A new method based on the combination of dispersive solid-phase extraction and capillary electrophoresis is proposed for the determination of sulfamethoxazole in milk samples. Butylamide silica was synthesized and used as extractant. Factors involved in sample treatment method such as: butylamide silica amount, NaOH concentration in methanol, sample volume, and dispersion time were evaluated using a Taguchi parameter design. Under optimal conditions, average recoveries ranged from 73 to 85% with a limit of detection of 0.05 mg L 1 were achieved. The proposed method is a useful technique for cleanup milk samples.
