We have successfully demonstrated the functionalization of MO LCP with an amphiphilic redox probe, dodecyl(ferrocenylmethyl)dimethylammonium bromide (Fc12-Br), to enhance the electroactivity of the entrapped GOx enzyme. Nonetheless, the activity of the Fc12-Br/MO/GOx bioelectrode rapidly decayed after 7 days, hindering practical applications. We hypothesised that this might be predominantly due to the instability of the redox probe because in other studies the LCP without Fc12 was found to enhance the stability of GOx at room temperature. Causes for this instability could be : a) Fc12-Br leaching at the interface into the bulk environment; 38 b) Fc12-Br inducing a localized phase transition away from the Pn3m structure into a phase such as the two-dimensional lamellar L ! phase which would show retarded 3D diffusivity; 39 and c) other processes, such as a surface adsorption or reaction, as previously reported. To develop a stable system for practical applications, it is important to discriminate between these alternatives, for example by localizing the Fc12-Br molecules during electrochemical reactions. Accordingly, in this work we performed in-situ small-angle neutron scattering (SANS), adopting the set-up from Randle et al and Draper. Neutron beams interact differently to matter compared to X-ray beams, which leads to intrinsic differences in values of scattering length density (SLD) for neutrons compared to X-rays.