質量分析法による有機化学反応中間体の構造解析(<特集>質量分析法の応用技術)
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概要
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Characterization of reaction intermediates formed during organic reactions is essential to understand the mechanisms of chemical reactions. We developed two methods to analyze and determine chemical structures of reaction intermediates using mass spectrometry. The one is "a FRIT-FAB LC/MS method" which consists of a fast atom bombardment mass spectrometer (FAB-MS : JEOL Model DX-303) connected to an HPLC via a pneumatic splitting interface. To perform LC/MS analysis, HPLC effluent was introduced into the mass spectrometer after mixing triethylene glycol as a matrix modifier. The FAB-MS was operated by applying an accelerating voltage of 3kV. The emission current and the voltage of the FAB gun was controlled to 10mA and 4kV, respectively. This method enables the detection of reaction having intermediates with more than 1 minute of life time. The other is "a Flow direct injection FAB-MS method (FDI/FAB-MS)". After mixing the solutions with two pistons continuously, the mixed solution is introduced into the FRIT-FAB mass spectrometer. The reaction time is controlled by changing the path-length of the sampling loops and the velocity of the flow rate. This is a suitable method by which to detect and estimate chemical structure of relatively short life time intermediates (more than a few seconds). Using these methods, we observed the oxidation reaction of hydrazine with quinone and clarifing the reaction scheme and confirming the validity of these methods.
- 社団法人日本分析化学会の論文
- 1996-06-05
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