A new method of determination of sulfadiazine, sulfamethazine and sulfadimethoxine in biological material based on HPLC with micellar mobile phase has been proposed. The separations were made on a column Nucleosil C-18 (150 x 4.6 mm) with a mobile phase of a water solution of sodium dodecylsulfate (SDS), phosphate buffer of pH 2.8 and propanol-2 as an organic modifier. The calibration curves determined for each sulfonamide were linear in the range from 0.05 µg/g to 4.0 µg/g meat and from 0.05 µg/ml to 2.0 µg/ml blood serum. The values of the linear correlation coefficient varied from 0.974 to 0.999, the detection limit was 0.025 µg for sulfadiazine and sulfamethazine and 0.05 µg for sulfadimethoxine, per 1 g of meat and 1 ml of cow´ s blood serum. The method proposed is characterised by good accuracy and precision. The accuracy of determination of the drugs in meat varied from -3.0 to 7.8 %, while for blood serum from 0.4 to 8.7 %. The method´ s precision was 3.67 to 6.0 % and 3.74 to 6.6 %, for sulfonamides in meat and blood serum. The recovery of sulfonamides introduced into meat and serum was determined as 87.2 and 92.0 % for sulfadimethoxine, 103 and 99.6 % for sulfamethazine.