Determination of sulfonamide compounds in sewage and river by mixed hemimicelles solid-phase extraction prior to liquid chromatography–spectrophotometry

Mixed hemimicelles-based solid-phase extraction was investigated for the preconcentration of five sulfonamides from environmental water samples prior to HPLC–spectrophotometry determination in this paper. A comparative study on the use of sodium dodecyl sulfate (SDS) coating γ-alumina or octadecyltrimethylammonium bromide (OTMABr) and OTMABr coating silica as sorbent materials were presented. The five analytes (sulfadiazine (SDA), sulfathiazole (STA), sulfapyridine (SPD), sulfamethazine (SMZ) and sulfamethoxazole (SMX)) were quantitatively adsorbed on OTMABr-γ-alumina and OTMABr-silica mixed hemimicelles, but OTMABr-γ-alumina was not adopted because it worked at a high pH (around 10), instead, OTMABr-silica was selected to overcoming the pH restriction. The analytes retained on the cartridge were quantitatively desorbed with suitable amounts of methanol. Factors influencing the extraction efficiency, such as the amount of surfactant, pH of sample and breakthrough volume were discussed. The proposed method had been applied to determining the five sulfonamides in several environmental water samples and concentration factors of 300 and 600 for SDA and other four analytes were achieved, respectively. Detection limits obtained ranged between 0.15 and 0.35 μg/L for this five sulfonamides under the optimized conditions. The accuracy of the method was evaluated by recovery measurements on spiked samples, and good recovery results (89–113%) with precision of 3–6% were achieved.