The work describes electrochemical (EC) protocol suitable for preparation of copper electrodes which can be used as substrates in surface-enhanced Raman spectroscopy (SERS). These SERS-active electrodes have been used for electrospectral studies based on the combination of electrochemical and SERS analysis (EC-SRS analysis). Several endogenous bodyfl uid components (urea, creatinine, uric acid, bilirubin) have been selected for the study because they can signifi cantly aff ect the SERS-based determination of other analytes in bodyfl uids (for example, drugs).