Related Experiment Video
Updated: Jun 28, 2026

Determination of the Gas-phase Acidities of Oligopeptides
Published on: June 24, 2013
Can alpha- and beta-alanine containing peptides be distinguished based on the CID spectra of their protonated ions?
Adrian K Y Lam1, Sri H Ramarathinam, Anthony W Purcell
1School of Chemistry, The University of Melbourne, Victoria, Australia.
Abstract:
The fragmentation reactions of isomeric dipeptides containing alpha- and beta-alanine residues (alphaAla-alphaAla, alphaAla-betaAla, betaAla-alphaAla, and betaAla-betaAla) were studied using a combination of low-energy and energy resolved collision induced dissociation (CID). Each dipeptide gave a series of different fragment ions, allowing for differentiation. For example, peptides containing an N-terminal beta-Ala residue yield a diagnostic imine loss, while lactam ions at m/z 72 are unique to peptides containing beta-Ala residues. In addition, MS(3) experiments were performed. Structure-specific fragmentation reactions were observed for y(1) ions, which help identify the C-terminal residue. The MS(3) spectra of the b(2) ions are different suggesting they are unique for each peptide. Density functional theory (DFT) calculations predict that b(2) ions formed via a neighboring group attack by the amide are thermodynamically favored over those formed via neighboring group attack by the N-terminal amine. Finally, to gain further insight into the unique fragmentation chemistry of the peptides containing an N-terminal beta-alanine residue, the fragmentation reactions of protonated beta-Ala-NHMe were examined using a combination of experiment and DFT calculations. The relative transition-state energies involved in the four competing losses (NH(3), H(2)O, CH(3)NH(2), and CH(2)=NH) closely follow the relative abundances of these as determined via CID experiments.
Related Concept Videos
Mass Spectrometry of Amines
NMR Spectroscopy and Mass Spectrometry of Aldehydes and Ketones
Mass Spectrometry: Amine Fragmentation
In amines, the number of nitrogen atoms affects the mass of the molecular ion, which is described by the nitrogen rule of mass spectrometry. This rule states that a compound containing a single or...
Peptide Identification Using Tandem Mass Spectrometry
This technique helps gather information regarding the protein from which the peptide was obtained and to study the peptides’ amino acid sequence. Identifying peptides from a complex mixture is an important component of the growing field of...
NMR and Mass Spectroscopy of Carboxylic Acids
While α protons of carboxylic acids absorb at 2–2.5 ppm, β protons absorb further upfield.
Carboxylic acids are easily identified by dissolving them in deuterium oxide, which results in a rapid exchange of the acidic protons with deuterium. This leads to the disappearance of the acidic...
NMR Spectroscopy Of Amines

