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目的:对人血浆利培酮浓度液质联用法(HPLC-MS/MS)测定的不确定度进行评定。方法:对HPLC-MS/MS法测定血浆中利培酮浓度的全过程进行分析,对于分析过程中称量、溶液配制、液液萃取、仪器以及标准曲线拟和等影响因素引起的不确定度进行了逐层分析,用A类评定程序评价了分析过程中随机效应引起的不确定度,用B类评定程序评价了分析过程的其他因素引起的不确定度,最后根据各分量计算出合成不确定度并进行了扩展。结果:置信概率P为95%时,血浆低(0.65ng·mL-1)、中(10.86ng·mL-1)、高(21.72ng·mL-1)浓度利培酮的扩展不确定度分别为0.24,0.35,0.70ng·mL-1。结论:该方法适用于HPLC-MS/MS法测定血浆中利培酮浓度的不确定度评定,为复杂生物基质分析过程的不确定度评定提供了重要参考。
Objective: To evaluate the uncertainty of determination of human plasma risperidone by liquid chromatography-mass spectrometry (HPLC-MS / MS). Methods: The whole process of determination of risperidone in plasma by HPLC-MS / MS method was analyzed. The uncertainty caused by influencing factors such as weighing, solution preparation, liquid-liquid extraction, instrument and standard curve fitting during the analysis A level-by-level analysis was conducted to evaluate the uncertainty caused by stochastic effects in the analysis process with a type A evaluation program. The uncertainty caused by other factors in the analysis process was evaluated with a class B evaluation program. Finally, The degree of certainty has been expanded. Results: The uncertainty of expansion of risperidone at low (0.65ng · mL-1), medium (10.86ng · mL-1) and high (21.72ng · mL-1) concentrations was 95% 0.24, 0.35, 0.70 ng · mL-1. Conclusion: This method is suitable for the evaluation of the uncertainty of determination of risperidone in plasma by HPLC-MS / MS, which provides an important reference for the evaluation of the uncertainty of complex biological matrix analysis.