Zöllner Peter, Lienau Annette, Albert Klaus, Lindner Wolfgang
Bayer Cropscience, Product Technology-Analytics Frankfurt, Industriepark Höchst-G836, D-65926 Frankfurt, Germany.
J Mass Spectrom. 2003 Jul;38(7):709-14. doi: 10.1002/jms.484.
The derivatization reaction of the mycotoxin moniliformin with 1,2-diamino-4,5-dichlorobenzene was previously introduced to improve distinctly the sensitivity of an assay applying high-performance liquid chromatography prior to fluorescence detection. In the course of the implementation of this derivatization approach into a liquid chromatographic/mass spectrometric method, an unexpected derivatization product has now been discovered by mass spectrometry. In order to elucidate its structure, detailed investigations with liquid chromatography/tandem mass spectrometry and liquid chromatography coupled on-line with NMR spectroscopy were performed. These studies give evidence for a heterocyclic structure that has been formed by the loss of one water and one carbon monoxide molecule. A reasonable mechanism for this derivatization reaction is proposed.
霉菌毒素串珠镰孢菌素与1,2 -二氨基-4,5 -二氯苯的衍生化反应先前已被引入，以显著提高在荧光检测之前应用高效液相色谱法的检测灵敏度。在将这种衍生化方法应用于液相色谱/质谱法的过程中，现在通过质谱法发现了一种意外的衍生化产物。为了阐明其结构，采用液相色谱/串联质谱法以及液相色谱与核磁共振光谱在线联用进行了详细研究。这些研究证明了一种由失去一个水分子和一个一氧化碳分子而形成的杂环结构。提出了这种衍生化反应的合理机制。
