Electrochemical treatment in KOH renews and activates carbon fiber microelectrode surfaces

Carbon fiber microelectrodes (CFMEs) are the standard electrodes for fast-scan cyclic voltammetry (FSCV) detection of neurotransmitters. CFMEs are generally used untreated but the surface can be activated with different treatments to improve electrochemical performance. In this work, we explored electrochemical treatments to clean and activate the CFME surface. We used different solution conditions for electrochemical treatment and found that electrochemical pretreatment in KOH outperforms treatment in KCl, H₂O₂, or HCl by accelerating the surface renewal process. The etching rate of carbon with electrochemical treatment in KOH is 37 nm/min, which is 10 times faster than that in the other solutions. Electrochemical treatment in KOH for several minutes regenerates a new carbon surface, which introduces more oxygen functional groups beneficial for adsorption and electron transfer. The KOH-treated CFMEs improved the limit of detection (LOD) to 9 ± 2 nM from 14 ± 4 nM for untreated CFMEs, and they successfully detected stimulated dopamine release in rat brain slices, demonstrating that they are stable and sensitive enough to use in biological systems. Electrochemical treatment in KOH completely restores the electrode sensitivity after biofouling. The proposed electrochemical treatment is simple and fast and can be applied prior to using CFMEs or after use to restore the surface. Thus, the method has potential to be a standard step to clean the carbon surface, or restore the sensitivity of electrodes from biofouling.