry
beef
phenylethanolamine A
uncertainty
作者简介
通信作者:倪永付,硕士,高级工程师,研究方向为食品安全检测。E-mail:niyongfu@126.com
