Alzheimer's disease (AD) is a highly heterogeneous and progressive dementia which is characterised by a progressive decline in cognitive functioning, selective neuronal atrophy, and loss of cortical volume in areas involved in learning and memory. However, recent research has indicated that the AD-affected brain is also besieged by increases in oxidative stress as well as perturbations to the homeostasis of biometals, such as copper and iron. These metals are known to interact with the neuropathological hallmark of AD, the β-amyloid peptide (Aβ), in a manner which increases Aβ's neurotoxic effects. This knowledge has led to the development of therapeutic measures which act to restore biometal homeostasis within the AD brain. This chapter outlines how Surface-Enhanced Laser Desorption/Ionisation Time-of-Flight Mass Spectrometry can be used to monitor Aβ levels within biological systems as well as describing the use of immobilised metal affinity capture in the observation of synthetic Aβ peptides.