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使用快原子轰击和串联质谱法对类固醇硫酸盐进行定量分析的评估。

Evaluation of the quantitative analysis of a steroid sulphate using fast atom bombardment and tandem mass spectrometry.

作者信息

Gaskell S J

机构信息

Tenovus Institute for Cancer Research, University of Wales College of Medicine, Health, Cardiff, UK.

出版信息

Biomed Environ Mass Spectrom. 1988 Jan 15;15(2):99-104. doi: 10.1002/bms.1200150207.

DOI:10.1002/bms.1200150207
PMID:2964883
Abstract

Dehydroepiandrosterone sulphate (DHAS) has been quantified in human blood serum by fast atom bombardment (FAB)/tandem mass spectrometry of immunoadsorption extracts. FAB of DHAS yielded abundant ions corresponding to the intact steroid sulphate; these were selected by a double-focusing mass spectrometer prior to collisionally activated decomposition in a quadrupole collision cell and mass analysis by a quadrupole mass filter. [HSO4]- (m/z 97) was the sole prominent daughter ion. For quadrupole mass filter was set to transmit m/z 97 and a narrow-range magnet scan yielded a spectrum of parents, including m/z 367 and 369, corresponding to DHAS and the (2H2)-analogue (used as internal standard), respectively. Serum concentrations by this procedure were in good agreement with data obtained by gas chromatographic/mass spectrometric analyses of DHA heptafluorobutyrate, formed by direct derivatization of the steroid sulphate.

摘要

已通过免疫吸附提取物的快原子轰击(FAB)/串联质谱法对人血清中的硫酸脱氢表雄酮(DHAS)进行了定量。DHAS的FAB产生了与完整甾体硫酸盐相对应的大量离子;在四极碰撞池中进行碰撞激活分解并通过四极质量过滤器进行质量分析之前,这些离子由双聚焦质谱仪进行选择。[HSO4]-(m/z 97)是唯一突出的子离子。将四极质量过滤器设置为传输m/z 97,并进行窄范围磁扫描,得到包括m/z 367和369的母离子谱,分别对应于DHAS和(2H2)类似物(用作内标)。通过该程序测得的血清浓度与通过对甾体硫酸盐直接衍生化形成的DHA七氟丁酸酯进行气相色谱/质谱分析获得的数据高度一致。

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