摘要
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 evaluate the uncertainty of LTB4 in determination in human plasma substitute matrix by UP- LC - MS/MS for plasma concentration study of LTB4 with the administration of Ephedra sinica extract. Methods ： Mathe- matical model was established for the evaluation of uncertainty to identify influential factors of uncertainty. The uncertainty caused by random effects was evaluated with type A and others were by type B, including the purity of the comparison, the tolerance of the measuring flask, weighing error, the tolerance of the suction pipet, the tolerance of the transferpettor, the recovery and the standard curve. The combined uncertainty was calculated and the expanded uncertainty was obtained. Results： The expanded uncertainty for the low （2. 00 μg/L）, medium （25.00 μg/L） and high （80. 00 μg/L） levels of LTB4 was 1.46 μg/L,3.00μg/L and 8.66 μg/L, respectively （P = 95%, k = 2）. Conclusion ： This method is environmentally friendly with high recover and accuracy, and applicable for uncertainty evaluation of LTB4 determination in human plasma substitute matrix. The uncertainty of the low concentration control sample was mainly caused by the linear regression, followed by the preparation of the plasma substitute matrix sample and the extraction of the sample. The uncertainty of the medium and high concentration control samples is mainly introduced by the preparation of the plasma substitute matrix sample, followed by the linear regression, the other components less affected. It meets the requirements of the analysis standards to ensure the international recognition of data.
出处
《中华中医药学刊》
CAS
北大核心
2017年第10期2670-2675,共6页
Chinese Archives of Traditional Chinese Medicine
基金
辽宁省大型仪器设备共享服务能力建设项目(2016LD0113)
