Abstract

A range of methods based on reverse-phase high-performance liquid chromatography is described for determining Al, Cu, Fe and Mn. The simplest method for determining Fe, Cu and Al involves direct formation and separation of the 8-quinolinol complexes on the column, with 1:1 acetonitrile/water containing 5 × 10 −3 M 8-quinolinol, 0.4 M potassium nitrate and 0.02 M acetate buffer (pH 6.0) as the mobile phase, followed by electrochemical detection at −0.5 V vs. Ag/AgCl and/or spectrophotometric detection at 400 nm. Electrochemical detection enables < 2 ng Cu and < 1 ng Fe to be quantified for injection volumes of 20 μ1. Spectrophotometric detection allows simultaneous determinations of Al, Cu and Fe with lower sensitivity. The method is applied to the determination of Cu, Fe and Al in bovine liver and oyster tissue. Down to 1 ng of manganese (in the 20 μ1 injected) can be determined in biological samples by liquid chromatography with a mobile phase containing 1 mM Tris buffer (pH 8.8) after injection of an externally prepared 8-quinolinol complex. Preconcentration on Sep-Pak cartridges after dichloromethane extraction is used for the determination of low concentrations of iron in water. A sensitive determination of aluminium based on detection at 254 nm is also reported.

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