This work discusses the primary methods of preparing urine samples for voltammetric analysis. To serve as model analytes, well-known and commonly used medicinal substances were employed. These substances exhibit distinct pharmacological effects and undergo varying transformations at the electrodes under voltammetry conditions. The selected model analytes encompass two alkaloids of plant origin – quinine and platyphylline, the platyphylline metabolite – its N-oxide, and the synthetic antibacterial drug sulfadimethoxine. The determination of model analytes in prepared samples of urine was carried out using a boron-doped diamond electrode and a dropping mercury electrode. The action of ultrasound on the urine sample turned out to be the optimal method of sample preparation, which allows you to liquid or other types of extraction and significant dilution of sample urine. Furthermore, the environmental aspects of voltammetric analysis for medicinal substance determination in urine, exemplified by quinine, were assessed. Various approaches, such as AGREEprep, AGREE metrics, Green Certificate, and Blue Applicability Grade Index (BAGI), were employed to evaluate environmental considerations. All these assessments yielded high ratings, indicating compliance with the principles of green analytical chemistry for the voltammetric technique in quinine determination in urine.