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活性过渡金属配合物的液体注射场解吸/电离

Liquid injection field desorption/ionization of reactive transition metal complexes.

作者信息

Gross Jürgen H, Nieth Norbert, Linden H Bernhard, Blumbach Ulrike, Richter Frank J, Tauchert Michael E, Tompers Rolf, Hofmann Peter

机构信息

Organisch-Chemisches Institut der Universität, Im Neuenheimer Feld 270, 69120 Heidelberg, Germany.

出版信息

Anal Bioanal Chem. 2006 Sep;386(1):52-8. doi: 10.1007/s00216-006-0524-0. Epub 2006 Jun 14.

Abstract

Liquid injection field desorption/ionization (LIFDI) has been applied to identify transition metal complexes that are highly reactive to air and moisture by mass spectrometry. The complexes of nickel and rhodium were supplied as dilute solutions (approximately 0.2 mg ml(-1)) in toluene, tetrahydrofuran or acetonitrile, and were applied onto the field desorption emitter inside the vacuum of the ion source under inert conditions by means of the injection capillary unique to the LIFDI set-up. LIFDI mass spectrometry on a double-focusing magnetic sector instrument provided spectra exhibiting intense molecular ion peaks for the species investigated or signals that could easily be related to the target compound by assuming neutral loss of the weakest-bound ligand. Eventually, byproducts of the synthesis or other components resulting from incomplete reactions or some degree of decomposition were also detected.

摘要

液体注射场解吸/电离(LIFDI)已被应用于通过质谱法鉴定对空气和水分具有高反应性的过渡金属配合物。镍和铑的配合物以甲苯、四氢呋喃或乙腈中的稀溶液(约0.2 mg ml⁻¹)形式提供,并通过LIFDI装置特有的进样毛细管在惰性条件下施加到离子源真空内的场解吸发射器上。在双聚焦磁扇形仪器上进行的LIFDI质谱分析提供了所研究物种的强分子离子峰光谱,或通过假设最弱结合配体的中性损失而容易与目标化合物相关的信号。最终,还检测到了合成的副产物或由不完全反应或某种程度的分解产生的其他成分。

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