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目的:建立中药麻黄提取物干预下,人血浆替代基质中炎症因子花生四烯酸代谢产物LTB_4的UPLC-MS/MS法测定的不确定度评定方法。方法:建立不确定度评定的数学模型,寻找不确定度的来源,确定影响不确定度的因素。用A类评定程序评价分析过程中随机效应引起的不确定度,用B类评定程序评价分析过程的其他因素引起的不确定度,包括:对照品纯度、量瓶允差、称量、移液管允差、移液器允差、回收率及标准曲线的拟合等,计算合成不确定度及扩展不确定度。结果:人血浆替代基质低(2.00μg/L)、中(25.00μg/L)、高(80.00μg/L)浓度LTB_4的扩展不确定度分别为1.46μg/L、3.00μg/L及8.66μg/L(P=95%,k=2)。结论:本方法绿色环保,样品回收率高,数据准确、可靠,适用于UPLC-MS/MS法测定人血浆替代基质中LTB_4浓度的不确定度评定,低浓度质控样品不确定度主要由线性回归过程引入,其次是含药血浆替代基质样品的配制及样品的提取,中、高浓度质控样品的不确定度主要由含药血浆替代基质样品的配制引入,其次是标准曲线的拟合,其他分量影响较小。本方法能够满足检测标准的要求,确保数据的国际互认。
OBJECTIVE: To establish a method for the determination of uncertainty in the determination of arachidonic acid metabolite LTB_4, which is an inflammatory cytokine, in human plasma substitute medium by the intervention of Chinese Herb Ephedra extract. Methods: To establish the mathematical model of uncertainty assessment, find the source of uncertainty and determine the factors that affect the uncertainty. Uncertainty caused by random effects in the analysis process is evaluated by the evaluation program of type A and the uncertainty caused by other factors of the analysis process is evaluated by the evaluation program of type B, including the purity of the reference substance, tolerance of the measuring bottle, weighing, pipetting Tube tolerance, pipette tolerance, recovery rate and the fitting of the standard curve to calculate the synthesis of uncertainty and expansion of uncertainty. Results: The extended uncertainty of LTB_4 for low, medium (2.00μg / L), medium (25.00μg / L) and high (80.00μg / L) human plasma were 1.46μg / L, 3.00μg / L and 8.66μg / L (P = 95%, k = 2). Conclusion: This method is environmentally friendly, with high sample recovery, accurate and reliable data, and is suitable for the evaluation of uncertainty of concentration of LTB_4 in human plasma replacement matrix by UPLC-MS / MS. The uncertainty of low- The regression process was introduced, followed by the preparation of drug-containing plasma substitute matrix samples and the extraction of samples. The uncertainty of medium- and high-quality control samples was mainly introduced by the formulation of medicated plasma-substitute matrix samples followed by the fitting of standard curve, Other components have less effect. The method can meet the requirements of testing standards and ensure the international mutual recognition of data.