The Bristol & Oxford Chemical Dynamics Group

Photodissociation of peptide model compounds

Mass spectrometry is an increasingly important analytical technique for the characterisation of a range of biological molecules.  Structural information may be obtained using tandem mass spectrometry (otherwise known as MS/MS) techniques, in which a single species is mass-selected in the first stage of the spectrometer, and is then fragmented and mass-analysed in the second stage.  This establishes the mass fragments associated with a given molecule under the chosen fragmentation conditions, allowing structural sub-units of the parent molecule to be identified.

 Schematic diagram of tandem mass spectrometry

Fig 1:  Tandem mass spectrometry

Fragmentation studies on large molecules have traditionally employed collisionally-induced dissociation (CID) or infra-red multiphoton dissociation (IRMPD).  In both of these methods, energy is added to the molecule gradually – in the former case through multiple collisions with an inert gas inside a collision cell, and in the latter through sequential absorption of a large number of infra-red photons – until it eventually reaches the dissociation threshold.  As a result, the fragmentation is a fairly slow process, and the fragments are generally well thermalised.  Alternative fragmentation techniques include electron capture dissociation (ECD) and ultra-violet photodissociation (UVPD), both of which are much more ‘direct’ and rapid processes.  There is considerable current interest in UVPD from an analytical perspective, as the fragmentation patterns observed are often complementary to those seen in CID or IRMPD, and therefore provide further structural information.

UVPD is often a very rapid process in peptides [1], occurring on a much faster timescale than intramolecular vibrational redistribution and leading to ‘non-statistical’ fragmentation patterns (e.g. weaker bonds may stay intact while stronger bonds are cleaved) and fragments with non-statistical energy content.   For example, photodissociation at 157 nm has been shown to favour cleavage of a carbon-carbon bond within the peptide backbone, rather than the carbon-nitrogen bond favoured by CID and IRMPD [2], and is thought to occur via a two-step mechanism involving an odd-electron intermediate species, with side chain fragmentation also occurring in some cases.  

We are using new ‘multi-mass’ variants of the velocity-map imaging technique, together with the H atom photofragment translational spectroscopy technique (PTS), to better our understanding of the UVPD process in peptides.  Our studies are directed towards understanding the nature of the participating electronic states, together with the fragmentation mechanism(s) and dynamics of the dissociation process.  The first step is an investigation into the dissociation dynamics of N,N-dimethylformamide, a useful small-molecule model for the peptide bond in proteins, following laser photolysis at 157, 193, 248 and 266 nm.  This compound is known to have a number of accessible dissociation pathways [3], which the velocity-map imaging technique will allow us to probe in detail.  Three previously identified pathways following 193 nm photolysis are shown in Figure 1 below.  Additional H-atom elimination channels are highly likely, and these will be ideal candidates for photofragment translational spectroscopy studies at Bristol.

 

Fig 2:  Pathways for photodissociation of N,N-dimethylformamide

Once we have a solid understanding of some of these ‘simplest’ of photodissociation processes in peptides, we will broaden our studies to explore a range of di- and tri-peptides, in order to investigate the effect of different amino acid residues on the fragmentation mechanisms and dynamics.  These investigations will form the foundation for later studies on larger peptides.

[1] R. Antoine, M. Broyer, J. Chamot-Rooke, C. Dedonder, C. Desfrancois, P. Dugourd, G. Grégoire, C. Jouvet, D. Onidas, P. Poulain, T. Tabarin, and G. van der Rest, Rapid Commun. Mass Spectrom. 20 1648 (2006).

[2] W. Cui, M.S. Thompson, and J.P. Reilly, J. Am. Soc. Mass Spectrom. 16, 1384 (2005); M.S. Thompson, W. Cui, and J.P. Reilly, Angew. Chem. Int. Ed., 43, 4791 (2003).

[3] N. R. Forde, L. J. Butler and S. A. Abrash, J. Chem. Phys, 110, 8954 (1999).