Highly sensitive analysis of multinuclear complexes using electrospray mass spectrometry with an electrolysis cell

使用电解池电喷雾质谱法对多核配合物进行高灵敏度分析

基本信息

批准号：
06640784
负责人：
ARAKAWA Ryuichi
金额：
$ 0.77万
依托单位：
Osaka University
依托单位国家：
日本
项目类别：
Grant-in-Aid for General Scientific Research (C)
财政年份：
1994
资助国家：
日本
起止时间：
1994 至 1995
项目状态：
已结题

项目摘要

Electrospray mass spectrometry (ES-MS) has recently been shown to be a powerful technique for the measurement of molecular mass of involatile and thermally ladile compounds. ES-MS has an attractive advantage of soft ionization. The ES ionization results from the transfer of ions initially present in solution into the gas phase. So it provides a quite simple mass pattern and allows us to determine molecular mass accurately with high sensitivity. Because of various superiority of ES technique, we felt that ES-MS may be a useful tool for on-line analysis of reaction products or reaction intermediates in solution phase. In order to make sure this idea, we have examined photosubstitution and photooxidation reactions of metal complexes of bidentate ligands. A multipurpose reaction cell of a cylindrical quartz cell (1mm i.d.) was developed and installed at the middle of the spraying needle. The sample solution in the cell was irradiated with a high pressure Xe lamp. Photolysis of [Ru (bpy) 2B] 2+ (bpy=2,2'-bipyridine and B=diamines) Ru (II) complexes were studied in acetonitrile solution. The monoimine intermediates for the oxidation process and monodentate intermediates of the bidentate diamine ligand for the stepwise photosubstitution were for the first time directly detected using on-line ES-MS.In this study, we demonstrated that the present ES-MS method proved analytically useful for easy identification of unstable intermediates or primary products in solution.

电喷雾质谱法（ES-MS）最近已被证明是一种用于测量intatile和热脂质化合物的分子质量的强大技术。 ES-MS具有软电离的吸引力。 ES离子化是由最初存在于溶液中的离子转移到气相中的。因此，它提供了非常简单的质量模式，并使我们能够以高灵敏度准确地确定分子质量。由于ES技术的各种优势，我们认为ES-MS可能是在溶液阶段对反应产物或反应中间体进行在线分析的有用工具。为了确保这个想法，我们检查了双齿配体金属配合物的摄影剂和光氧化反应。开发了一个圆柱石英池（1mm I.D.）的多功能反应细胞，并安装在喷雾针中间。用高压XE灯照射细胞中的样品溶液。 [RU（BPY）2B] 2+的光解（BPY = 2,2'-双吡啶和B =二胺）RU（II）在乙腈溶液中研究了复合物。单二胺中间体用于氧化过程和单次二胺配体的单次中间体用于逐步摄影固定的二胺配体，这是第一次使用在线ES-MS.S.中直接检测到这项研究，我们证明了当前的ES-MS方法在分析中证明了有用的有用为了轻松识别解决方案中不稳定的中间体或主要产品。