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学科主题: 临床医学
题名:
Performance of tiloronoxim and tilorone determination in human blood by HPLC-MS/MS: Method validation, uncertainty assessment and its application to a pharmacokinetic study
作者: Zhang, Xianhua1,2; Duan, Jingli1; Zhai, Suodi1,2; Yang, Yiheng1; Yang, Li1
关键词: Tiloronoxim ; Tilorone ; HPLC-MS/MS ; Blood ; Total error ; Measurement uncertainty ; Pharmacokinetics
刊名: JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
发表日期: 2010-02-01
DOI: 10.1016/j.jchromb.2009.12.016
卷: 878, 期:3-4, 页:492-496
收录类别: SCI
文章类型: Article
WOS标题词: Science & Technology
类目[WOS]: Biochemical Research Methods ; Chemistry, Analytical
研究领域[WOS]: Biochemistry & Molecular Biology ; Chemistry
关键词[WOS]: QUANTITATIVE ANALYTICAL PROCEDURES ; SFSTP PROPOSAL ; HUMAN URINE ; HARMONIZATION ; STRATEGIES ; TIMOLOL ; RISK
英文摘要:

A highly sensitive and selective HPLC-MS/MS method is presented for the quantitative determination of tiloronoxim and its metabolite tilorone in human blood. An aliquot of 200 mu l human blood was extracted with a mixture of chloroform/ethyl ether(1/2, v/v), using metoprolol as the internal standard (the IS). Separation was achieved on an Xterra MS C18 column (50 mm x 2.1 mm, 5 mu m) with a gradient mobile phase of methanol/water containing 15 mM ammonium bicarbonate (pH 10.5). Detection was performed using positive MRM mode on a TurbolonSpray source. The mass transitions monitored were m/z 426.3 -> 100.0, m/z 411.3 -> 100.0 and m/z 2683 -> 116.1 for tiloronoxim, tilorone and the IS, respectively. The method was fully validated using total error theory, which is based on beta-expectation tolerance intervals and include trueness and intermediate precision. The method was found to be accurate over a concentration range of 1-100 ng/ml for both compounds. The measurement uncertainty based on P-expectation tolerance intervals was assessed at each concentration level of the validation standards. This method was successively applied to a pharmacokinetic study of tiloronoxim in healthy volunteers. (C) 2009 Elsevier B.V. All rights reserved

语种: 英语
WOS记录号: WOS:000274414500032
Citation statistics:
内容类型: 期刊论文
URI标识: http://ir.bjmu.edu.cn/handle/400002259/58654
Appears in Collections:北京大学第三临床医学院_药剂科_期刊论文

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作者单位: 1.Peking Univ, Hosp 3, Dept Pharm, Beijing 100191, Peoples R China
2.Peking Univ, Ctr Therapeut Drugs Monitoring & Clin Toxicol, Beijing 100191, Peoples R China

Recommended Citation:
Zhang, Xianhua,Duan, Jingli,Zhai, Suodi,et al. Performance of tiloronoxim and tilorone determination in human blood by HPLC-MS/MS: Method validation, uncertainty assessment and its application to a pharmacokinetic study[J]. JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES,2010,878(3-4):492-496.
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