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An indirect simple and rapid cloud point extraction is proposed for separation and preconcentration of sulfadiazine and its determination by flow injection-flame atomic absorption spectroscopy (FI-FAAS). The sulfadiazine from 35 mL of solution was readily converted to silver sulfadiazine upon addition of silver nitrate (9.7 × 10 -5 mol/L). Then, Triton X-114 a non ionic surfactant was added and the solution was heated to 60°C. At this stage, two separate phases was formed and silver sulfadiazine enters the surfactant rich phase of non-ionic micelles of Triton X-114. The surfactant-rich phase (~50 µL) was then separated and diluted to 300 µL with acidic methanol. The concentration of silver in the surfactant-rich phase which is proportional to the concentration of sulfadiazine in sample solution was determined by FI-FAAS. The parameters affecting extraction and separation were optimized. Under the optimum conditions (i.e. pH 2-10, silver concentration (9.7 × 10 -5 mol/L), Triton X-114 (0.075% v/v) and temperature 60°C) a preconcentration factor of 117 and a relative standard deviation of 4.9% at 37 mg L -1 of sulfadiazine was obtained. The method was successfully applied to analysis of milk, urine and tablet samples and accuracy was determined by recovery experiments.

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