A simple and efficient method for separation and determination of dimethylarsenate DMAs(V) was developed in this work. Two resins, a strong base anion exchange (SBAE) resin and iron-oxide coated hybrid (HY) resin were tested. By simple adjusting pH value of water at 7.00, DMAs(V) passed through the HY column without any changes, while all other arsenic species [inorganic arsenic and monomethylarsonate, MMAs(V)] were quantitatively bonded on HY resin. The resin capacity was calculated according to the breakthrough points in a fixed bed flow system. At pH 7.00 the HY resins bonded more than 4150 μg g-1 of As(III), 3500 μg g-1 of As(V) and 1500 μg g1 of MMAs(V). Arsenic adsorption behavior in the presence of impurities showed tolerance with the respect to potential interference of anions commonly found in natural water. DMAs(V) was determined in the effluent by ICP-MS. The detection limit was 0.03 μg L?1 and relative standard deviation (RSD) was between 1.1?7.5 %. Proposed method was established performing standard procedures: with external standard, certified reference material and the standard addition method