In this thesis study, a dried-droplet LIBS methodology at reduced pressures for determining cadmium in aqueous media and in biological samples has been developed. With the advantage of the signal enhancement effect at reduced pressures, the optimum pressure for Cd detection was determined. Results were justified with the plasma images taken at different pressures. 100 mbar pressure was found as the optimum for most emission lines of Cd. To find the most suitable substrate onto which analyte droplets will be loaded, silicon wafer-based substrates of different coating types and coating thicknesses were studied. Among them, the c-Si substrate was found to show the highest signal enhancement for Cd detection. The performance of the methodology for quantitative analysis of Cd was shown by standard solutions and certified reference water samples. Calibration curves were constructed, and performance characteristics (limit of detection, accuracy, precision) were evaluated. Detection limits in absolute amounts of 6.8 pg and 1.05 pg were obtained at atmospheric and 100 mbar pressures, respectively. The application studies involve the determination of Cd bound to whey proteins. For this purpose, standard protein (BSA) and whey protein extracted from the milk were incubated in standard Cd solutions for several hours and filtered through cut-off filters via centrifugation. The unreacted cadmium in the filtrate and Cd-bound protein in fraction were analyzed separately. It has been shown that dried-droplet LIBS at reduced pressures is a suitable methodology for identifying and determining Cd and Cd bound to proteins with a picogram amount of detection capability.