An anion-exchange fast protein liquid chromatographic–inductively coupled plasma atomic emission spectrometric procedure (FPLC–ICP-AES) was developed for speciation of Al–citrate and other negatively charged Al complexes. FPLC separations were carried out on a Mono Q HR 5/5 strong anion-exchange FPLC column over a pH range from 3.5 to 11.0. An aqueous—NaNO 3 (4 mol dm −3) linear gradient elution was applied over 10 min for separation of a particular Al species. The separated Al species were determined in 0.5 cm 3 eluate fractions `off line' by ICP-AES. Under optimal analytical procedures Al–citrate was separated from Al–oxalate and Al–EDTA in a neutral pH range. Good reproducibility of the FPLC–ICP-AES procedure was obtained for determination of a particular Al species at optimal measurement conditions (RSD ±2%). Al 3+ and neutral Al–citrate species were strongly adsorbed on the column resin and did not interfere with the separation of negatively charged Al complexes. Al(OH) 4 − species were separated from Al–citrate in an alkaline pH region, but quantitatively determined only at a pH of 11.0. The distribution of Al species over a pH range from 3.5 to 11.0 agreed with the reported calculated data. The limit of detection (3 σ basis) for separated Al species was 0.1 μg cm −3.