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目的:评定液相色谱-串联质谱(LC-MS/MS)法测定人尿液中头孢替安浓度的不确定度。方法:本研究对头孢替安浓度测定过程的各种影响因素,包括测定精密度、称量、标准溶液的配制、含药尿液的配制、尿液样品预处理、仪器、标准曲线拟合等进行分析评定,采用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,采用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,根据各分量计算得到扩展不确定度和合成不确定度。结果:人尿液中0.2,4和80μg·m L-1头孢替安的扩展不确定度分别为1.139 6,1.139 6和6.118 4μg·m L-1(P=95%,k=2)。结论:LC-MS/MS法测定人尿液中头孢替安浓度的不确定度主要由标准曲线拟合和回收率引入。
OBJECTIVE: To evaluate the uncertainty of the determination of cefotiam in human urine by liquid chromatography-tandem mass spectrometry (LC-MS / MS). Methods: Various influencing factors of cefotiam concentration determination were studied in this study, including precision, weighing, preparation of standard solution, preparation of drug-containing urine, pretreatment of urine sample, instrument, standard curve fitting, etc. A type A evaluation program was used to evaluate the uncertainty caused by random effects in the analysis process. The B type evaluation program was used to evaluate the uncertainty caused by other factors in the analysis process. Based on each component, the extended uncertainty and Synthetic uncertainty. Results: The extended uncertainty of cefotiam for 0.2, 4 and 80 μg · mL -1 human urine was 1.139 6,1.139 6 and 6.118 4 μg · m L-1, respectively (P = 95%, k = 2). Conclusion: The uncertainty of LC-MS / MS method for the determination of cefotiam in human urine is mainly induced by standard curve fitting and recovery.