A new chemiluminescence (CL) method is proposed for the determination of quinine sulphate, which is based on the dichloromethane solvent extraction of the ion-pair complex of tetrachloroaurate (III) with quinine sulphate, and luminol CL detection in a reversed micellar medium formed by the cation surfactant cetyltrimethylammonium bromide in a dichloromethane–cyclohexane (3:7, v[sol ]v)–water (0.35 mol[sol ]L Na2CO3 buffer solution, pH 11.5). The ion-pair complex of tetrachloroaurate (III) with quinine sulphate produced an analytical CL signal when it entered the reversed micellar water pool. In optimum conditions, CL intensities are proportional to the concentrations of the studied drug over the range 0.015–10 µg[sol ]mL, with a detection limit of 1.5 ng[sol ]mL. The relative standard deviation (RSD) is 1.38% for 2.5 µg[sol ]mL quinine sulphate (n = 11). The method has been applied to the determination of the studied drug in biological fluids, with satisfactory results. Copyright © 2005 John Wiley & Sons, Ltd.