A chromatographic procedure is described for the separation of metal-cyano complexes using reversed-phase ion-interaction high-performance liquid chromatography. Cyano complexes of copper(I), silver(I), iron(II), cobalt(III), iron(III), gold(I), palladium(II) and platinum(II) may be resolved on a C 18 column using a mobile phase of acetonitrile-water (23:77, v/v) containing 0.005 M tetramethylammonium hydroxide, with UV detection at 214 nm. Alternatively, cyano complexes of cobalt(III), copper(I), silver(I), nickel(II), palladium(II), gold(I) and platinum(II) may be resolved on a cyano column using a mobile phase of acetonitrile-water (8:92, v/v) containing 0.005 M tetramethylammonium hydroxide. The influence of variation of the nature of the ion-interaction reagent is discussed. The method is applied to the analysis of gold in processing solutions taken from the carbon-in-pulp process and excellent agreement between the chromatographic method and inductively coupled plasma atomic emission spectroscopic analysis is reported. Detection limits for precious metals were 1.9, 2.6, 0.9 and 0.8 ng for silver(I), gold(I), platinum(II) and palladium(II), respectively. Precision of the method for gold at the 0.1-μg level was 1.00% for peak area measurements and the calibration plot for gold was linear for injections containing up to 0.3 μg of gold.