A new, simple and fast protocol to generate gold-based SERS substrates is presented in this work. Melamine is a
compound widely used in the industry that can be toxic for humans if consumed even in low concentrations.
EC-SERS is an excellent alternative to classical methods to detect and quantify this compound because Raman
spectroscopy provides a fingerprint of the molecules, providing very good sensitivity. In this work, timeresolved Raman spectroelectrochemistry is employed to generate a SERS substrate and to detect melamine,
all in a single experiment. The dynamic character of this technique provides valuable information about the
interaction of the molecule with the generated substrate. An optimization of the spectroelectrochemical
method based on a multi-pulse amperometric detection has been performed. The new protocol presented in
this work shows significant figures of merit in a very short experiment time, just 25 s.
