© 2022, Pleiades Publishing, Ltd.Abstract: Deep eutectic solvent extraction for As, Mn, Pb, Cr, and Ni from spleen, kidney, and brain samples was investigated. The experimental parameters such as type and amount of deep eutectic solvent and sample/deep eutectic solvent ratio were optimized. The method optimization was conducted with the certified reference material (BCR 185-R). The analytical characteristics such as limits of detection and quantitation, relative standard deviation, and calibration equations were determined. Different deep eutectic solvent types were prepared and examined for better extraction. Choline chloride was used as a quaternary ammonium salt, and oxalic acid, urea, thiourea, and citric acid were used as hydrogen bond donors. Better results and recoveries higher than 90% were obtained with oxalic acid. The calculated LOD values for As, Mn, Pb, Cr, and Ni were 1.1, 0.3, 1.3, 1.4, 0.8, and LOQ values were 3.8, 1.1, 4.3, 4.7, 2.7 mg/kg, respectively.