A novel vortex-assisted magnetic solid phase extraction method followed by flame atomic absorption spectrometry was improved to separate, preconcentrate and determine the lead, copper and cadmium ions by using 1-Nitro-2-naphthol-3, 6-disulfonic acid disodium salt (Nitroso-R salt) impregnated magnetic Ambersorb-563 resin. The adsorbent was characterised by Fourier transform infrared spectra, BET surface analyser and scanning electron microscopy. The influences of various analytical parameters, such as pH value, type and volume of the eluent, sample volume, were optimised and the effects of potentially interfering ions were investigated. The analyte ions were quantitatively recovered at pH 7.0 on magnetic adsorbent and desorbed with a 2.0 M HNO3 in 10% acetone as eluent. The detection limits were 1.4, 5.8 and 1.5ngmL(-1) for Cd(II), Cu(II) and Pb(II), respectively. The method has been validated with analytically by the analysis certified reference materials and standard additions prior to application to determine metal ions in water samples.