Identifying reactive intermediates by mass spectrometry

Abstract

Development of new reactions requires finding and understanding of novel reaction pathways. In challenging reactions such as C-H activations, these pathways often involve highly reactive intermediates which are the key...

Reaction Monitoring and Structural Characterisation of Coordination Driven Self-Assembled Systems by Ion Mobility-Mass Spectrometry

“…The challenge of identifying and resolving occluded species is non-trivial to the study of dynamic libraries of self-assembling species in solution ( Figure 3 ) ( Misuraca et al, 2014 ). Mass spectrometry gives ready access to real time analysis of dynamic systems on a millisecond timescale ( Schalley and Springer, 2009 ; Hudgens et al, 2011 ; Pettibone and Hudgens, 2012 ; Olivares et al, 2014 ; Yunker et al, 2014 ; Ligare et al, 2017a ; Ligare et al, 2017b ; Ujma et al, 2017 ; Schnell et al, 2019 ; Mehara and Roithová, 2020 ; Zelenka and Roithová, 2020 ). The difficulties of occluded isobaric and isomeric species can be overcome by adding a filter for shape and size, in addition to m/z , namely, an ion-mobility spectrometer (IMS) ( Ujma et al, 2017 ; Polewski et al, 2021 ).…”

A “one pot” mass spectrometry technique for characterizing solution- and gas-phase photochemical reactions by electrospray mass spectrometry

“…7,8 This is despite the fact that it has been widely used to investigate non-photochemical reactions. [9][10][11] Very recently, a number of on-line photolysis set ups have been demonstrated that dramatically enhance the potential of mass spectrometry as a tool for monitoring photochemical reactions. [12][13][14] In this paper, we describe the application of an instrument that combines on-line photolysis with electrospray ionization mass spectrometry detection and laser-interfaced mass spectrometry (LIMS) to study the photodissociation of CO from metal carbonyl compounds.…”

“…| RSC Adv., 2021,11,[19500][19501][19502][19503][19504][19505][19506][19507] © 2021 The Author(s). Published by the Royal Society of Chemistry…”

Photodegradation of Riboflavin under Alkaline Conditions: What can Gas-Phase Photolysis Tell Us About What Happens in Solution?

“…This experimental approach which characterizes the gas-and solution-phase behavior of a chosen system provides a "one-pot" tool for approaching the understanding photochemistry. The technique builds on other recent experiments which have employed on-line photolysis, with subsequent mass spectrometric detection [16][17][18][19][20]. The benefit of this approach is that the solution-phase measurements probe a more "real-world" environment for the riboflavin vitamin (e.g., when it is in milk or within a cosmetic formulation), while the gas-phase measurements aid the understanding of the solution-phase photochemical mechanisms.…”

“…The benefit of this approach is that the solution-phase measurements probe a more "real-world" environment for the riboflavin vitamin (e.g., when it is in milk or within a cosmetic formulation), while the gas-phase measurements aid the understanding of the solution-phase photochemical mechanisms. The solution-phase environment is potentially much more complex, since direct photoproducts can undergo secondary reactions and will be subject to environmental factors, i.e., pH, solvent, and aggregation [5,[16][17][18][19][20]. This two-step method provides a new approach that could be widely applied to characterize the photochemical breakdown of food, beauty, and pharmaceutical products.…”