Specific and sensitive sensing of most pesticide residues
relies
on enzymes such as acetylcholinesterase and advanced materials, which
need to be loaded on the surface of working electrodes, leading to
instability, uneven surface, tedious process, and high cost. Meanwhile,
employing certain potential or current in electrolyte solution could
also modify the surface in situ and overcome these drawbacks. However,
this method is only regarded as electrochemical activation widely
applied in the pretreatment of electrodes. In this paper, by means
of regulating the electrochemical technique and its parameters, we
prepared a proper sensing interface and derivatized the carbaryl (a
carbamate pesticide) hydrolyzed form (1-naphthol) to enhance sensing
by 100 times within several minutes. After regulation I by chronopotentiometry
with 0.2 mA for 20 s or chronoamperometry with 2 V for 10 s, abundant
oxygen-containing groups form and the ordered carbon structure is
destroyed. Sweeping from −0.5 to 0.9 V through cyclic voltammetry
for only one segment, following regulation II, the composition of
oxygen-containing groups changes and the disordered structure is alleviated.
Finally, on the constructed sensing interface, test by regulation
III through differential pulse voltammetry from 0.8 to −0.4
V, resulting in derivatization of 1-naphthol during 0.8–0 V,
followed by electroreduction of the derivative at around −0.17
V. Compared with the electro-oxidation peak at 0.5 V in previous reports,
it is essential to improve specificity, even toward several other
carbamate pesticides with similar structures. Hence, the in situ electrochemical
regulation strategy has demonstrated great potential for effective
sensing of electroactive molecules.