In recent years there has been an increasing focus on the design and synthesis of electrochemical biosensors as they can lead to the analytical determination of biological and organic analytes. As amino acid and peptides play such a diverse role within biological systems incorporation of a redox active, chromophoric group into these compounds is of particular interest. This coupling is usually carried out as the last step in the preparation of such bioorganometallic compounds as the ferrocene moiety can prove sensitive to the conditions employed during peptide synthesis.