The antioxidant activity of small natural compounds found in spices and herbs was evaluated using electrochemical and spectrophotometric methods. The characteristic plants of the Dalmatian region were selected: rosemary, bay leaf and immortelle. In order to achieve the best possible extraction, 4 methods for the extraction of bioactive substances from aqueous preparations were tested. An electrode was made of pyrolytic graphite with a surface area of 7,5×10 -4 cm 2 , hypothesizing that the exceptional properties of this material would enable and facilitate electron transfer between the analyte and the electrode. By optimizing the parameters of differential pulse voltammetry (DPV), conditions were found that ensure high sensitivity, selectivity and reproducibility of results. The factor 35,8 mA/cm 2 indicates a high sensitivity and good linearity (R 2 =0,980) of the proposed method. Together with the selected parameters, the concentration of gallic acid in real samples was determined using the DPV method. The concentration of total phenols and antioxidant activity were also determined by spectrophotometric methods (SP). The best extraction method was microwave extraction for rosemary and bay leaf samples, simple extraction at 100 ºC for 5 minutes for the immortelle extract. The highest gallic acid concentration by SP method was found in immortelle extract (917,1 mg dm -3 ) and the highest antioxidant activity in microvawe-assisted rosemary extract (6406,4 μM Fe 2+ ). The results of DPV method follow the same trend. To evaluate the application of electrochemical methods for the determination of gallic acid or total phenolics, a mathematical correlation was established between the DPV and SP methods. The constant ratio of the gallic acid concentration determined by the DPV and SP methods of about 5,62 indicates that the proposed method is suitable for the estimation of total phenols in real samples.