LC-MS/MS法测定人尿液中伪人参皂苷GQ浓度的不确定度评定
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篇名: LC-MS/MS法测定人尿液中伪人参皂苷GQ浓度的不确定度评定
TITLE:
摘要: 目的:评定液相色谱串联质谱 (LC-MS/MS) 法测定人尿液中伪人参皂苷GQ (PGQ) 浓度的不确定度。方法:全面分析LC-MS/MS法测定人尿液中PGQ浓度的整个过程,对测量重复性、标准品称量、工作液配制、生物样品配制、萃取回收过程、仪器允差和标准曲线拟和等引起的不确定度分别进行评定,计算合成不确定度并进行扩展。结果:人尿液中低、中、高(5.59、48.07、744.60 ng/ ml) 浓度PGQ的扩展不确定度分别为0.58、3.33、50.62(P=95%,k=2)。结论:LC-MS/MS法测定人尿液中PGQ浓度的不确定度在低浓度时主要由萃取回收率、生物样品制备和测量重复性引入,在中、高浓度时主要由生物样品制备和萃取回收率引入。
ABSTRACT: OBJECTIVE: To evaluate the uncertainty for the determination of pseudo-ginsenoside GQ (PGQ) concentration in human urine by LC-MS/MS. METHODS: The whole process of PGQ determination by LC-MS/MS in human urine was analyzed, and the uncertainty caused by repeatability, weighing, standard solution preparation, biological sample preparation, recovery, instrument precision and calibration curve fitting were evaluated. The combined uncertainty were calculated and expanded. RESULTS: The expanded uncertainty for low, medium, high (5.59, 48.07, 744.60 ng/ml) levels of PGQ in human urine were 0.58, 3.33, 50.62, respectively (P=95%,k=2). CONCLUSIONS: The uncertainty of the PGQ determination in human urine by LC-MS/MS is mainly caused by recovery, repeatability of biological sample preparation and determination at low concentration; by sample preparation and recovery at medium and high concentration.
期刊: 2016年第27卷第2期
作者: 霍记平,梅升辉,赵志刚,李新刚,胡蓓,李平亚,刘金平,江骥
AUTHORS: HUO Jiping,MEI Shenghui,ZHAO Zhigang,LI Xingang,HU Bei,LI Pingya,LIU Jinping,JIANG Ji
关键字: 液相色谱串联质谱法;尿液;伪人参皂苷GQ;不确定度
KEYWORDS: LC-MS/MS; Urine; Pseudo-ginsenoside GQ; Uncertainty
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