A simple and available method for on-line preparation of the adsorbent and solid phase extraction procedure for multi-element determination by inductively coupled plasma mass spectrometry (ICP-MS) has been proposed. The adsorbent (Al 2 O 3 -PB-AC) was synthesised by sequential impregnation of Al 2 O 3 with Polybrene (PB) and Alizarin Complexone (AC). Cd(II), Cr(III), Ni(II), Pb(II) and Zn(II) were quantitatively recovered using Al 2 O 3 -PВ-AC from aqueous solutions at pH 6.5 and at a flow rate of 1.0 mL min −1 . All the elements can easily be eluted by 3.0 mL 0.5 M HNO 3 . A mini-column packed with 0.100 g Al 2 O 3 -PB-AC retained all elements quantitatively from up to 50 mL multi-element solution with an enrichment factor of 16.7. The relative standard deviation for five replicate determinations was 3.5%, 7.3%, 6.2%, 7.4% and 4.7% for Cd(II), Cr(III), Ni(II), Pb(II) and Zn(II), respectively, for determination of 5 μg L −1 level. The developed method was applied for SPE-ICP-MS determination of Cd, Cr, Ni, Pb, Zn in snow and river waters.