A method of ion-pair chromatography was developed on a reversed-phase silica-based monolithic column for the fast and simultaneous determination of trifluoromethanesulfonate (CF 3 SO 3 -) and p-toluenesulfonate (C 7 H 7 SO 3 -). The analysis was performed using a mobile phase of tetrabutylammonium hydroxide ? citric acid ? acetonitrile on the Chromolith Speed ROD RP-18e column with direct conductivity detection. The effects of the eluent, column temperature and flow rate on the retention of the anions were investigated. The experimental phenomenon was discussed according to hydrophobic interaction and ionexchange mechanism in the separation. The optimized chromatographic conditions were selected. The optimized eluent for the separation consisted of 0.2 mmol L -1 tetrabutylammonium hydroxide ? 0.10 mmol L -1 citric acid ? 9% acetonitrile (pH 5.5). The flow rate was set at 6.0 mL min -1 . The column temperature was 25°C. Under the optimal conditions, the better separation of CF 3 SO 3 -and C 7 H 7 SO 3 -was achieved without any interference by other anions (Cl -, Br -, I -, NO 3 -, SO 4 2-, ClO 3 -, BF 4 -and PF 6 -). The detection limit (S/N = 3) was 0.28 and 0.71 mg L -1 for CF 3 SO 3 -and C 7 H 7 SO 3 -, respectively. The method has been applied to the determination of CF 3 SO 3 -and C 7 H 7 SO 3 -in ionic liquids. The spiked recoveries of CF 3 SO 3 -and C 7 H 7 SO 3 -were 101.1 and 100.2%, respectively.