论文部分内容阅读
目的:探讨固相萃取-气相色谱(SPE-GC)法测定人血中丙戊酸浓度的不确定度评定方法。方法:通过分析测定过程,确定并简化不确定度来源;通过统计学方法,量化SPE-GC法测定人血中丙戊酸浓度过程中各不确定度分量,包括仪器测定精密度、对照品称量、标准溶液的配制、含药血清的配制、血清药物提取等;计算合成不确定度和扩展不确定度。结果:血清中低、高(16.8,134.5μg·mL-1)质量浓度丙戊酸的扩展不确定度分别为5.04μg·mL-1和11.84μg·mL-1(P=95.45%,k=2)。结论:SPE-GC法测定人血清中丙戊酸浓度时,低浓度样品不确定度主要来自标准曲线的拟合,高浓度样品不确定度主要来自血清药物提取(回收率)及仪器测定重复性(精密度)。
OBJECTIVE: To evaluate the uncertainty of the determination of valproic acid in human blood by solid-phase extraction-gas chromatography (SPE-GC). Methods: To determine and simplify the sources of uncertainty through the analysis of the measurement process; Quantification of the uncertainty components in the determination of valproic acid concentration in human blood by the SPE-GC method, including the precision of the instrument, the reference substance Preparation of standard solution, preparation of medicated serum, extraction of serum drug and the like; and calculation of synthetic uncertainty and extended uncertainty. Results: The extended uncertainty of valproic acid in low and high serum (16.8,134.5μg · mL-1) were 5.04μg · mL-1 and 11.84μg · mL-1, respectively (P = 95.45%, k = 2). CONCLUSION: When the concentration of valproic acid in human serum is determined by SPE-GC, the uncertainty of the low concentration sample mainly comes from the fitting of the standard curve. The uncertainty of the high concentration sample mainly comes from the serum drug extraction (recovery) and the repeatability of the instrument (Precision).