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Development of effective chromatographic or electrophoretic separation involves judicious deciding of selection of optimal experimental conditions that can provide an adequate resolution at a reasonable run time for the separation of interested components. Box-Behnken factorial design was effectively applied for the separation optimization of eight structurally related sulfonamides using capillary zone electrophorosis and reverse high performance liquid chromatography. Optimum values for volume ratio of THF to H2O in eluent, column temperature and flow rate of eluent are found as 12 to 88, 35 ℃ and 1.0 mL/min, respectively.Box-Behnken modified optimization model is extended to separation by capillary electrophoresis (CE). While using CE, a satisfactory separation is achieved with a minimum resolution larger than 1.0 for a separation time less than 10 min.