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学科主题: 临床医学
题名:
DETERMINATION OF DIETHYLSTILBESTROL IN HUMAN PLASMA WITH MEASUREMENT UNCERTAINTY ESTIMATION BY LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY
作者: Liu, Yi1; Li, Na2; Ma, Liping2; Huang, Lin1; Jing, Shan3; Zhao, Libo1; Feng, Wanyu1
关键词: diethylstilbestrol ; LC-MS ; MS ; measurement uncertainty ; plasma ; total error ; validation
刊名: JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
发表日期: 2014-02-07
DOI: 10.1080/10826076.2012.745140
卷: 37, 期:3, 页:353-366
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 ; SOLID-PHASE MICROEXTRACTION ; METHOD VALIDATION ; SFSTP PROPOSAL ; STEROID-HORMONES ; PROSTATE-CANCER ; HARMONIZATION ; STRATEGIES ; ESTROGENS ; URINE
英文摘要:

A rapid and sensitive liquid chromatography/tandem mass spectrometry (LC-MS/MS) using an electrospray ionization (ESI) method was developed and validated to determine the concentration of diethylstilbestrol in human plasma. Samples were extracted with methyl tert-butyl ether after alkalified by sodium tetraborate solution, using 3,5-dihydroxy-4-isopropyl toluylene as the internal standard (IS). Separation was performed on a Restek C-18 column (2.1mmx150mm, 5.0 mu m) guarded by a Hypersil Gold pre-column (2.1mmx10mm, 3 mu m). The mobile phase consisted of acetonitrile-water (85:15, containing 0.2mmol/L ammonium acetate) at a flow rate of 0.3mL/min. Detection was performed using negative multiple reaction monitoring (MRM) mode. The mass transitions monitored were [M-H](-)m/z267.2237.2 and [M-H](-)m/z253.2211.0 for diethylstilbestrol and IS, respectively. The method was fully validated using total error theory, which is based on -expectation tolerance intervals and include trueness and intermediate precision. The method was found to be accurate over a concentration range of 0.1-50ng/mL. The main advantages of this method were the high sensitivity (a lower limit of quantification, LLOQ, of 0.1ng/mL) and the short analysis time (total run time 5min per sample). The measurement uncertainty based on -expectation tolerance intervals was assessed at each concentration level of the validation standards. The method is specific, sensitive, and accuracy, and it is suitable for plasma concentration determination of diethylstilbestrol.

语种: 英语
所属项目编号: RDB2010-28
项目资助者: Peking University People&prime ; s Hospital Research and Development Funds
WOS记录号: WOS:000326867400006
Citation statistics:
内容类型: 期刊论文
URI标识: http://ir.bjmu.edu.cn/handle/400002259/51917
Appears in Collections:北京大学第二临床医学院_药剂科_期刊论文

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作者单位: 1.Peking Univ Peoples Hosp, Dept Pharm, Beijing 100044, Peoples R China
2.Peking Univ Peoples Hosp, Cent Lab, Beijing 100044, Peoples R China
3.Peking Univ Peoples Hosp, Dept Cardiol, Beijing 100044, Peoples R China

Recommended Citation:
Liu, Yi,Li, Na,Ma, Liping,et al. DETERMINATION OF DIETHYLSTILBESTROL IN HUMAN PLASMA WITH MEASUREMENT UNCERTAINTY ESTIMATION BY LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY[J]. JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES,2014,37(3):353-366.
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