Uncertainty Evaluation for Determination of Sibutramine in Health Food by HPLC-MS/MS

Abstract

High-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was used to determine the content of sibutramine in health foods according to the BJS 201701 standard Determination of Compounds such as Sibutramine in Food. By evaluating each uncertainty component, the influencing factors of the uncertainty were identified and the expanded uncertainty of sibutramine detection in health foods was provided. Using the example of illegal addition of sibutramine to health products, the HPLC-MS/MS method was used for qualitative screening and quantitative analysis of samples. The sources of uncertainty in the quantitative results were analysed, including sample weighing, sample volume determination, standard solution preparation, standard curve fitting and determination of sample repeatability. The synthetic relative standard uncertainty of the measurement results was calculated and the expanded uncertainty was reported. By optimizing the liquid phase conditions, the sample can be detected within 5 min with a linear correlation coefficient of 0.998. When the content of sibutramine in health products was 42.2 mg/kg, the extended uncertainty of the results was 4.56 mg/kg (k = 2) with a 95% confidence interval. Among the various components affecting the results of detection, the uncertainty introduced during the process of preparing the standard solution has the greatest impact on the results. A proper evaluation of the uncertainty, detailed analysis and quantification of the various sources of uncertainty can help to improve the reliability of test results.