In this research, the first study on the high performance of Nanoparticled γ-alumina coated with sodium dodecyl sulfate and 4-2-pyridylazo-resorcinol (SDS-PAR) as a new sorbent solid phase extraction has been reported. Sorbent with adjusted nanometer-sized alumina was used to preconcentrate and separate Cu in plant belonging to the legume family and natural water samples. A microsample introduction system was employed for the nebulization micro-volume of diluted solution by FAAS (flame atomic absorption spectrometry) method. Various influencing parameters on the separation and preconcentration of trace metal, such as pH, amount of sorbent, and volume of the chelating agent, were studied. The calibration graph was linear in the range of 1-800 μg L-1 with detection limit of 0.21 μg L-1. RSD for ten reproduce measurements was 1.8%. The proposed method has been applied to the decision of Cu ions at trace levels in substantial samples such as cucumber, eggplant, mint, tomato, potato, parsley, spinach, apple, mangosteen, kiwi, banana, The apple core, macaroni, pea, wheat flour, red beans, lentil, barley, tap water, river water, sea water. The proposed analytical method was successfully applied to the determination of Cu in mentioned samples.