The development of an efficient process to simultaneously extract oxygen and metals from lunar regolith by way of in-situ resource utilisation (ISRU) has the potential to enable sustainable activities beyond Earth. The Metalysis-FFC (Fray, Farthing, Chen) process has recently been proven for the industrial-scale production of metals and alloys, leading to the present investigation into the potential application of this process to regolith-like 2 materials. This paper provides a proof-of-concept for the electro-deoxidation of powdered solid-state lunar regolith simulant using an oxygen-evolving SnO2 anode, and constitutes the first in-depth study of regolith reduction by this process that fully characterises and quantifies both the anodic and cathodic products. Analysis of the resulting metallic powder shows that 96% of the total oxygen was successfully extracted to give a mixed metal alloy product. Approximately a third of the total oxygen in the sample was detected in the off-gas, with the remaining oxygen being lost to corrosion of the reactor vessel. We anticipate, with appropriate adjustments to the experimental setup and operating parameters, to be able to isolate essentially all of the oxygen from lunar regolith simulants using this process, leading to the exciting possibility of concomitant oxygen generation and metal alloy production on the lunar surface.