A new method is reported for the separation of aluminum ions [AI(III)] from interfering elements in parenteral and pharmaceutical solutions (PS) and bottled mineral water (BMW) samples, through solid-phase extraction with 2-methyl-8-hydroxyquinoline (quinaldine) adsorbed onto activated silica gel. While the enrichment step of separated AI(Ill) was carried out by cloud point extraction (CPE) using 8-hydroxyquinoline as complexing reagent, the resulted complex was entrapped in a non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114). The enriched Al(III) in sample solutions were determined by spectrofluorometry (SPF) at lambda(excitation) 370 nm and lambda(emission) 510 nm, and flame atomic absorption spectrometry (FAAS) for comparative purpose. The variables affecting the complexation and extraction steps were studied and optimized. The validity of methodology was checked with certified reference material of water and standard addition method. The enrichment factor and detection limit of Al(III) for the preconcentration of 50 ml of PS and BMW were found to be 100 and 0.25 mu g/L, respectively. The proposed method has been applied for the determination of trace amount of AI(III) in PS and BMW samples with satisfactory results. In PS the levels of AI(III) are above than permissible limit (25 mu g/L). (C) 2009 Elsevier B.V. All rights reserved.