Methods for separation and detection of ketosteroids and other carbonyl-containing compounds
    4.
    发明授权
    Methods for separation and detection of ketosteroids and other carbonyl-containing compounds 有权
    分离和检测酮类和其他含羰基化合物的方法

    公开(公告)号:US07807472B2

    公开(公告)日:2010-10-05

    申请号:US10511409

    申请日:2003-04-15

    IPC分类号: G01N33/00 G01N1/00

    摘要: Methods for enhancing detection by mass spectroscopy (MS) and/or chromatographic separability of carbonyl-containing compounds such as steroids are disclosed. Reaction of a carbonyl compound with a sulfonhydrazide compound provides a sulfonhydrazone with enhanced ionization efficiency during the electrospray ionization process. In a particularly disclosed embodiment, derivatization of catechol estrogens with p-toluenesulfonhydrazide enhances both detection by atmospheric pressure ionization-MS (API-MS), such as electron spray ionization-MS (ESI-MS) and separation by liquid chromatography (such as HPLC) under reverse phase conditions. In yet other embodiments, the sulfonhydrazone is further reacted with a sulfonyl halide under alkaline conditions to derivatize hydroxyl groups in the compound. Prior formation of the sulfonhydrazide derivative protects the carbonyl bond of the compound during subsequent alkaline reaction with the sulfonyl halide.

    摘要翻译: 公开了通过质谱(MS)检测和/或含羰基化合物如类固醇的色谱分离性的方法。 羰基化合物与磺酰肼化合物的反应提供了在电喷雾电离过程期间具有增强的电离效率的磺酰腙。 在特别公开的实施方案中,儿茶酚雌激素与对甲苯磺酰肼的衍生增强了通过大气压电离-MS(API-MS)的检测,例如电子喷雾离子化-MS(ESI-MS)和通过液相色谱法分离(例如HPLC )在反相条件下。 在其它实施方案中,磺酰腙在碱性条件下进一步与磺酰卤反应以衍生化合物中的羟基。 磺酰肼衍生物的先前形成在与磺酰卤的随后碱性反应期间保护化合物的羰基键。