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Spinel-type MgAl 2 O 4 nanoparticles with high surface area were synthesized by thermal decomposition of three different ion-pair complexes precursors, including [Mg(H 2 O) 6 ][Al(dipic) 2 ] 2 •6H 2 O, [Al(sal) 2 (H 2 O) 2 ] 2 [Mg(dipic) 2 ] and [Mg(H 2 O) 6 ][Al(ox) 2 (H 2 O) 2 ] 2 •5H 2 O. Influence of the inorganic precursor was investigated on synthesis and textural properties of magnesium aluminate nanopowders. The precursors [Mg(H 2 O) 6 ] [Al(dipic) 2 ] 2 •6H 2 O and [Al(sal) 2 (H 2 O) 2 ] 2 [Mg(dipic) 2 ] displayed pure spinel-type MgAl 2 O 4 , while the sample synthesized by [Mg(H 2 O) 6 ][Al(ox) 2 (H 2 O) 2 ] 2 •5H 2 O precursor consisted of MgAl 2 O 4 and MgO. The MgAl 2 O 4 synthesized via [Al(sal) 2 (H 2 O) 2 ] 2 [Mg(dipic) 2 ] precursor exhibited higher BET specific surface area (226.7 m 2 g −1) and smaller particle size than those of the samples obtained from the two other precursors.