UPLC-MS/MS法检测肉制品中克伦特罗残留量的不确定度评定

建立了UPLC-MS/MS法检测肉制品中克伦特罗残留量的不确定度评定方法,分析了肉制品中克伦特罗残留量的测定过程中供试品重复性测量、标准曲线拟合残差、标准品溶液的配制、供试品溶液的配制、分析仪器等因素对测定的不确定度的影响。结果表明,按照JJF1059-1999《测量不确定度评定与表示》对各不确定度分量合成和扩展,当置信概率为95%,包含因子k=2,其扩展相对不确定度为16.08%。通过对不确定度的分析,发现标准曲线拟合残差是不确定度的主要来源,并由此提出了质量控制改进方法。该研究对于肉制品中克伦特罗残留量测量的不确定度标准制定具有一定的示范意义。 

Evaluation of uncertainty measurement in the content determination of clenbuterol residues in meat products by UPLC-MS/MS

A method for the evaluation of the uncertainty of clenbuterol residues in meat products by UPLC-MS/ MS was established. The influencing factors on the uncertainty in the procedure of the content determination were evaluated, including repeatability of results of measurements, the fitting of standard curves, the preparation of standard solutions and sample solutions and the analytical instrument.According to JJF1059-1999, the component uncertainties were synthesized and extended.An expended uncertainty of 16.08% was obtained at the confidence probability of 95% and coverage factor of k = 2.Based on the analysis of uncertainty, the fitting residual of standard curves were the major source of the uncertainty. Meanwhile, some strategies for improving quality control were proposed.Measurement of uncertainty was applicable to set the limit of the clenbuterol. It was important to the standards studies of uncertainty of clenbuterol residues in meat products.